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NATIONAL INSTITUTE OF

STANDARDS AND TECHNOLOGY

MIST

PUBLICATIONS

GAINING THE

COMPETITIVE EDGE

Sales of U.S. exports are booming. Business and

Innovation are flourishing, and the United States is an

Industrial power to be reckoned with. The year is 1901

and the U.S. Congress has just created the National

Bureau of Standards to help the nation's industries reach

their full potential.

Ninety years and a new name later, the National Institute

of Standards and Technology continues its mission with

renewed purpose. After more than a decade of trade

deficits and losses in global market share in key

industries, U.S. industry's prospects are again on the rise.

Exports are up. Productivity is rising. While competition

remains fierce, a ground swell of new determination

among U.S. business leaders to produce high-quality,

low-cost products makes me optimistic about the future.

Here at NIST we have a similar determination. We have

made it our top priority to help U.S. industry improve the

quality and international competitiveness of its products.

In the last few years, we have added new services and

outreach efforts to complement long-standing research

programs of proven practical value to business and

industry. We have expanded the range of topics available

for research collaborations and the mechanisms for doing

so—from one-on-one joint studies to industry/government

consortia with dozens of members. And we've worked

through NIST's management of the Malcolm Baldrige

National Quality Award to help U.S. companies adopt

management practices that improve product quality and

customer satisfaction.

Each year more than 1,000 researchers from industry,

universities, or other government agencies come to NIST

to conduct cooperative research projects lasting from a few weeks to several years. What they find here is a capable, motivated staff and many first-class laboratory

facilities—like a 20-megawatt research reactor with a cold neutron source, a video supercomputer, and an automated manufacturing research facility.

In years past, some U.S. companies have been reluctant

to conduct joint research with federal agencies for fear

their competitors could gain access to proprietary

information through Freedom of Information Act (FOIA)

requests. Other firms have been unwilling to invest in
cooperative research when the results of that research

would be co-owned with the government and thus available to competitors.

Since the passage of the Federal Technology Transfer

Act in 1986 these fears have been laid to rest. The act

explicitly protects proprietary information provided by a cooperative research and development partner from FOIA

requests. It also allows federal laboratories to grant exclusive licenses to cooperative research partners for the

intellectual property developed during a given project.

In today's fast-paced business environment, major

scientific advances are commercialized in a year or two

rather than a decade, and product life cycles are dramatically shorter. Business survival demands that

companies continuously improve their products and

fine-tune their processes. In such an environment, NIST

research, services, and facilities can help provide

companies with that critical competitive edge needed for success in the marketplace.

The pages that follow describe the full spectrum of NIST

programs and facilities available for industry participation

and use. Each item includes the name and phone number

of a NIST program manager or researcher to contact for

more information. Take time now to find the NIST

resources and research projects of greatest interest to you. Then give us a call. Chances are there's a NIST

program or service that can help your company meet its research and product quality goals.

2
CONTENTS

GAINING THE 1 UUIVIrC 1 1 1 IVC cUuc

SERVING THE CUSTOMER 4

TECHNOLOGY SERVICES 8

ELECTRONICS AND ELECTRICAL 12

ENGINEERING LABORATORY

MANUFACTURING ENGINEERING 24

LABORATORY

CHEMICAL SCIENCE AND 32

TECHNOLOGY LABORATORY

PHYSICS LABORATORY 47

MATERIALS SCIENCE AND 55

ENGINEERING LABORATORY

BUILDING AND FIRE 72

RESEARCH LABORATORY

COMPUTER SYSTEMS 80

LABORATORY

COMPUTING AND APPLIED 86

MATHEMATICS LABORATORY

FACILITIES INDEX 88

SUBJECT INDEX 88

3
SERVING

THE CUSTOMER

MEETING

CHALLENGES

In business circles these days, the

concept of "total quality management" is rapidly taking hold. Its main tenets are quite simple. Involve everyone in the organization

from production-line workers to

the CEO in producing quality products and never lose sight of one

thing—your customers.

At the National Institute of

Standards and Technology, U.S.

businesses, large and small, are our most important customers. Our full range of programs

from direct grants for development

of generic technologies to frontier

studies of physical laws to calibrations of quality control instru- ments—is designed to help

U.S.-based companies compete in

the marketplace.

NIST is a strategic national

resource. The Institute offers a

"critical mass" of resources, research personnel, and facilities

that can help firms leverage their

research and development invest- ment and speed progress toward

meeting technology goals for new

products or improved processes. It does so through several major

avenues:

direct technical or financial assistance to U.S.-based companies;

measurement and standards

services, such as Standard Refer- ence Materials or equipment

calibrations;

joint research with industry,

university, or other government

scientists and engineers;

standards activities with industry; local, state, and federal governments; and international

organizations; and

availability of selected research

facilities for cooperative research

or for proprietary work on a costrecovery basis. Within each of these areas, many different levels of interactions are possible. Technical

assistance provided by NIST or its

regional Manufacturing Technology Centers may mean answering

a single question over the phone

or offering guidance for a complete overhaul of a company's

shop floor operations. Joint research may involve exchanging a few samples for measurements or

several years in which an industry

researcher works side-by-side with a NIST researcher on a project of mutual benefit. In fact, cooperative efforts may involve any number of different combinations of

personnel, equipment, funds, or

facilities resources.

TANGIBLE

BENEFITS

Companies that take advantage of NIST programs reap tangible, lasting benefits. Bell Helmets recently

cooperated with NIST's "Shop of

the 90s" researchers, six computer

software and hardware companies,

and the United States Performance

Engineering Program to produce an aerodynamic helmet for the

U.S. Olympic speed-skiing team.

In about 1 month, the cooperative

research and development project

resulted in a computer-designed

and manufactured (CAD/CAM)

mold for producing the futuristic- looking helmets.

Prior to the project, Bell Hel- mets made all its new helmet

molds by hand. With its new

CAD/CAM expertise, the company now plans to convert all of its research and development design

work to computer technology by

1993- The changeover should save

the company up to 9 months of

design time for each new helmet.

In a different type of cooperative effort, NIST physicists have

provided critical measurements to AT&T Bell Laboratories, the Lockheed Corp., Ovonics Inc., and

several government and university

laboratories involved in the new

field of soft X-ray optics. With a

special characterization facility

the only one of its kind in the

United States available to the

general scientific community

the NIST researchers evaluate

multilayer "mirrors" provided by

the companies and used for focusing X-ray beams like a lens

focuses light.

Measurements of properties

like homogeneity, reflectivity, and

Soft X-ray "mirrors" made

from a sample material,

held here by physicist

Richard Watts, could

dramatically improve the

performance of certain

telescopes, lasers, microscopes, and semiconductor

integrated circuits.

surface roughness made at the NIST facility allow the cooperating companies to accelerate their

research by matching precise

property data with processing

parameters. A lucrative market

awaits commercial production

of the new X-ray "mirrors," which

could dramatically improve the performance of certain telescopes,

lasers, and microscopes and

allow semiconductor manufac4
Using the neutron depth

profiling apparatus with the

new cold neutron source

at the NIST 20-megawatt

research reactor, NIST re- searchers have collaborated

with the Intel Corp. to map

precisely boron concentrations in silicon wafers.

turers to further shrink the size of

integrated circuits. An example of NIST working

with industry on a large scale is

the North American ISDN Users' Forum. The group addresses the

protocol standards and other user

needs for the emerging technology

called Integrated Services Digital

Network (ISDN). The technology

promises to revolutionize telecommunications by making it possible

to send voice, data, and images

simultaneously over telephone

lines. Working cooperatively, NIST

computer researchers and forum

committees have developed a series of test specifications for these

systems designed to ensure that ISDN products by different manufacturers work compatibly. The

recent acceptance of these test

specifications by international

standards organizations governing

such standards will enhance the

ability of U.S. -based manufacturers to compete in international

markets.

BETTER "CHIPS"

A project carried out over the last

7 years between NIST chemists

and researchers from Intel Corp.

has helped the company reduce

waste in production of its advanced semiconductor "chips."

Working at the Institute's 20-megawatt research reactor,

Intel and NIST researchers use the unique capabilities of two neutron

depth profiling facilities to map

precisely the chemical composition of silicon wafers used in making integrated circuits. The

non-destructive method allows the

researchers to pinpoint the location and concentration of otherwise difficult-to-measure elements

like boron in the surface of the

wafer and then to test the same

sample with optical or chemical

analysis techniques. Precise chemical composition data are critical

NIST AT A GLANCE

The National Institute of Standards and Technology was

established by Congress to "assist Industry In the develop

ment of technology . . . needed to Improve product quality, to modernize manufacturing processes, to ensure

product reliability ... and to facilitate rapid commercialization ... of products based on new scientific

discoveries."

An agency of the U.S. Commerce Department's

Technology Administration, NIST's main goals are to strengthen U.S. industry's competitiveness, advance

science, and improve public health, safety, and the

environment.

NIST conducts basic and applied research in the physi

cal sciences and engineering, developing measurement

techniques, test methods, standards, and related services. The Institute does generic and precompetitive re- search and development work on new advanced

technologies.

Budget $354 million

(FY 91 estimated resources from all sources)

Staff More than 3,000 scientists, engineers, technicians, and support personnel, plus some

1,000 visiting researchers each year

Sites Gaithersburg, Md. (headquarters —

234-hectare campus)

Boulder, Colo. (84-hectare campus)

Main Electronics and electrical engineering

Research Manufacturing engineering

Areas Chemical science and technology

Physics

Materials science and engineering

Building and fire research

Computer systems

Computing and applied mathematics

for quality production of the boron-containing glasses used as

insulating layers in such circuits.

In the same field of semiconductor manufacturing, a

senior research fellowship pro- gram coordinated by the American

Statistical Association with funds

from the National Science Foundation placed an industrial research

consultant on a 1-year appointment at NIST to study statistical methods for improving quality

control. The consultant and

NIST statisticians and electronics engineers applied an alternative model to one widely used in

5
First presented in 1988, the Malcolm Baldrige National

Quality Award has quickly become both the U.S. standard

of quality achievement In industry and a comprehensive

guide to quality improvement. Tens of thousands of U.S.

companies are using the application guidelines to evaluate their operations in seven key areas of quality

management and performance: leadership, information

and analysis, planning, human resource use, quality assurance of products and services, quality results, and

customer satisfaction. The results of these internal evaluations provide firms with a clear view of where they stand

and of how far they must go to achieve world-class levels

of quality—and to compete for the national quality award.

The award program, developed and managed by MIST

with the cooperation and financial support of the private

sector, recognizes quality achievements in three

categories: manufacturing, service, and small business.

Up to two awards can be made in each category. Applications for the award undergo a rigorous evaluation by an independent review board composed of quality experts

from the private and public sectors. Examiners conduct

on-site reviews at firms that receive high scores after an

initial screening. All applicants receive a written summary that identifies their strengths and points out areas

for improvement.

Firms entering the competition pay a fee that covers

the cost of the evaluation and feedback reports. Profiles on the quality programs of past award winners are available upon request. Copies of application guidelines also are available.

Contact: Malcolm Baldrige National Quality Award Office

A537 Administration

(301) 975-2036

the industry to predict when

integrated circuits will fail due

to a phenomenon called

"electromigration."

As manufacturers make integrated circuits smaller and

smaller, high densities of electrical current running through

microscopic "wires" in the circuits

are more likely to cause the aluminum in the "wires" to move

or migrate out of position. When

enough metal in the "wire" moves, a void forms in the circuit and the entire device fails. The

NIST cooperative research team

has suggested an improved model

that better accounts for circuits of

vaiying lengths. Once the model is

validated with laboratory experiments using special test structures,

the industry as a whole should

benefit through more accurate

predictions of lifetimes for these complex devices.

INDUSTRIAL

CONSORTIA

Other research programs incorporate formal consortia in which a

group of companies exchange

data, ideas, researchers, and/or

materials with NIST to meet

agreed-upon research goals. For example: A NIST consortium consisting of Cascade Microtech Inc., ITT

Defense and the Gallium Arsenide

Center, TRW Electronic System

Group, and several U.S. Department of Defense laboratories contributes funding to Institute

research on standards and test methods for a new type of miniaturized microwave device. The devices incorporate components for generating or processing

MALCOLM BALDRIGE

NATIONAL QUALITY AWARD

microwave and millimeter-wave

signals on a single integrated

"chip," just like current integrated

circuits used in computers. The new technology could cut the cost

of some microwave systems by tens

of thousands of dollars. In return

for their support of NIST research

in this area, members of the consortium receive new standards and

software developed through the

program 1 year in advance of the

general technical community.

A cooperative project with the Automotive Composites Consor- tium (ACC) aims to improve the manufacture of new structural polymer composites for use in future automobile frames. ACC members include Chrysler Corp., Ford

Motor Co., and General Motors

Corp. NIST materials science researchers have created a computer

model that describes in three dimensions the flow of a polymer

into a mold containing reinforc- ing fibers. The polymer hardens

around the fibers to create these

lightweight, yet strong, automotive frames. The participating companies will use the NIST flow

model to improve the efficiency

of their companies' fabrication of such components.

A consortium of manufacturers

and trade associations provided

$1 million through the National

Fire Protection Research Foundation to fund NIST research on a new method for estimating fire

risks. Working collaboratively with

scientists and engineers from the National Fire Protection Association and Benjamin/Clarke

Associates, a fire protection consulting firm, NIST researchers

developed a way to estimate on a

national scale fire death rates associated with new product designs.

The method uses fire incidence

data to produce descriptions of

tens of thousands of fires in different settings, such as single-family

homes, offices, and hotels. This in- formation is used with a NIST

software program called HAZARD I

to predict how new compositions

or designs for furniture, building

materials, or other products would

affect the number of fire deaths associated with each scenario. Combining the expected outcomes

from all of the fire simulations allows manufacturers to determine

whether new product designs will

increase or decrease fire risks compared with current products.

6
PROJECT

CONTACTS

To help you identify which NIST

programs, services, or facihties

best fit the needs of your particular organization, the remainder of this booklet provides

detailed descriptions of individual

activities. The cooperative research opportunities and facilities

listed are representative of what is

available within each major NIST

laboratory. Unless otherwise

noted, all addresses listed are at NIST, Gaithersburg, Md. 20899-

If you are not sure which

NIST research area or facility

matches best with your

organization's needs, the NIST

Technology Development Pro- gram staff can probably help you. This office handles NIST patents,

licensing, cooperative research

and development agreements, and

other formal cooperative research

contracts.

CONTACT: Bruce E. Mattson A345 Physics

(301) 975-3084

ADVANCED TECHNOLOGY

PROGRAM

Many of tomorrow's commercial success stories will start with today's basic research discoveries and technological

innovations. Perhaps understood in only scant detail,

today's laboratory curiosities provide a glimpse of potentially far-reaching future applications in products and

processes. But in the foreground stand tremendous

obstacles—high development costs and technical

challenges that may take many years to resolve.

NIST's Advanced Technology Program (ATP) provides

partial funding to single firms or industry-led joint ventures that undertake high-risk, high-return research projects to develop generic, precompetitive technologies. The

aim of the cost-sharing program is to reduce some of the

risk inherent in pursuing applications of emerging technologies. Once technical feasibility is established, companies can undertake on their own development of a prototype product and the other steps needed for

commercialization.

The ATP embraces all areas of technology but emphasizes those with a broad range of potential applications. Grants to Individual firms are limited to $2 million over 3 years; awards to joint ventures can be up to 5 years, with the total grant determined on a case-by- case basis. The private sector must share the costs of all ATP projects. Awards are made yearly, and the program

budget is set annually by Congress.

Contact: Advanced Technology Program

A430 Administration

(301) 975-2636

Senior research fellow

Wayne Nelson (left) poses

with NIST collaborators

(from left to right) electronics engineers Harry

Schafft and John Suehle and

statistician James Lechner.

The team developed an

alternative model to predict

failure of integrated circuits due to a phenomenon

called "electromigration."

7
TECHNOLOGY

SERVICES

NIST provides a wide variety of services and programs to

lielp U.S. industry get on witli its most pressing tasks:

innovation, rapid commercialization of new technology,

and achieving total quality in all facets of business operations. The programs and services described below complement NIST's basic and applied research programs. New

outreach efforts like the regional Manufacturing Technology Centers build on NIST's long-standing experience serving industry's needs for reference materials and standards

development.

The measurement services work performed by Technology

Services offices has applications in every area of manufacturing and technology development. If a process cannot

be measured, then it cannot be fully understood. Incomplete understanding, in turn, increases the likelihood of

process errors, product flaws, and other problems that

lead to inefficiency and variations in quality. Companies

spanning nearly all industrial sectors depend on the

precision and reliability of NIST measurement services to keep their production processes running smoothly and

efficiently.

Similarly, standards information and development are

critical elements for every industry sector in the global

marketplace. As national economies become more interdependent and as foreign sales account for an ever-larger

share of many firms' bottom lines, domestic and international standards-setting activities have grown in economic

and strategic significance. NIST staff members are active

in more than 800 voluntary standards committees. In addition, the Institute provides a variety of informational and

advisory services that can help businesses and other interested observers stay abreast of developments in the

nation's and world's standards bodies.

Contact: Donald R. Johnson

A363 Physics

(301) 975-4500

MANUFACTURING

TECHNOLOGY

CENTERS

Hands-on technical assistance for small and mid-sized manufacturers—that's the mission of the

five Manufacturing Technology

Centers (MTCs) jointly funded by

NIST, business, and state and

local governments. Programs are

tailored to the needs of local industry, but each MTC emphasizes

technology transfer, helping

manufacturers make effective use

of the advanced technology most

appropriate for their operations.

The other common emphasis is educating companies on the concepts and practices of total quality

management.

For many of the nation's more

than 350,000 small and mid-sized

manufacturers, moving up the

technological ladder from

manual operations to flexible computer-integrated manufacturing systems can be a risky and

difficult task. Using in-house

demonstration facilities, MTC

teams of business, manufacturing,

marketing, and training experts

help companies identify the best combination of equipment and

software for particular business

needs. They also follow up with

worker training programs and

other measures to ensure that the new technology delivers all of its

anticipated benefits.

CONTACTS:

General Information: Philip

Nanzetta, MTC program director,

B124 Metrology, NIST, Gaithersburg, Md. 20899, (301) 975-3414

Great Lakes MTC: George

Sutherland, director. Great Lakes

MTC, Cleveland Advanced Manufacturing Program, 2415 Woodland Ave., Cleveland, Ohio 44115,

(216) 987-3200

Northeast MTC: Gene Simons,

director. Northeast MTC,

Rensselaer Polytechnic Institute,

CII-9009, Troy, N.Y. 12180,

(518) 276-6682

Southeast MTC: Steven Eisele,

assistant director. Southeast

MTC, University of South

Carolina, Swearingen Engineering

Center, Columbia, S.C. 29208,

(803) 777-9595

Mid-American MTC: William

Brundage, acting director, Kansas Technology Enterprise Corp., 112

S.W. 6th Ave., Suite 400, Topeka,

Kan. 66603, (913) 296-5272

Mid-West MTC: Jack Russell,

director. Industrial Technology

Institute, 2901 Hubbard Rd.,

Ann Arbor, Mich. 48106,

(313) 769-4690

STANDARDS AND

CERTIFICATION

INFORMATION

The NIST National Center for Standards and Certification Information is the U.S. focal point for information on standardization

programs and related activities at home and abroad. Center staff provide information on U.S., foreign,

regional, and international voluntary standards bodies, as well as mandatory government regulations and conformity assessment

procedures for non-agricultural

products. As the U.S. member of

the International Organization for

Standardization Information Net- work (ISONET), NIST has access

to foreign national standards information through approximately

60 other ISONET members and the

8
ISO information center in Geneva,

Switzerland. NIST also serves as

the U.S. inquiry point under the General Agreement on Tariffs and

Trade (GATT) Agreement on Technical Barriers to Trade.

At the center, NIST maintains an extensive collection of refer- ence materials, including U.S.

military and other federal govern- ment specifications, U.S. industry

and national standards, international standards, and selected

foreign national standards. Staff members respond to requests for information either directly or by

identifying the most appropriate

source of information. They also

prepare directories and indexes of

specialized standards information,

arrange for translations of foreign

standards, and issue periodic publications explaining ongoing

developments in domestic and international standards activities. Two telephone hotlines located

within the center offer weekly updates on draft European standards

[(301) 975-4164] and on

proposed foreign regulations that may significantly affect trade

[(301) 921-4041]. Information

for the latter hotline is supplied by

the GATT Secretariat in Geneva.

CONTACT: JoAnne Overman

A163 TRF

(301) 975-4037

STANDARDS

MANAGEMENT

NIST manages U.S. technical

representation and participation

in the International Organization

of Legal Metrology (OIML) and administers the U.S. Department of Commerce's Voluntary Product

Standards (VPS) program.

OIML is a treaty organization

with a membership of 49 voting

and 34 non-voting nations. It works to enhance trade by har- monizing national regulations

governing performance requirements for measuring instruments

used in commerce and for monitoring and maintaining

public health and safety. NIST

standards management staff

solicit technical advice and support from U.S. trade associations,

instrument manufacturers,

academia, and federal and state

regulatory agencies in developing

and approving OIML draft documents.

Staff members also serve as the

secretariat for the development of

voluntary standards for selected

The Great Lakes Manufacturing Technology Center

helped AccuSpray Inc. redesign its product and

production method. Here,

AccuSpray employee Kevin

Rowell demonstrates the

special paint spraying equipment, which uses half the

paint of conventional

methods.

products, with the costs being paid

by proponent trade associations or

other groups. Current standards

published and maintained under

this VPS program include

softwood lumber, construction

and industrial plywood, and glass

bottles for soft drinks.

CONTACT: Samuel E. Chappell

A625 Administration

(301) 975-4023

WEIGHTS AND

MEASURES

Helping state and local govern- ments ensure the equity of weights

and measures in the marketplace

is one of NIST's longest running

and best known programs. It includes a certification program for

state weights and measures

laboratories in the areas of mass,

length, and volume, as well as providing test protocols, certification training, and ongoing

laboratory assistance. NIST sponsors the National

Conference on Weights and

Measures, which involves over

3,000 industry and regulatory

agency representatives, and pro- gram staff produce numerous

training manuals, handbooks,

and other publications. The staff

also operate an electronic bulletin board to provide the weights and

measures community with a mechanism for rapidly exchanging information.

CONTACT: Carroll S. Brickenkamp

A617 Administration

(301) 975-4004

STATE TECHNOLOGY

OUTREACH

The State Technology Extension

Program staff work with state and

local technology outreach

programs to improve the competitiveness of small and mid-sized

businesses through the application

of science and technology. Assistance offered by program staff

includes:

stimulating cooperation and

communication between and

within states to enhance their

capability to meet the needs of

local businesses;

collecting and disseminating in- formation about successful tech- nology assistance activities, such

as best practices, model programs,

and common tools; and

providing matching grants for development and coordination of technology assistance activities.

CONTACT: Gale R. Morse

A343 Physics

(301) 975-4520

RESEARCH AND

TECHNOLOGY

APPLICATIONS

Facilitating the transfer of NISTdeveloped technologies to business

and industry is the function of the NIST Research and Technology

Applications Program. The office

staff identify NIST research staff,

publications, and technologies to respond to technical questions

from individual businesses. Staff members organize or participate

in workshops and seminars on

specific technical topics and new

technology transfer methods. Pro- gram staff also arrange visits to NIST for business and industiy

9
researchers and managers interested in learning more about Institute research programs.

The office staff serve as the NIST point of contact for the

Federal Laboratory Consortium.

CONTACT: Joseph G. Berke

A343 Physics

(301) 975-5017

TECHNOLOGY

DEVELOPMENT AND

SMALL BUSINESS

INNOVATION

A variety of outreach efforts managed under the Technology

Development Program aim to increase the number of NIST

cooperative research projects and

to improve the transfer of NIST

technologies to U.S. -based industries. Program staff members

help industrial, academic, or government researchers locate NIST personnel and facilities in

their fields of interest for either

collaborative or proprietary research and they facilitate preparation of formal cooperative

research and development agree- ments. They also handle the licens- ing and administration of NIST's more than 120 patents and other

intellectual properties.

In a separate program, a per- centage of NIST's extramural research budget is earmarked for funding of innovative research and development by small businesses—those with fewer than 500

employees. Each year, the Department of Commerce, NIST's parent

organization, issues a list of recommended research and

development topics. NIST personnel evaluate the proposals submitted by small businesses for

research in these areas. Winners of

To help ensure the accuracy

of environmental quality

measurements, NIST sells a wide range of Standard Ref- erence Materials from

"Estuarian Sediment" to "Trace Elements in Coal."

Phase I awards receive $35,000 to support studies of technological

feasibility. In Phase II, applicants

may receive up to $200,000 to support development of promising

technologies.

CONTACT: Bruce E. Mattson A343 Physics

(301) 975-3084

STANDARD

REFERENCE DATA

Working closely with industry,

NIST provides well-documented

numeric data to scientists and

engineers for use in technical

problem-solving, research, and

development. These recommended

values are based on data which

have been extracted from the

world's literature, assessed for

reliability, and then evaluated to

select the preferred value. The

evaluations are carried out through a network of data centers,

projects, grants, and cooperative

programs.

Standard Reference Data

(SRD) have a variety of uses in

industrial applications and are

available as databases for personal

computers, as well as in other computerized forms, and as publications. Common applications

include use for calibration points

(such as spectral wavelengths and

transition energies) and as input

to the design of new processes and materials. Among the many

subjects covered by the data are

analytical chemistry, atomic and

molecular physics, chemical

kinetics, fluid mixtures, thermochemistry, materials properties,

and phase equilibria.

To increase the usefulness and

accessibility of data, NIST has

developed a series of personal computer databases with interactive programs, search routines, and

other calculational and graphical

software features. Most databases

are updated yearly, adding more

data and more software

capabilities.

A free catalog of NIST SRD

data products and services is available. Program staff also issue related publications, respond to telephone inquiries on data

sources, and sponsor seminars on

the program and selected data

centers.

CONTACT: Malcolm W. Chase

A323 Physics

(301) 975-2200

STANDARD

REFERENCE

MATERIALS

Now numbering more than 1,200

and steadily growing to meet the needs of industry. Standard Refer- ence Materials (SRMs) are a

diverse collection of solids, liquids, and gases certified for their chemical composition or physical

properties. With an SRM, companies can verify the accuracy of

analytical or monitoring methods

under development or calibrate established measurement systems to ensure consistently accurate per- formance of equipment and

operators. Specific types of SRMs

range from linewidth standards

for producing integrated circuits

to metal alloys for checking quality control in steel production, to radiopharmaceuticals for calibrating medical equipment.

NIST's SRM catalog provides a complete listing of available reference materials along with a

description of their certified

properties. In addition, the Handbookfor SRM Users offers practical guidance on the use of the

materials, describes the fundamental elements and concepts of quality control and measurement

processes, provides advice on

using control charts and statistical

10
tools to evaluate measurement

quality and uncertainty, and in- cludes articles on quality as- surance, sampling, and validation

of analytical instruments.

The SRM program staff also publish timely information on ref- erence materials, offer telephone

consultations on SRM uses, and or- ganize seminars to advise industry on SRM applications.

CONTACT: Lee T. Best 204 Engineering

Mechanics

(301) 975-6776

CALIBRATION AND

RELATED

MEASUREMENT

SERVICES

NIST provides more than 500

different services to ensure that manufacturers and other users of

precision instruments achieve

measurements of the highest possible quality. These services, which

satisfy the most demanding and

explicit requirements, link a

customer's precision equipment or

in-house standards to national

standards. For calibrations and

special tests, NIST personnel

check, adjust, or characterize an

instrument, device, or set of inhouse, or transfer, standards. Customers are assured that measurements are consistent with national standards and adequate for

their intended use. Besides individual equipment items, NIST

measurement assurance programs

calibrate entire measurement

systems.

The full range of NIST calibration services ensures the accuracy and compatibility of measure- ments used in day-to-day qualitycontrol applications. The services,

available for a fee, encompass

seven major areas: dimensional

measurements; mechanics, including flow, acoustic, and ultrasonic; thermodynamics; optical radiation; ionizing radiation; electro- magnetics, including direct

current, alternating current, radio

frequency, and microwave; and

time and frequency.

The program staff publish a

regularly updated catalog describ- ing available services, fee

schedules, and detailed descriptions of calibration protocols.

Staff members offer telephone consultations on the use of services and on the importance of

traceability to national standards,

and they make presentations to

business groups and other

organizations.

CONTACT: Joe D. Simmons

B362 Physics

(301) 975-2002

VOLUNTARY

LABORATORY

ACCREDITATION

staff of the NIST National Voluntary Laboratory Accreditation

Program (NVLAP) rigorously

evaluate the competencies and

technical qualifications of public

and private laboratories for conducting specific tests or types of

tests in key areas of commerce,

health, and safety. Among other

benefits, certification of proficiency by the NIST program

provides laboratory managers with

a quality-assurance check on

laboratory performance, concrete

advice for improving performance,

and national recognition of competency. At the same time, pro- gram certification helps

users—from industry, govern- ment, and elsewhere—identify

providers of high-quality testing

services.

For a fee, NVLAP currently

accredits laboratories offering

services in the following areas:

acoustical testing, asbestos fiber

analysis, product testing (carpets,

paints, papers, plastics, plumbing,

seals, and sealants), testing of interface protocols for computer networks, construction testing

services, electromagnetic compatibility and telecommunications, personnel radiation

dosimetry, wood stoves, and ther- mal insulation materials. Any interested laboratory, organization,

or agency can request accreditation in these and other areas.

Requests for expanded program

services will be evaluated on a

case-by-case basis. The program staff publish an annual directory of NVLAPaccredited laboratories.

CONTACT: Albert Tholen

A146 TRF

(301) 975-4016

ENERGY-RELATED

INVENTIONS

In cooperation with the U.S. Department of Energy (DOE),

NIST evaluates new product or

process ideas for their potential to improve energy efficiency, reduce energy costs, or increase energy

supply. Besides their energyrelated merits, inventions are

evaluated on the basis of technical

and commercial feasibility. Inventions may be submitted to the program at any stage of development—conceptual, prototype, or

actual production. All inventors

are informed, in detail, of the

results of the free evaluations.

Inventions that satisfy NIST

criteria are recommended to DOE,

which may choose whether to support development and commercialization. Since 1975, DOE has

awarded more than $24 million to move NIST-recommended inventions closer to commercialization.

In addition, inventors may use the NIST recommendation report to

help attract private investment

capital.

CONTACT: George Lewett A115TRF

(301) 975-5500

INFORMATION

SERVICES

The Office of Information Services

maintains a comprehensive international collection of information

in scientific disciplines such as

metrology, mathematics, computer science, and materials

science. The staff serve the technical information needs of NIST

scientists and engineers and

communicate the results of NIST

research to scientific and engineering communities worldwide.

The office staff participate in

national and international publications and technical information

networks and consortia, as well as

a document exchange program to ensure that NIST publications are

available to scholars, scientists, engineers, industry researchers, and

others. An inquiries service assists

the public in obtaining information about past and present NIST

programs, publications, and special projects.

CONTACT: Peggy M. Saunders

El 28 Administration

(301) 975-3058

11 TECHNOLOGY SERVICES
ELECTRONICS AND

ELECTRICAL ENGINEERING

LABORATORY

Vying in fiercely competitive world markets, U.S. manufacturers of electronic products continually push the limits

of current technology, presenting new and ever-morestringent demands for measurement accuracy and

precision. NIST's Electronics and Electrical Engineering

Laboratory works to meet these demands, consulting

closely with industry to identify the most critical

measurement needs in the manufacture of semiconductor,

magnetic, radio frequency, microwave, optical, and

optoelectronics devices and products, as well as

electrical power systems.

In the area of lightwave technology, for example, the

laboratory is developing methods for evaluating the efficiencies of interconnections in optical-fiber networks. In another project, researchers use a newly installed video

supercomputer to develop Improved circuit designs and

test methods for advanced imaging technologies. Other

new or stepped-up research programs are addressing the

measurement needs of companies employing advanced

magnetic or microwave technologies.

While working to improve manufacturing methods for

silicon-based electronic devices, NIST researchers are

also looking beyond the current technological horizon to future generations of devices that will embody new materials and create new market opportunities. The

laboratory's fundamental studies on the properties and

characteristics of high-temperature superconductors support American industry's efforts to develop commercial

applications for the highly promising, yet technically challenging materials. Other basic research is paving the way

for the manufacture and use of devices that transmit and

process both electronic and lightwave signals.

This laboratory provides the fundamental basis for all electrical measurements in the United States.

Contact: Judson C. French

B358 Metrology

(301) 975-2220

COOPERATIVE

RESEARCH

OPPORTUNITIES

ELECTRICITY

PROCESSING

Data compression, motion encoding, scan-rate conversion, scientific visualization, image analysis,

and other video processing research topics are being explored at NIST using a massively parallel

video supercomputer, the Prince- ton Engine. The Princeton Engine,

developed by the David Sarnoff Research Center, Princeton, N.J., is a

l4-giga-instruction-per-second

image-processing system capable

of simulating video rate signals,

including conventional National

Television Standard Code and

high-definition video, in real

time. Because the engine is programmable, it can be used to evaluate software prototypes of image-processing components

rapidly and at a cost below that of building hardware.

The Princeton Engine consists

of 1,024 parallel processors, where

each 1 6-bit processor has its own

ALU, multiplier, and 128 kilobytes

of local memory. Each processor

operates on one picture element

per video scan line, and all processors execute the "same" instructions. Wideband input and output

channels accept and produce a number of analog and digital

video formats. For many applications, video data can be processed

and output at the same rate as

they are input, that is, in realtime. For longer algorithms up to

7 seconds of video data may be acquired in real time, stored in local memory, and, once processed, dis- played at the output at the

original data rate. Programming is accomplished

using a proprietary graphical

programming system intended to

Below. Schematic of the

Princeton Engine and as- sociated equipment. Right.

With images of the ozone

hole over Antarctica,

electronics engineer Bruce

Field demonstrates how the

Princeton Engine video

supercomputer can be used

to design circuits for compressing high-definition

television signals.

+^PIV Vioee?

V

n

•fceMopuiArog

H-f&C.

HOS<

WOtZlC- WOKK12
simulate a circuit design of videoprocessing circuits. Video recorders, multiscan monitors,

high-definition monitors, and additional video support equipment

are available. NIST researchers are interested

in using the Princeton Engine

laboratory for a wide variety of collaborative research projects. Such

collaborations would focus on precompetitive research with broad

applications in advancing the

state of the art in high-definition

systems.

CONTACT: Bruce F. Field B344 Metrology

(301) 975-4230

ELECTRICAL METROLOGY

WITH OPTICAL SENSORS

Researchers at NIST are developing electro-optical methods to measure electrical quantities and

phenomena as part of a program

to develop theory, methods, and

physical standards for measuring

electrical quantities in advanced

high-voltage/high-power systems.

Theoretical studies are focused on

the use of finite-element code for

electric-field computation and

computer-aided data acquisition

and analysis. Experimental research includes high-voltage ac,

dc, and impulse measurements;

high-speed camera techniques; optical multichannel analyzers; and

lasers and detectors.

CONTACT: William E. Anderson

B344 Metrology

(301) 975-2403

GASEOUS

ELECTRONICS

NIST scientists are developing

measurement methods to characterize gaseous dielectrics for highvoltage power systems. Emphasis

is on investigation of phenomena

that affect reliability and safety

associated with operation of

gas-insulated systems, such as production of toxic byproducts in

electrical discharges. Theoretical

work addresses Boltzmann equilibrium statistics, chemical kinetics code, and computer-aided

data acquisition and analysis.

Experimental work focuses on

high-voltage ac and dc tests, gas chromatograph and mass spectrometer techniques for chemical

characterization, and partial dis- charge measurements. Researchers are investigating rf discharges

used for processing electronic materials, including the study of plasma diagnostics and kinetics as

they apply to the plasma processing of semiconductor materials.

CONTACT: Richard J. Van Brunt William E. Anderson

B344 Metrology

(301) 975-2403

AC VOLTAGE

STANDARDS

NIST is conducting both theoretical and experimental research on

the synthesis of precision ac waveforms for use in ac voltage

standards operating nominally

below 10 MHz. The theoretical work includes Walsh functions

and Fourier analysis, timedomain analysis, and precision

RMS-to-dc conversion techniques.

Experimental work involves highspeed, high-accuracy digital-toanalog conversion; precision,

high-speed switching; assembly

and interpretive-level programming for hardware control; and

wideband, fast-settling amplifiers.

CONTACT: Barry A. Bell Bl62 Metrology

(301) 975-2402

TESTING

ELECTRONIC SYSTEMS

New strategies are needed to

evaluate the performance of complex electronic circuits using the

fewest possible tests. A program is under way at NIST that includes

theoretical studies of modeling for

non-linear systems, optimization

techniques using matrices, statistical and random processes, and artificial intelligence. In addition,

experimental work will address

test strategies for component and

instrument testing; fault diagnosis, functional testing, and

calibration; and computer

analysis using both desktop computers and supercomputers.

CONTACT: Barr)' A. Bell Bl62 Metrology

(301) 975-2402

13
COOPERATIVE RESEARCH OPPORTUNITIES

WAVEFORM RECORDER

STANDARDS

As part of a program aimed at meeting tlie metrological needs involved in improving signal acquisition and processing systems, NIST

researchers are developing theory,

methods, and standards for waveform metrology of conducted

signals. The scientists are conducting the theoretical and experimental research necessary to develop

standards for determining the per- formance of waveform recorders

operating nominally below 1 GHz

and will develop techniques for

synthesis of precision waveforms

and for characterization of those waveforms. Theoretical studies

will be conducted on Fourier

analysis, deconvolution techniques, and time-domain analysis.

Program plans include experimental work in precision pulse generation, static and dynamic testing,

and assembly and interpretivelevel programming for hardware

control.

CONTACT: Barry A. Bell BI62 Metrology

(301) 975-2402

ADVANCED AC VOLTAGE

AND CURRENT

MEASUREMENTS

Thermal voltage and current converters offer the most accurate and

broadband method for measuring

ac voltage and current for applications in communications, power

generation, aerospace, and

defense. Thermal transfer standards are calibrated by NIST in terms of reference converters, which have themselves been characterized by reference to the NIST

primary standards—special multijunction thermal converters whose

performance is known. These

primary and working standards in common use throughout the metrology community employ

thermal converters fabricated

from wire elements. Researchers at NIST are studying new methods

for the manufacture of film ther- mal converter structures made by

the use of photolithography on

silicon substrates. The application

of this new technology may result

in improved performance and

reduction in the cost of thermal

converters.

CONTACT: Joseph R. Kinard

(301) 975-4250

Norman B. Belecki

(301) 975-4223

Bl46 Metrology

JOSEPHSON-EFFECT

VOLTAGE STANDARDS

High-accuracy voltage-standard

systems have proliferated among

many industrial, government, and

international standards laboratories with the advent of the

Josephson-array device. Within

this laboratory, there are three

array voltage-standard systems in

operation, including a fully

automated 10-V array system. Guest researchers can gain hands- on experience with array system

operation and verification, as well

as cooperate on studies into both

precision voltage metrology and

Josephson array physics. The

metrology goals are to improve

measurement precision to better than one part in 10^ in applications of direct system-to-system

intercomparisons and lab-to-lab

volt transfers, achieve greater

reliability in automation algorithms, and further the development of solid-state reference

standards and precision digital

voltmeters. The physics research

addresses the effects of electro- magnetic noise on the stability

and accuracy of the Josephson

quantized-voltage steps, studies

the boundaries of chaotic behavior

in junction-junction interactions,

and explores other possible array

device applications, such as the

generation of ac signals through

frequency modulation of the millimeter-wave drive frequency.

CONTACT: Richard L. Steiner

(301) 975-4226

Alan F. Clark

(301) 975-2139

B258 Metrology

RESISTANCE STANDARDS

AND MATERIALS

Component precision resistors of both film and wire construction

have found widespread use as references and dividers in precision instrumentation, such as digital

multimeters and calibrators. The

quality of these resistors and their

level of immunity to the effects of environmental parameters, such

as temperature and mechanical

shock, have enabled the 3-month

performance of these instruments

to begin to approach that of the

standards most commonly used to

calibrate them. This fact and the

desirability of calibrating such in- struments where they will be used

has engendered the need to

develop the next generation of

resistance standards—standards

whose performance in adverse conditions would eclipse that of existing standards in a laboratory

environment.

NIST scientists are beginning a program to develop new standards

with sub-ppm performance, both

short- and long-term, under field

conditions. To do so, the electrical/physical properties of a number of alloys are being investigated, and new resistor designs

are being formulated and tested. Future efforts will investigate

metallurgical techniques such as

rapid quenching, ion implantation in glasses and semiconductors for resistors >10'' Q, and

Evanohm or Nichrome film deposition on Si substrates. The desired

output will be fixed-value standards in the range from 1 Q. to 10'^ Q with sub-ppm per year

drift rates, temperature coefficients less than 0.1 ppm/°C, and

low power and voltage coefficients. A metallurgical facility with the

capability of monitoring the

electrical properties of materials

during annealing and a silicon

processing facility are available

along with access to precision

resistance measurement systems

and the national resistance

standards.

CONTACT: Ronald F. Dziuba

(301) 975-4239

Norman B. Belecki

(301) 975-4223

B146 Metrology

QUANTUM HALL EFFECT

When an electrical current is

passed through the microscopically thin layers of a GaAs/AlGaAs

heterostructure at low temperatures in very high magnetic fields,

plateaus of constant resistance for

certain values of the magnetic

field are observed. These values of

the device resistance are equal to

h/ie^ where h is Planck's constant,

i is an integer, and e is the

14
electronic charge. On Jan. 1, 1990,

this effect, which is known as the quantum Hall effect, became the

basis for the new world standard of

resistance. The adoption of this standard was in large part due to

the development of measurement

systems of unprecedented accuracy

developed at NIST. While the quantum Hall effect provides a stan- dard of resistance that does not

drift with time and is independent

of the specific device used, many

features of the effect and its use as

a basis for a standard are not well

understood.

Researchers at NIST are attacking these problems on three broad

fronts, including understanding

the physical principles underlying

the effect, understanding samplespecific artifacts, and improving

the measurement systems. A

15.5-T magnet and dilution

refrigerator facility is being used

to conduct research on the range

of parameters over which the quantum Hall effect provides the most accurate and reproducible

standard of resistance. Work at NIST has already shown that the quantum Hall resistance may

deviate from its ideal value of

h/ie^ above certain temperatures

and above certain currents.

Recent research at NIST has

opened up the possibility that quantum Hall devices may be a

source of very-high-frequency

phonons when large current densities are passed through the devices. Using GaAs heterostructures grown at NIST, researchers are

using a dedicated class 10 clean room facility to investigate different methods of making contacts

to the devices that will have very

low resistances (in the milli-ohm

range) even at temperatures below

4.2 K and in high magnetic fields.

Research is also being conducted on determining the degree

to which the device resistance is independent of its material by

comparing the resistances of devices made from silicon and

GaAs/AlGaAs heterostructures. NIST researchers are also working to improve and simplify

the measurement systems used to

calibrate resistors; a new He-3

refrigerator and l6-T magnet

facility are being developed for

use with a new cryogenic current comparator. This should enable

the accuracy of NIST calibrations

to be increased severalfold.

CONTACT: Marvin E. Cage

(301) 975-4248

Man F. Clark

(301) 975-2139

B258 Metrology

APPLYING HIGH-Tc

SUPERCONDUCTORS TO

PRECISION ELECTRICAL

MEASUREMENTS

NIST and other national standards

laboratories for years have used

cryogenic current comparators

(CCCs) to make ratio measure- ments of voltage, current, and

resistance with accuracies of

0.01 ppm or better. This approach

has not found widespread commercial use because the cryogenic current comparator must be operated

at liquid-helium temperatures,

which presents a variety of operational difficulties. Moreover, existing comparators are working

prototypes rather than completed

instrumentation systems and, accordingly, are difficult to use.

Recent advances in superconductivity technology have

made the application of hightemperature superconductors practical. In at least one case, an integrated circuit SQUID magnetometer, similar to devices used in CCCs to detect low levels of magnetic flux, has been built that

operates at liquid-nitrogen

temperatures. Thus, the possibility

for developing a commercial in- strument based on a CCC has now

been opened. Such an instrument

might be run with a refrigerator at

liquid-nitrogen temperatures.

This development and the possibility of commercialization

make it feasible to automate the

basic CCC design, which then will

be more attractive for general

calibration use. NIST scientists are now engaged in designing, building, and testing CCCs to support

measurements of the new national

resistance standards based on the quantized Hall effect. This involves establishing a few select

ratios that range from 1:1 to

100:1. Future efforts will include

the development of CCCs with

selectable ratios over a somewhat

larger range.

CONTACT: Ronald F. Dziuba

(301) 975-4239

Randolph E. Elmquist

(301) 975-6591

Norman B. Belecki

(301) 975-4223

Bl46 Metrology

SEMICONDUCTOR

ELECTRONICS

SILICON

CHARACTERIZATION

NIST conducts research in semiconductor materials, processes,

devices, and integrated circuits to

provide the necessary basis for understanding measurement-related

requirements in semiconductor

technology. As part of this pro- gram, NIST scientists are using

electrical, optical, and X-ray

methods to study the resistivity,

dopant distribution, and concentration of electrically inactive

impurities, such as carbon and

oxygen, in silicon. They are developing new or improved

techniques by two- and three- dimensional mapping of these

properties, refining the

quantitative aspects of existing

methods, and developing nondestructive methods. Measurement

techniques include four-probe,

spreading resistance, and

capacitance-voltage; Fourier trans- form infrared spectroscopy; deeplevel transient spectroscopy; X-ray

topography; and synchrotron

radiation studies.

CONTACT: James R. Ehrstein

(301) 975-2060

Paul M. Amirtharaj

(301) 975-5974

A305 Technology

COMPOUND

SEMICONDUCTORS AND

SEMICONDUCTOR

MICROSTRUCTURE

The electronics industry now requires light-emitting and detection devices and ultraliigh-speed

structures that cannot be fabricated from silicon. Compound

semiconductors including III-V

binaries and alloys, such as GaAs

and AlGaAs, and II-VI materials,

such as CdTe and HgCdTe, are employed to complement the functions of the Si circuitr)'. In addition, special and unique electronic and structural properties can be

obtained using artificially structured materials, such ;ls quantum

15 ELECTRONICS AND ELECTRICAL ENGINEERING
COOPERATIVE RESEARCH OPPORTUNITIES

wells and superlattices. Efficient

exploitation of these novel materials and structures in the production of useful electronic devices

requires detailed studies to understand the fundamental physics involved as well as characterization

of possible device structures.

Scientists and engineers at NIST currently are involved in producing and characterizing III- V binary and alloy materials and

device structures using optical

techniques, such as ellipsometry;

electrical procedures, such as

variable temperature Hall effect;

resistivity measurements;

capacitance-voltage profiling;

deep-level transient spectroscopy;

photoconductivity and X-ray diffraction; and rocking curve studies with conventional and synchrotron radiation sources.

CONTACT: David G. Seller James R. Ehrstein

A305 Technology

(301) 975-2081

MOLECULAR BEAM

EPITAXY

The controlled growth capabilities

of molecular beam epitaxy (MBE)

have resulted in the fabrication of

structures that represent a new

class of semiconductors with

properties that do not exist in bulk

materials. The MBE program at NIST includes the growth and

characterization of GaAs and

AlGaAs layers, as well as the growth of heterostructures for superlattice and quantum confinement studies. Scientists examine

fundamental properties of the MBE layers using photoluminescence, deep-level transient

spectroscopy, Hall effect.

secondary-ion mass spectroscopy,

and in-situ reflection high-energy

electron diffraction (RHEED).

Studies are under way to correlate RHEED oscillation intensity measurements with material quality

and growth parameters. The MBE

program is an interactive effort, and cooperative research opportunities exist in a variety of

materials characterization and

device-related areas.

CONTACT: James Comas

(301) 975-2061

Wen F. Tseng

(301) 975-5291

Joseph G. Pellegrino

(301) 975-2123

A357 Technology

SEMICONDUCTOR

SPECTROSCOPY

Spectroscopic studies in the visible and near visible regions of the

electromagnetic spectrum are

invaluable in investigating both

materials and device-related

properties. The ability to couple

to electronic states of interest in

device applications as well as the

non-destructive nature of the

spectroscopic analyses makes

them attractive research and

analytical tools. Studies currently

under way at NIST focus on the

electronic and structural behavior

of semiconductor materials, such

as Si, GaAs, and HgCdTe;

microstructures, including quantum well and superlattices; and

photonic and electronic devices.

Excellent spectroscopic facilities

are available to perform highresolution photoluminescence,

Raman scattering, reflection,

absorption, spectroscopic ellipsometry and modulation spectroscopic measurements, such as

electroreflectance and photoreflectance. The equipment in use

includes one of the highest resolution ellipsometers in the world, excitation lasers, spectrometers,

cryostats, and associated optical

and electronic instruments.

CONTACT: Paul M. Amirtharaj

(301) 975-5974

David G. Seiler A305 Technology

(301) 975-2081

SEMICONDUCTOR

DEVICES

To develop physically sound tech- niques for characterizing, analyzing, and predicting the operation

and performance of semiconductor devices, NIST researchers are designing and improving measure- ment methods to determine critical device parameters for both

VLSI-scale and power devices.

Electrical engineer Dylan

Williams examines a microwave chip at a NIST

wafer-probe workstation.

Research in device modeling includes two-dimensional silicon MOSFET and GaAs MESFET model

development and investigations

into the validity of the physical as- sumptions typically employed in

silicon bipolar and GaAs device

models. Theoretical research is

carried out on the transport of

ions and electrons in semiconductors for improved process modeling, and experimental research on

the nature and characterization of

electronic states in oxides and at oxide/semiconductor interfaces is under way. NIST scientists are

developing methods for physical

and electrical measurements of device and material parameters that

16
are critical for verifying the accuracy and validity of device

models. In addition, they are researching the electrical and

thermal properties of power semiconductor devices.

CONTACT: Herbert S. Bennett B3 10 Technology

(301) 975-2053

ADVANCED

INTEGRATED-CIRCUIT

TEST STRUCTURE

METROLOGY

Integrated-circuit (IC) test structures and test methods developed

by NIST are used widely by the semiconductor industry and other

government agencies. These devices can be used to characterize

integrated-circuit manufacturing

processes, to evaluate the effectiveness of semiconductor processing

equipment, to obtain crucial

parameters for process or circuit

simulators, to perform product

acceptance tests, and to determine

the reliability of the products

manufactured. NIST work involves

test structure design, modeling,

data acquisition, and data

analysis. Institute engineers are

investigating pattern recognition

techniques for the rapid diagnosis

of IC manufacturing processes and for establishing methods to determine the reliability of thin

films used in state-of-the-art

microcircuits.

CONTACT: Loren W. Linholm

8360 Technology

(301) 975-2052

ELECTROMAGNETIC

FIELDS

ADVANCED MICROWAVE/

MILLIMETER-WAVE

METROLOGY

Rapidly developing and expanding

microwave technology requires

research in advanced microwave

measurements and standards. The microwave industry and the Department of Defense depend on

NIST for calibrations of transfer

standards to provide the measure- ment traceability required for

quality assurance and perfor- mance evaluations. NIST researchers have developed highly

accurate six-port techniques for automated measurements of microwave power, attenuation, impedance, scattering parameters,

and noise. They currently are developing greatly improved power

and impedance standards and ex- tending measurement services to

cover millimeter waves and subminiature coaxial connectors.

Collaborative work is particularly desirable in microwave

and millimeter-wave circuit

theory as applied to both tradiional and advanced circuits and

systems, such as MMIC

(monolithic microwave/millimeter-wave integrated circuit)

devices. Applications include

development of advanced

wideband automated network

analyzers using six ports and coplanar and microstrip-on-wafer

MMIC standards.

CONTACT: David Russell

Div. 813.01

Boulder, Colo. 80303

(303) 497-3148

DIELECTRIC PROPERTIES

OF MATERIALS

Inadequate knowledge of the electromagnetic properties of materials inhibits development of new technologies, drives up the

cost of systems and components,

and may prevent achievement of optimal performance levels. A relatively new NIST program in materials is aimed at developing

primary standards and accurate

techniques for measuring the

dielectric properties of materials

used in electromagnetic applications. Scientists at NIST have

developed precision measurement

techniques for complex permittivity based on improved theory

and new cavity and transmission

line sample holders. The

researchers currently are performing the necessary error analyses

and, in the future, plan to cover a

variety of important materials and

temperature ranges over the fre- quency range of approximately

10 MHz to 100 GHz. Reliable nondestructive methods are needed to measure complex permittivity and

the reflectivity of large sheets of

material or structures.

CONTACT: William A. Kissick

Div. 813.02

Boulder, Colo. 80303

(303) 497-3339

ELECTROMAGNETIC

INTERFERENCE AND

COMPATIBILITY

NIST researchers are engaged in a wide range of projects aimed at

quantifying electromagnetic interference (EMI) and electromagnetic compatibility (EMC). One

thrust of the NIST work is to

develop measurement techniques

and methodologies for measuring

emission of unintentional radiation from electronic devices. Another aspect under active investigation is the susceptibility of

electronic equipment to such

radiation. The researchers are

identifying and defining quantities that characterize the susceptibility of a device and then

developing methods to measure

those quantities. Successful completion of this research should

result in the development of standards and measurement techniques for EMI and EMC that are meaningful, technically practical,

and reliable. These techniques

could then be incorporated into

voluntary standards by both U.S. and international standards

organizations.

CONTACT: Motohisa Kanda

Div. 813.03

Boulder, Colo. 80303

(303) 497-5320

ANTENNA

MEASUREMENTS

Researchers at NIST are developing reliable techniques and standards for measuring key

performance parameters of anten- nas and components used with

satellites, Earth terminals, radars,

and communications systems.

Near-field scanning is now used

routinely to characterize

microwave and millimeter-wave

antennas. NIST researchers are now focusing on developing and

implementing techniques to correct for errors in the scan surfaces and applying all near-field tech- niques to higher frequencies.

Software for the analysis of spherical near-field data recently has

been rewritten and improved.

Other research areas include

17 ELECTRONICS AND ELECTRICAL ENGINEERING
COOPERATIVE RESEARCH OPPORTUNITIES

spacecraft and phased-array an- tenna measurements, antenna

diagnostics using near-field techniques, and antenna systems measurements using celestial radio

sources.

CONTACT: Allen C. Newell

(303) 497-3743

Carl F. Stubenrauch

(303) 497-3927

Div. 813.05

Boulder, Colo. 80303

ELECTROMAGNETIC

TECHNOLOGY

NIST researchers characterize

magnetic materials, such as ferro- magnetic and magnetoresistive

films, recording tapes and disks,

ferromagnetic steels, very weakly

magnetic alloys, amorphous ribbons, spin glasses, ferrites, and per- manent magnets, as a function of magnetic field and temperature.

Traditional and improved magnetometer techniques are used, in- cluding vibrating-sample, SQUID,

and Hall-probe. Alternating-field

techniques (ac susceptometry,

B-H loops, rf permeability) and

magnetic-force microscopy also

are used. Attention is given to

calibration accuracy, measure- ment precision, and instrument

development. The research has applications in basic physics and in

applied engineering. Theoretical

work is done in particulate record- ing media and mixtures and

demagnetizing factors. Eddycurrent probes for non-destructive

evaluation are designed and used

to map flaws in metals.

CONTACT: Fred Fickett

Div. 814.05

Boulder, Colo. 80303

(303) 497-3785

Physicist John W. Ekin (left)

and electronics engineer

Steven L. Bray measure the

effect of transverse stress on the electrical properties

of a superconducting material sample.

SUPERCONDUCTOR

MEASUREMENTS

Recent advances in superconductivity have resulted in a critical need for measurement technology

to characterize the different types

of superconductors, which now

range from very fine filament

alloy conductors used in the Superconducting Super Collider cables

to a variety of high-temperature

ceramic superconductors. Active research programs at NIST involve

measurement techniques for critical current, critical magnetic

field, ac losses, magnetic

hysteresis, and electron tunneling.

In addition, specialized experimental work is being done to deter- mine the effect of strain on the superconducting properties of lowtemperature commercial conductors and the high-temperature

materials.

In a recent collaboration with

industry, the resistance of contacts between normal metals and hightemperature superconductors was

decreased by eight orders of magnitude, allowing accurate measurements of the magnetic-field

dependence of the critical current. A standard for measuring critical

current in low-temperature superconductors has been published

through ASTM, and a Standard

Reference Material has been

produced for use in calibrating

critical current measurement apparatus. A new reference material

for large currents is being

developed.

CONTACT: Fred Fickett

Div. 814.05

Boulder, Colo. 80303

(303) 497-3785

18
Engineer Paul Rice positions the piezoelectric scanner of a scanning tunneling

microscope designed to study magnetic features in materials with submicron

resolution.

OPTICAL

ELECTRONICS

NIST researchers are studying optical fiber measurements, optical

communication device metrology,

laser measurements, and optical

fiber sensors. These activities range from the growth of optical

and electronic materials, through

the fabrication of integrated optic

devices, to the development and

evaluation of new measurement

systems. Materials are grown by

chemical beam epitaxy, chemical

vapor deposition, and sputtering.

Devices are created with optical

and electron-beam lithography.

The measurement systems may

incorporate new, in-house

microstructures or an assembly of commercially available components. This research results in

publication of new technology and

measurement procedures and

calibration services to support the

laser and optical communications

industries.

CONTACT: Aaron A. Sanders

Div. 814.02

Boulder, Colo. 80303

(303) 497-5341

LOW-TEMPERATURE

ELECTRONICS

Cryogenic, and especially superconducting, electronics provide

remarkably high speed and sensitivity, coupled with exceptionally

low-power dissipation. NIST has

a complete facility for fabricating

superconducting integrated circuits from conventional lowtemperature superconductors and

is developing a similar capability

for high-temperature ceramic

superconductors.

NIST research spans a range

from very basic studies of ultra- small tunnel junctions to a super- conducting series array voltage

standard in operation at more

than two dozen laboratories

around the world. The work has established numerous world perfor- mance records over the years with

such devices as analog-to-digital

converters, samplers, electrometers, microwave and infrared

detectors, lithographed antennas,

and magnetic flux detectors using

SQUIDS. NIST efforts support

private industry through cooperative research and assistance with

measurement techniques.

CONTACT: Richard E. Harris

Div. 814.03

Boulder, Colo. 80303

(303) 497-3776

19 ELECTRONICS AND ELECTRICAL ENGINEERING
RESEARCH

FACILITIES

SEMICONDUCTOR

PROCESSING RESEARCH

LABORATORY

As integrated circuit sizes increase

to more than 1 cm^ and feature

sizes within the circuits decrease

to less than 1 |im, critical demands are placed on the meas- urement capability required to

control and monitor their fabrication successfully. To meet the demand, NIST researchers are

developing state-of-the-art meas- urement procedures for

microelectronics manufacturing.

The semiconductor processing

research laboratory provides a

quality physical environment for a broad variety of research in semiconductor microelectronics as well

as in other areas of physics,

chemistry, and materials research. The laboratory facilities are used

for projects addressing many areas

of semiconductor materials and

processes, including process control and metrology, materials characterization, and the use of

integrated circuit materials and

processes for novel applications.

The laboratory complex occupies about 372 square meters,

approximately half of which is composed of clean rooms. Within

the clean rooms, work areas are maintained at class 10 or better. The facility is designed so that the work areas can be easily modified

to accommodate the frequent

equipment and other changes required by research.

CAPABILITIES: The laboratory

has a complete capability for integrated circuit fabrication. Principal processing and analytical

equipment are listed below. The

capabilities are expanded and improved continuously to meet the

technological challenges.

Diffusion, Oxidation, and Annealing. Six furnace tubes for up

to 75-mm-diameter wafers and

nine tubes for up to 100-mmdiameter wafers.

Photolithography. Research

mask aligner (proximity and contact) for wafers up to 100 mm in diameter and irregularly shaped

samples and lOx direct-step-on

wafer system for 75-mm-diameter

wafers. Photoresist spin coating

and developing and related chemical processing, including oxygen

plasma stripping.

Film Deposition. Low-pressure

chemical vapor deposition systems

for depositing silicon nitride,

polysilicon, and low-temperature

silicon dioxide. Rf and dc vacuum

sputtering of metals and dielectrics. Electron beam and hot fila- ment vacuum evaporation of

metals.

Etching. Wet and dry etching

processes. Reactive ion beam

etcher capable of ion milling and

chemical etching with gases such

as freon, sulfur hexafluoride,

oxygen, and chlorine. Ion Implantation. Multipurpose

200-KeV ion implanter.

Analytical Measurements. Thinfilm reflectometry and other thickness measurements, optical

microscopy, and grooving and

staining. Automated and manual

probe stations for current-voltage

measurements and capacitance

measurements as a function of

voltage, frequency, and time.

APPLICATIONS: Small quantities

of specialized semiconductor test

specimens, experimental samples,

prototype devices, and processed

materials can be produced. The

processes and processing equipment can be monitored during

operation to study the process chemistry and physics. The effects

of variations in operating conditions and process gases and chemical purities can be investigated.

Research is performed under wellcontrolled conditions.

Because the work is of a research nature, the laboratory is not designed to produce largescale integrated circuits or similar

complex structures. The breadth

and flexibility of the laboratory is

primarily to support the varied

types of projects performed.

Currently, active research

projects address many aspects of

microelectronic processing steps and materials as well as silicon micro-machining. Examples

include: metal-oxide-semiconductor measurements; metalsemiconductor specific contact

resistivity; uniformity of resistivity,

ion implanted dopant density, surface potential, and interface state

density; characterization of

deposited insulating films on

silicon carbide; ionization and activation of ion-implanted species

in semiconductors as a function of

Below. Schematic of the

Semiconductor Processing

Research Laboratory. Right.

At the NIST High-Voltage

Measurement Facility, re- searchers study how electrical equipment and insulation materials perform if subjected to power surges

or struck by lightning.

\ fe^G^ > I ---A^^Q^J^t H

20
annealing temperature; electrical techniques for dopant profiling

and leakage current measurements; and processing effects on

silicon-on-insulator materials. A

simple CMOS process has been

established.

AVAILABILITY: Laboratory staff welcome collaborative research

projects consistent with the

research goals of the NIST semiconductor program. Work is per- formed in cooperation with the

technical staff of the laboratory.

The most productive arrange- ment begins with the development

of a research plan with specific

goals. The commitment of knowledgeable researchers to work

closely with NIST staff and the provision of equipment and other

needed resources are required. Because hazardous materials are

present, laboratory staff must

supervise all research activities.

CONTACT: Donald B. Novotny

B3 10 Technology

(301) 975-2699

HIGH-VOLTAGE

MEASUREMENT FACILITY

NIST maintains a high-voltage

measurement facility in which researchers develop and evaluate the measurement techniques needed

for the efficient, reliable transmission and distribution of electric power (including for defense purposes). Major programs now being

pursued using this facility are the measurement of transient voltages and currents; the development of techniques to quantify

pre-breakdown and breakdown

phenomena in liquid and gaseous

dielectrics; and the measurement

of low-frequency electric and magnetic fields.

CAPABILITIES: With existing

power sources, direct voltages of

300 kV, 60-Hz alternating voltages

of 175 kV, and standard lightning

impulses of 500 kV can be

produced. Selected waveforms,

such as microsecond duration

trapezoidal waveforms up to 300 kV and gated 60-Hz

waveforms up to 100 kV, are also

available. Supporting equipment

includes high-voltage standard

capacitors rated at 200 kV; highaccuracy, current-comparator

bridges for 60-Hz measurements; a

precision dc divider rated at 200

kV; dividers to measure standard

lightning impulses up to 1-MV

peak; partial discharge measure- ment systems; high-speed camercus and supporting optical equipment

(including an image-preserving

optical delay); a computercontrolled system to measure the

electric field in transformer oil; a gas-chromatograph/massspectrometer system; and a system

to produce a known electric field and current density in air at at- mospheric pressure. Measurement systems are available to measure pulsed voltages

and currents with characteristic

times ranging from nanoseconds

to milliseconds. These systems include Rogowski coils and capacitive probes as well as the necessary

recording equipment to acquire

and store digital records. These

conventional measurement sys- tems are supplemented by optical

sensors and couplers.

APPLICATIONS:

Instrumentation and Component Evaluation. Impulse, ac, and dc dividers; electric and magnetic field meters; capacitors;

transformers; lightning arresters; and ion counters.

Dielectrics Research and

Development. Chemical degradation studies; measurement of the fundamental processes of dis- charge initiation; onset and magnitude of partial discharges; space

charge measurement; and

streamer propagation studies.

AVAILABILITY: The high-voltage

facility is used by NIST staff and

by guest researchers from industry,

universities, and other federal

agencies. Use of the facilities must

be scheduled in advance. Because

of the complexity of the system,

typical use of the facility is in the form of a collaborative investigation with NIST staff.

CONTACT: William E, Anderson

B344 Metrology

(301) 975-2403

21 ELECTRONICS AND ELECTRICAL ENGINEERING
RESEARCH FACILITIES

liPiii

planar technique is the most popular. Efficient computer programs

are available for processing the

large quantities of data required.

When operated in the planar

mode, the facility is capable of measuring over a 4.5-m x 4.5-m

area with probe position errors of

less than ±0.01 cm. Improved position accuracy is possible with further alignment, especially over

smaller areas. Antennas with apertures up to about 3 ni in diameter can be measured with a single

scan. The facility has been used

successfully over the frequency

range 750 MHz to 75 GHz. It incorporates provisions for scanning

larger antennas in segments.

APPLICATIONS:

Antenna Characteristics. The

facility is used primarily for deter- mining the gain, pattern, and

polarization of antennas. Accuracies are typically ±0.15 dB for

absolute gain and ±0.10 dB/dB for

polarization axial ratio. Patterns can be obtained down to the -50 dB to -60 dB levels with side

lobe accuracy typically about

±1.0 dB at the 40-dB level. (The

exact uncertainties depend on the

frequency, type, size of antenna,

and other factors.) Near-field data

also can be used to compute nearfield interactions (such as mutual

coupling) of antennas and

radiated field distributions in the near zone. Antenna Diagnostics. Near-field scanning is also a valuable tool

for identifying problems and for achieving optimal performance of

various types of antenna systems.

It has been used to advantage in

locating faulty elements in phased

array antennas and for adjusting

feed systems to obtain the proper

illumination function at the main

reflector. Phase contour plots of

the near-field data also can be

used to determine surface imperfections in reflectors used for antennas or compact ranges. Probe Calibrations. A spherical

probe calibration facility is used

as a far-field range for measuring

the receiving characteristics of

probes used to obtain near-field

data. These measurements are required to determine the probe coefficients, which, in turn, are used

to calculate accurate, probecorrected, far-field gain and pattern characteristics of an antenna.

AVAILABILITY: Two kinds of ar- rangements can be made to use

this facility. NIST staff can per- form specified tests or measure- ments on a reimbursable basis. In

this case, the customer has no

direct use of the facility; all measurements are performed by NIST

staff and the customer is issued a

test report. As an alternative, work

may be performed on a cooperative basis with NIST staff. This ar- rangement permits the user the advantage of developing firsthand

knowledge of the measurement

processes, and the user is responsible in large part for the accuracy

of test results. In either case, arrangements need to be made

well in advance, and reimbursement is required for the facility

use and time of NIST staff

involved.

CONTACT: Allen C. Newell

Div. 813.05

Boulder, Colo. 80303

(303) 497-3743

GROUND SCREEN

ANTENNA RANGE

The ground screen antenna range

is an open area test site.

CAPABILITIES: The ground screen

consists of 6.35-mm mesh galvanized hardware cloth stretched

over a level concrete slab. The

screen is 30.5 m wide x 6l m long

and is spring-loaded around the

perimeter to ensure uniform tension, a flat surface, and adequate

compensation for thermal expansion. The overall size of the ground screen permits far-field measurements in the highfrequency portion of the spectrum,

and the mesh dimension provides

for an efficient ground plane well

into the ultrahigh frequency

region.

APPLICATIONS: The range can be

used for the following:

antenna calibrations; antenna patterns at any

polarization;

electromagnetic susceptibility measurements;

electromagnetic radiated emission measurements;

calibration of field intensity

meters; and

wave propagation studies in fre- quency or time domains.

AVAILABILITY: This facility is used heavily in performing calibrations for industry and other

government agencies. The

facilities are available for independent or collaborative work.

CONTACT: Motohisa Kanda

Div. 813.03

Boulder, Colo. 80303

(303) 497-5320

MODE-STIRRED

CHAMBERS

NIST researchers have designed

and constructed mode-stirred

(reverberating) chambers to measure radiated electromagnetic

emissions and susceptibility of

electronic equipment and shielding effectiveness of materials and

cable/connector assemblies. A

mode-stirred chamber is an electrically large (in terms of wavelength), high-quality cavity whose

boundary conditions are varied by means of a rotating conductive

tuner or stirrer. The time-averaged

field inside such a cavity, when a

sufficient number of modes are excited, is formed by uniformly distributed plane waves coming from

all directions. This causes the

polarization of the field to vary randomly, hence eliminating the need for, or the utility of, physical

rotation of test objects in the field. A microwave oven is a simple ex- ample of a mode-stirred chamber

without measurement support instrumentation.

CAPABILITIES: The mode-stirred

chamber simulates near-field conditions for tests at frequencies

from 200 MHz to 40 GHz. Highlevel test fields (up to 1000 V/m)

can be generated efficiently over a

large test volume in the chamber,

or the chamber can be used to measure low-level radiated emissions (total radiated power down

NEAR-FIELD SCANNING

FACILITY FOR ANTENNA

MEASUREMENTS

The automated facility is designed

to measure the near-zone phase

and amplitude distributions of the

fields radiated from an antenna

under test. Mathematical transfor- mations are used to calculate the

desired antenna characteristics.

CAPABILITIES: Near-field data can

be obtained over planar, cylindrical, and spherical surfaces; the

22
to -100 dBm) from equipment

under test with minor instrumentation changes. Equipment as large

as 1.5 m X 2.0 m X 3.0 m can be

tested.

APPLICATIONS: In addition to per- forming radiated emission or susceptibility measurements of

electronic equipment, the modestirred chambers can measure the

shielding effectiveness of gasketing, composites, and other materials used for radio frequency

shielding applications. The chambers also can be used to measure

the shielding effectiveness of

wiring harnesses and electrical

cables, connectors, and assemblies.

LIMITATIONS: The usable lower

frequency is limited by insufficient mode density, tuner effectiveness,

and ability to uniformly excite all modes in the chamber. These

factors are a function of both

chamber geometry and size. Measurement uncertainties vary from

±10 dB at 200 MHz decreasing to ±4 dB from approximately

1.0 GHz to 18 GHz. Directional

characteristics of an antenna or

test equipment placed inside a

mode-stirred chamber are lost,

resulting in the need to estimate

their free-space maximum gain as

a function of frequency in order to

correlate results obtained by openfield tests. However, tests can be

performed cost effectively in a

shielded environment, with sufficient accuracy to make these

facilities veiy attractive for diagnostic testing and for minimizing

the need for expensive testing in

facilities such as anechoic

chambers.

AVAILABILITY: Two mode-stirred

chambers are available: one that

is 2.74 m x 3.05 m x 4.57 m and

a smaller version, l.l6mx 1.425 m X 1.47 m. NIST staff are available for collaborative programs or

to advise and interpret measure- ment results. Independent testing

also can be arranged.

CONTACT: Motohisa Kanda

Div. 813.03

Boulder, Colo. 80303

(303) 497-5320

TRANSVERSE

ELECTROMAGNETIC

CELLS

NIST researchers have designed

and constructed several transverse

electromagnetic (TEM) cells that

are available for use. A TEM cell is

a device for performing radiated

electromagnetic emission and susceptibility measurements of

electronic equipment. Its design is

based on the concept of an ex- panded transmission line operated

in a TEM mode. The cell is a two- conductor system with the region

between the inner and outer conductors used as the test zone. The

tapered sections at both ends are

required to match the cell to

standard 50 Q coaxial-cable

connectors.

CAPABILITIES: The cell provides a

shielded environment for testing

without introducing multiple

reflections experienced with the

conventional shielded enclosure.

It simulates very closely a planar

far field in free space and has constant amplitude and linear phase

characteristics. The external

electromagnetic signals will not affect the measurement of low-level

radiated emission from the device

under test. The high-level test field

generated inside a cell for radiated

susceptibility tests will not interfere with external electronic

systems.

APPLICATIONS: In addition to

radiated electromagnetic compatibility/interference testing,

other applications of the TEM cells

include the calibration of anten- nas and the study of biological effects of radio-frequency radiation.

LIMITATIONS: The usable fre- quency range is limited by an

upper bound determined by the ap- pearance of the lowest high-order

mode. The volume available for

testing purposes is inversely

proportional to this upper frequency limit. The size of the device to

be placed inside a TEM cell for testing should be small relative to the

available test volume in order that

the field structure associated with

the ideal TEM mode existing in an empty cell not be significantly

perturbed.

AVAILABILITY: Several TEM cells

with five different sizes and five upper frequency limits in the range 100 MHz to 1 GHz are available. In collaborative programs,

NIST staff are available to advise

and interpret measurement

results. Independent testing also can be arranged.

CONTACT: Motohisa Kanda

Div. 813.03

Boulder, Colo. 80303

(303) 497-5320

ELECTROMAGNETIC

ANECHOIC CHAMBER

The electromagnetic (EM)

anechoic chamber at NIST is a

facility for generating standard

(known) electromagnetic fields. Such fields are fundamental to the

research, development, and evaluation of antennas, field probes, and

EM material properties.

CAPABILITIES: EM fields up to

100 V/m can be established in the chamber over the broad frequency

range from 200 MHz to 18 GHz,

and up to 200 V/m for certain fre- quency bands above 1 GHz. A

majority of the individual systems

composing the measurement sys- tem are under computer control,

thus enhancing statistical control

of the measurements. Work is under way to extend the frequency

range to 40 GHz and to improve

the computer control of the chamber systems. The chamber dimensions are 8.5 m x 6.7 m x 4.9 m.

APPLICATIONS: The EM chamber

is used in areas such as:

research, development, and

evaluation of new EM-fieldgeneration and measurement

methods;

antenna and field-probe

development and evaluation;

calibration of field measure- ment instruments;

susceptibility testing of

electronic equipment;

shielding effectiveness and material parameter studies; and

special tests for government

agencies, industry, and

universities.

AVAILABILITY: This facility is

used heavily in performing calibrations for industry and other

government agencies. The

facilities are available for independent or collaborative work with

NIST.

CONTACT: Motohisa Kanda

Div. 813.03

Boulder, Colo. 80303

(.^03) 497-5320

23 ELECTRONICS AND ELECTRICAL ENGINEERING
MANUFACTURING

ENGINEERING

LABORATORY

NISI engineers and scientists are developing many of the

essential elements of automated intelligent processing

systems tliat will soon be at the core of all world-class

manufacturing operations. These components include

robotics; advanced sensors for real-time in-process measurements; software for precision control of machine tools;

and information technology for integrating all elements of a product's life cycle, from planning and design through

marketing and customer support. Building on its in-house

research and development, the laboratory provides technical support for industry groups that are developing standards for measurements, measurement techniques,

hardware, software, and data interfaces.

Two projects illustrate the broad scope of the laboratory's

research activities. In one major initiative, staff members

are refining the laboratory-designed and -built molecular

measuring machine for precision engineering. Intended

to support the fabrication and characterization of future

generations of integrated circuits and other "nanotechnologies," the instrument will be able to measure

atomic and molecular structures over an area of 25 square

centimeters.

In NIST's "Shop of the 90s," technical experts from the

Institute are helping small metal fabrication plants modernize their operations. The majority of the nation's

125,000 job shops, which turn out 75 percent of the fabricated metal parts used in construction and manufacturing, use decades-old technology. To help these companies

become more efficient and competitive without incurring

prohibitively high expenses, the "Shop of the 90s" uses

off-the-shelf computer technology to help integrate and

automate manufacturing and other business operations.

Technology transfer is part and parcel of the Manufacturing Engineering Laboratory's activities. In their

laboratories, at the Automated Manufacturing Research

Facility, and on the floors of U.S. manufacturing plants,

the Manufacturing Engineering Laboratory staff work

closely with their counterparts from industry.

Contact: John A. Simpson

B322 Metrology

(301) 975-3400

COOPERATIVE

RESEARCH

OPPORTUNITIES

PRECISION

ENGINEERING

ATOMIC-SCALE

MEASURING MACHINE

By the year 2001, uncertainty

requirements for dimensional

metrology of step heights, surface

roughness, linewidth, and line

spacing for the integrated circuit and optics industries will be

0.1 nm to 1 nm. Furthermore,

these uncertainties must be held

over areas ranging from several

square millimeters to fractions of

a square meter. To address these

needs, NIST is building the molecular measuring machine

(M^). will be capable of

positioning and measuring to

atomic-scale accuracies over an

area of 25 cml It incorporates a scanning tunneling microscope

into a unique system design that

includes a very stiff core structure,

carriages for moving the probe

over the sample, interferometry for measuring probe and sample position, and two stages of isolation from seismic and acoustic perturbations. Construction and testing

are under way.

After construction is completed, will serve as an independent means for characterizing

distances, geometries, and distortions of highly ordered arrange- ments of atoms on single-crystal

surfaces. also will serve as an

exploratory tool for building

mechanical and electrical structures in the nanometer-size range. Among the organizations collaborating on the construction

of are several major universities and national laboratories, as

well as Watson Research Center,

AT&T Bell Laboratories, and Zygo

Corp.

CONTACT: Clayton E. Teague

A117 Metrology

(301) 975-3490

ADVANCED OPTICAL

SYSTEMS

Advanced optical systems increasingly are designed around highaccuracy, aspheric optical

elements. Measuring the figure

error of generalized aspheres to

the required accuracy is a complex

and unsolved problem. NIST is embarking on a program to characterize the systematic errors of commercial, phase-measuring interferometers used for surface figure metrology and to develop

techniques to use these instru- ments for aspheric metrology. The

goal of the program is to close the

gap between the resolution and

the accuracy of phase-measuring

interferometers. NIST researchers

are working with personnel at

Within the spherical copper

frame of the molecular

measuring machine, NIST

scientists plan to use a scanning tunneling microscope and lasers to measure the positions of

individual atoms over distances hundreds of millions

of atoms wide.

24
Wyko Corp. and Zygo Corp., which

manufacture these interferoraetry

systems.

NIST researchers already have

demonstrated a significant sensitivity to fringe density of the measured figure error for several commercial phase-measuring

interferometer systems. They are working to build a dedicated test

facility for future systematic

investigations. The results of this work will make it possible to manufacture lightweight, highperformance optical systems for space-based applications and

multilayer mirror systems for

projection X-ray lithography.

CONTACT: Tyler W. Estler A107 Metrology

(301) 975-3482

MEASURING

PATTERNED LAYERS ON

INTEGRATED CIRCUITS

NIST researchers are developing

techniques for measuring the critical dimensions of patterned layers on integrated circuits. The work involves theoretical projects on the formation of images in the optical

and scanning electron microscopes, as well as experimental

and design projects on the construction of new metrology instru- ments for the calibration of

standards. The project was initiated about 15 years ago at the request of the semiconductor

industry.

The ever-smaller dimensions on integrated circuits have created

a demand for new and improved

techniques of measurement and

their related standards, especially

as feature sizes approach and be- come smaller than the wavelength

of light used in conventional optical metrology instruments. The

dimensions of present interest

range from about 0.5 |im to 30 jim and will extend to smaller

dimensions in the future. A series

of three linewidth/pitch Standard

Reference Materials for photomasks are presently in production.

Research is in progress to develop new and improved standards for use in instruments utilizing

optical or scanning electron microscopy.

CONTACT: Robert D. Larrabee

A347 Technology

(301) 975-2298

VISION-BASED

MEASURING SYSTEMS

NIST has extended its study of

coordinate measuring machines

to equipment with computer

vision sensors. The use of video

sensors is a much more complicated process than the traditional

touch-trigger probes. Much work

remains to be done to develop

suitable standards for characterizing the performance of these

types of measurement systems.

Even procurement is a problem if

there is no standard way to specify,

characterize, and test the accuracy

of the equipment. The goal is to produce a knowledge base that can be used to develop standardized methods for both testing

and using vision-based measuring

machines.

NIST researchers currently are

using a Precis 3000 vision-based

measuring machine on loan from

View Engineering of Simi Valley,

Calif. It is being used to test different methods for characterizing

the precision and accuracy of

vision-based measuring systems.

NIST researchers are introducing

the concept of error enhancement

into video-based coordinate

measuring systems. NIST

pioneered this technique, and it

has been used with touch-trigger

and analog probes for several

years. The NIST researchers are active members of standards committees

for dimensional measurement and

will use the results of these studies

to assist the committees in developing appropriate standards and

guidelines.

CONTACT: Theodore D. Doiron

A107 Metrology

(301) 975-3472

MEASURING SURFACE

ROUGHNESS

The need for effective, on-line control of surface texture is increasing. In fact, many U.S. automobile

companies are beginning to see superior coatings as a potential competitive advantage over foreign

competition. One of the keys to achieving this advantage is better

on-line surface measurement

methods. NIST is using contacting

and optical profiling techniques

as well as optical scattering to

develop such methods (which will

be sensitive to the functionality of

the components). The researchers

already have used an experimental light-scattering instrument

and a long-range scanning tunneling microscope to generate accurate descriptions of light scattering from rough metal parts and

from glossy paper. They currently

are studying the effects of using a

light-scattering system to inspect

glossy paper during manufacturing. The researchers plan to

adapt this system for other materials and manufacturing processes. They also intend to build a

remotely controlled profiling

instrument.

These advances will provide

a better understanding of the

relationship between process parameters and surface finish. NIST researchers currently are working closely with academia,

the automotive and painting

industries, and standards

committees.

CONTACT: Theodore Vorburger

A117 Metrology

(301) 975-3493

CAD-DIRECTED

INSPECTION

NIST researchers are implementing a CAD-directed inspection sys- tem for manufactured parts that

utilizes the ANSI/CAM-I Dimensional Measuring Interface Stan- dard (DMIS) and the Initial Graphics Exchange Specification.

The goal is to produce a closedloop, integrated inspection system

completely from commercially

available products. Six companies

have loaned products to NIST to

be used in this project. They are Automation Software, CADKEY

Inc., CMX Systems Inc., ICAMP

Inc., Renishaw Inc., and Sheffield Measurement.

NIST researchers already have

built the first prototype of such a system for simple parts on a single

personal computer platform. Currently, the inspection plan is input

manually using a mouse. Research continues in several areas: expanding probing capabilities,

adding more complex part inspections, expanding and refining

DMIS, and automating the actual

inspection planning. The research

results of this project are being

used to iissist tiie committees

ANSI/CAM-I DMIS, ANSI/ASME

B89.3, and ANSI/ASME B89.4—in

the development of the appropriate standards and guide25
COOPERATIVE RESEARCH OPPORTUNITIES

lines. NIST researchers also are working with the University of North Carolina-Charlotte to make

use of process information in

developing the inspection plan.

CONTACT: David C. Stieren A107 Metrology

(301) 975-3197

AUTOMATED

PRODUCTION

TECHNOLOGY

QUALITY IN AUTOMATION

PROGRAM

This program is an effort to

achieve higher part accuracy from

existing discrete-parts manufacturing equipment. A four-layer,

closed-loop, control architecture

has been proposed. Three layers

are being implemented: real-time

(RT), process-intermittent (PI),

and post-process (PP) control

loops. The RT and PI loops implement algorithms to predict and/or measure machine- and processrelated systematic errors and compensate for them via real-time tool path modification and NC pro- gram modification. The PP loop is

used to verify the cutting process and to tune the other two control

loops by detecting residual systematic errors measured on the

finished parts, correlating these

errors to the uncompensated

machine- and process-related

errors, and modifying the control parameters of the other loops

accordingly.

Feature-based error analysis

techniques are being developed

to identify the residual systematic

errors of the system. NIST researchers are working with industry and academia to use DMIS-defined features in their

analyses. They are developing

tools for feature segmentation of any computer-aided design for manufacture and analysis point of

view. They are also developing a

quality database using feature

types and the errors measured on

these features as key fields.

CONTACT: M. Alkan Donmez

BIO6 Sound

(301) 975-6618

MACHiNE-TOOL

PERFORMANCE

EVALUATION AND

ACCURACY ENHANCEMENT

Deterministic manufacturing is a

concept based on the premise that most errors in manufacturing are

repeatable, thus predictable.

Errors that are predictable can be

measured and corrected, thereby

improving quality through better

control of the existing manufacturing equipment. Machine tools

are computer-controlled, multidegree-of-freedom structures that have inherent quasistatic and ther- mally induced geometric errors. Complete characterization of these

errors is being investigated to

evaluate and enhance perfor- mance under changing thermal

conditions. This process is complicated and time consuming.

NIST researchers are working

with industry and academia to

optimize this process to make it

feasible for even small manufacturers. NIST, industry, and

academia worked together to

develop the industry standard for machining center performance

evaluation (ASME B5.54). Compensation of machine-tool errors

is an area of continuing interest.

Researchers are developing

generic electronic hardware to implement error compensation

without any intrusion into the existing machine-tool controllers. They also are working to speed up

the on-machine part inspection by

introducing fast probing and

powerful data analysis capability

at the machine-tool level.

CONTACT: M. Alkan Donmez

BIO6 Sound

(301) 975-6618

Mechanical engineer

Nicholas Dagalal(is monitors

the performance of the Advanced Deburring and Chamfering System, an industrial

robot and cutting tool that

produces beveled edges in metals, such as titanium, at high speeds.

PORTSMOUTH

WORKSTATION

The Fastener Quality Act, Public

Law 101-592, recently passed by

Congress, requires the inspection

and certification of industrial

fasteners used in critical applications. The fabrication of hightolerance fasteners, such as hex

head bolts, screws, and studs, is

critical to the maintenance of submarines. With tolerances as small

as 12.7 |J.m, these fasteners often

require frequent inspection at

various stages of production. In

addition, they are typically made

in small lots from hard-to-cut materials such as k-monel. These

three facts—tight tolerances,

small lots, and exotic materials

make them difficult and costly to

procure. NIST is working with personnel

from the Portsmouth Naval Shipyard and several private companies to build an advanced,

computer-controlled, machining

workstation capable of automatically manufacturing, inspecting,

and engraving these fasteners. The

hardware and software have been

integrated, and the first certified

parts have been produced. Two

techniques pioneered at NIST,

error compensation and in-process

control, are now being incorporated. In addition, NIST researchers expect to develop new

statistical process control techniques to be used in this and other

26
small batch production environ- ments. This will maximize the production rate and minimize

scrap.

CONTACT: Kang Lee B106 Sound

(301) 975-6602

ROBOT SYSTEMS

INTELLIGENT MACHINE

CONTROLS

The concept of advanced realtime, sensory-based control of machines has been a goal of researchers and system developers

for over a decade. However, the

lack of a structured, theoretical ap- proach for designing and developing such systems has severely

limited the number and sophistication of applications seen in operation today. Based on years of

research and development in realtime, sensory control of robots and

manufacturing systems, NIST is conducting the research necessary

to develop a standardized architecture for implementing intelligent

machine control. This architecture has been adopted by such

organizations as the National

Aeronautics and Space Administration and the U.S. Air Force.

NIST's current research seeks

to expand and document a formal

mathematical theory for the control of intelligent machines and to

verify these theories using testbeds

involving both simulation and

actual controller hardware. Advanced control concepts, involving

planning, sensory processing,

world modeling, and knowledge

representation, are being investigated. Several independent

development projects are under

way to demonstrate implementations of these control principles on

functioning machines. They involve automated manufacturing,

robotic deburring, space robotics,

construction, remotely operated

land vehicles, underground mining, and undersea vehicles.

CONTACT: James S. Albus

8124 Metrology

(301) 975-3418

mm mum

SENSORY PROCESSING

AND WORLD MODELING

FOR INTELLIGENT CONTROL

Intelligent control of machines

requires a detailed knowledge of

both the machine and its operating environment. Since these are both dynamic in nature, it is

necessary to measure, analyze,

and comprehend changes in real

time to achieve intelligent, sensorybased control of machines. NIST

has a number of projects focused on developing advanced sensory

processing and world modeling

capabilities. Sensory processing research includes work on specialized vision systems, real-time

image processing, and sensor data

fusion. Vision systems being investigated include non-uniform

resolution, active scanning of the

fovea over points of interest, and

active control of multiple cameras. Under investigation are imageprocessing techniques for obtaining dense range maps from image

flow and from stereo images.

World modeling research is concentrating on data structures that can represent both spatial and

symbolic information about surfaces, objects, and regions of

space. Methods are being

developed for comparing world

model and sensory data so that one could, for example, generate a map overlay that is registered with

and tracks camera images in real

time. Also being developed are Kalman filtering techniques for updating the world model based

upon sensory data.

CONTACT: Ernest W. Kent B124 Metrology

(301) 975-3418

OFF-LINE PROGRAMMING

OF ROBOTIC SYSTEMS

Off-line programming (OLP) sys- tems are used to generate robot programs without the use of the

actual robot. OLP has two advanThis computerized turning

workstation operated by

numerical control programmer Richard Beaulieu (left)

of the Portsmouth Naval

Shipyard and NIST mechanical engineer Mahn Hee

Hahn can produce precision

machined fasteners in less

than one-tenth the time re- quired with conventional

equipment.

tages over the traditional teachingdependant programming method:

It improves safety because the

robot is not run and robot/

operator interactions are reduced,

and the system downtime is reduced because the robot is not

involved in developing and debugging programs. But most commercially available OLP systems rarely

produce the final robot control programs.

Research at NIST has focused on the use of OLP to generate

directly robot control programs to determine robot trajectories for

part handling and deburring.

Since the models of the robot and

the workstation layout never exactly match the actual equipment,

there can be significant errors be- tween the OLP-generated robot

positions and the actual points

through which the robot will move. To compensate for this, NIST has developed several sensor- based approaches for automatically calibrating or registering

the OLP model of the robot and

workstation with the real systems.

This permits automatic generation

of reliable robot programs in a

matter of seconds or minutes instead of the hours or days required

for manual teaching.

CONTACT: Ronald Lumia

B 127 Metrology

(301) 975-3452

ROBOT METROLOGY

The characterization of the perfor- mance of a robotic system is important in understanding the

limitations of the system and in optimizing its operation. Although

several U.S. and international standards committees are working on

27 MANUFACTURING ENGINEERING
COOPERATIVE RESEARCH OPPORTUNITIES

measuring robot performance, no

standard robot acceptance and

characterization tests currently

exist. Research is ongoing at NIST

to develop and validate standard

test procedures for measuring

robot performance. NIST has been

working closely with the Robot Industries Association subcommittee on developing such tests.

Currently, a laser tracking

interferometer system, originally

designed and developed by NIST

and now available commercially,

is used to make these measurements. This system provides very

accurate position measurements

of 1 to 2 parts in 100,000 and an

angular accuracy of 1 to 2 seconds

of arc. Also under development is

a low-cost robot calibration sys- tem that consists of a series of

string encoders mounted to a fixture. This system provides a

relatively inexpensive robot

calibration system with an ac- curacy of ±0.127 cm. Currently,

research is being conducted to

characterize the performance of

this system and to expand its

capabilities from being able to measure three degrees-of-freedom

to a full six degrees-of-freedom.

CONTACT: Kenneth R. Goodwin

B124 Metrology

(301) 975-3421

MOBILE ROBOTIC

SYSTEMS

Current applications of robotic sys- tems are typically limited to industrial operations such as part

handling, assembly, welding, and

painting. A number of applications are being investigated by the

research community that place a

different emphasis on the requirements for a mobile robotic

system.

The U.S. Olympic speedskiing team races at speeds

of up to 190 km/li using a

special computer-designed

lielmet produced tlirougli a

cooperative project involving NIST researchers, Bell

Helmets, and several other

industrial partners.

NIST has been conducting a

joint research program with the

U.S. Army on the development of a mobile robotic platform for

military applications. NIST is involved in specifying the basic control system architecture for the mobile vehicles. This control sys- tem handles mobility functions on

the vehicle—both teleoperation

and autonomous-subsystem integration—and communication with the remote operator station.NIST has demonstrated remote

operation of the vehicle over an rf

radio link and "retro-traverse"

an autonomous operation where

the vehicle retraces a previously

traveled path based upon data

from an onboard inertial navigation system (INS). Other research

aspects include video data compression for remote driving, a lowcost INS, and obstacle-detection

sensor systems. The goal is to have

a standard architecture that could

be adopted by the military for all

of its robotics applications,

thereby significantly reducing

integration costs and allowing

subcomponents to be transferred between different robotics systems.

CONTACT: Maris Juberts B 127 Metrology

(301) 975-3422

ROBOTIC DEBURRING

OF MACHINED PARTS

Engineers at NIST are developing an automated system that produces precision chamfers on

aircraft engine components fabricated from titanium and inconel.

The chamfers, or beveled edges,

must be placed on parts such as

turbine engine blades and hubs to

relieve potential areas of stress

concentration and ease assembly.

The system, called the advanced

deburring and chamfering system

(ADACS), consists of a six-axis

electric robot fitted with an actuated chamfering tool. This tool

is capable of high-speed force control within a small work area. The approach is to use the industrial robot as a coarse positioning device, while relying on the

actuators and force sensors of the

tool to provide control of cutting

force and stiffness at the part

edges. The tool also compensates

for robot inaccuracies and other

factors, such as part misalignment and large tolerances. The sys- tem has maintained chamfers of

38 |im on titanium while traversing corners, in spite of part positioning errors on the order of

several millimeters. The ADACS

builds on two techniques

pioneered in the Automated Manufacturing Research Facility: a tech- nique to generate robot trajectories

off-line from CAD data and a tech- nique to integrate a variety of sensors into the robot-control system.

CONTACT: Maris Juberts 31 27 Metrology

(301) 975-3422

COMPOSITE-PART

MANUFACTURING

USING ROBOTIC FIBER

PLACEMENT

The manufacture of highperformance composite parts

remains very time and labor

intensive. NIST has initiated the development of an advanced

manufacturing workstation for the

fabrication of composite parts. The project will apply sensorbased, hierarchically controlled

robotic systems to automated fiber placement of thermoplastic composite materials. In such a system,

continuous, fiber-reinforced thermoplastic polymer is fed from a

spool onto a mandrel or part form.

The orientation of the fiber is

based on the part's geometry and

structural design. As the composite

28
material is applied, it is heated to melt the polymer matrix and then

consolidated in place as it cools. The project will demonstrate

that fiber placement via two

cooperating robot manipulators

and in-situ consolidation can

produce composite parts with complex shapes. Finite-element ther- mal modeling of the process is being conducted to gain insight

into the relationships between the

various process parameters and

other system variables. Sensor sys- tems are integrated into the process to provide necessary feedback

data. The finished parts are inspected using various mechanical

testing and non-destructive evaluation techniques to determine the

relationships between the process parameters and the resulting part

integrity.

CONTACT: Maris Juberts B127 Metrology

(301) 975-3422

FACTORY

AUTOMATlii

SYSTEMS

PRODUCT DATA

EXCHANGE STANDARDS

FOR THE APPAREL

INDUSTRY

Numerous vendors supply computer-aided apparel design and

pattern-making equipment. Each

vendor's equipment represents the

design and pattern data in a unique or proprietary file structure, preventing the direct

electronic exchange of data

among different organizations.

NIST is helping the apparel industry to develop standards for

product data exchange. NIST researchers have developed a

prototype computer program

for translating apparel pattern

data between different file storage

formats. The program demonstrates the feasibility of using a

single, standard, interchange for- mat. The program implements an

information model also developed

at NIST. The software was developed as

part of an ongoing project at NIST

to extend the emerging international Standard for the Exchange

of Product Model Data to apparel

applications. The work is partially

sponsored by the Defense Logistics

Agency and is being carried out in

cooperation with the Computer

Integrated Manufacturing Committee of the American Apparel

Manufacturing Association. In the

short term, the goal is to develop a

neutral data format for exchanging two-dimensional pattern data

between apparel CAD systems. In

the longer term, researchers plan

to develop an information model

that can be used to encompass the

entire apparel life cycle.

CONTACT: Theodore Hopp

A 127 Metrology

(301) 975-3545

INSPECTION AND

TOLERANCES RESEARCH

To establish a unified framework

of U.S. and international standards dealing with mechanical

tolerance issues, NIST scientists

are carrying out a program of research and technology development in inspection and tolerances.

These activities are aimed at

developing a common technical

basis for tolerance standards. The

efforts involve support of the

development of emerging standards on dimensional measure- ment methods, particularly

regarding coordinate measuring

machine (CMM) methods.

The standards of interest include standards for tolerance models, inspection performance,

mathematics of tolerances, and

statistical tolerance methods. Ex- amples of critical emerging and

draft standards are the Standard

for the Exchange of Product Model

Data, the Mathematical Definitions of Dimensions and Tolerances, and Performance Testing of

Coordinate Measuring Machine

Software. The work also involves

participation on standards committees, research on measurement

methods, and interaction with

other government agencies to assess and improve the performance

of CMMs used in their laboratories

and production facilities.

CONTACT: Theodore Hopp

A127 Metrology

(301) 975-3545

NATIONAL

PDES TESTBED

Product data is an integral part of

the information shared across computer applications and organizations. That is, it is a crucial

part of any integration scheme.

Currently, no commercial products exist that allow systems to

share information in a standard

way and, consequently, be integrated together. STEP (the Standard for the Exchange of Product

Model Data), when implemented.

will simplify this integration problem. However, STEP is still in the

definition/testing phase. NIST is

developing the National PDES

Testbed to provide technical

leadership and a testing-based

foundation for the rapid and complete development of STEP. (PDES

stands for "Product Data Ex- change using STEP.")

Major objectives of the testbed

project include: the identification

of computer software applications

that will use STEP, the specification of technical requirements for

these applications, the evaluation

of the proposed STEP standard

with respect to application requirements, the design and implementation of prototype STEP

applications, the establishment of

configuration management for STEP specifications and certain

supporting software, and improved

interactions between organizations working to develop STEP.

CONTACT: Charles R. McLean

A 127 Metrology

(301) 975-3511

MANUFACTURING

SYSTEMS INTEGRATION

Despite years of product development, truly modular, flexible, integrated manufacturing systems

are still not prevalent in U.S. industry. In particular, information

sharing across engineering,

production management, and control systems is still not possible.

Furthermore, no standards specify

the precise interactions among

these systems. To address these

problems, NIST has embarked on

the manufacturing systems integration (MSI) project. The goal

is to build a testbed environment

for conducting integration experiments with a variety of commer29 MANUFACTURING ENGINEERING
COOPERATIVE RESEARCH OPPORTUNITIES

CL^Ai^iNi6?4 Ax'VvMi:^ vei?-fi^:A^ rtx^'i&^oivi^

cial, university, and in-house

software/hardware.

The MSI research team has

designed, and is in the process of implementing, a systems architecture to serve as the foundation for

this experimentation. The MSI architecture is a step in the continuing evolution and refinement of

hierarchical control principles

developed in the NIST Automated

Manufacturing Research Facility.

Ongoing research topics include:

distributed, real-time planning,

scheduling, and control; running

the systems with both real and

animated equipment; separate but

integrated administrative control and task control; information

models for all subsystems; and

production management error

recovery. NIST researchers are working with several major universities, auto companies, aerospace companies, and vendors. Team

members are active in the international standards arena.

CONTACT: Mark E. Luce A127 Metrology

(301) 975-2802

DESIGN RESEARCH

LABORATORY

As automated design becomes more and more prevalent,

researchers are, of necessity,

becoming more interested in the

"process" of design. Furthermore,

the emphasis on concurrent engineering is making this an iterative and integrated process, rather than a one-shot, stand-alone one.

Several research questions remain.

Can software tools be developed to

create and maintain candidate

designs in digital form? Can data

structures for representing and updating the knowledge contained in

these designs be developed? Can

formats for exchanging that

knowledge across manufacturing

functions be devised? To address

these and other interesting questions, NIST is building an engineering design laboratory

equipped with state-of-the-art computers and software. NIST researchers are investigating the issues involved in integrating a variety of commercial and

university "design" tools. They

also have begun a project aimed

at capturing and representing

"design knowledge and intent" in

a manner that is compatible with

the emerging Standard for the Ex- change of Product Model Data. The work currently is focused on

rigid mechanical parts, including

assemblies. NIST researchers are working with several major universities through the Defense Advanced Research Projects Agency.

CONTACT: Mark E. Luce A127 Metrology

(301) 975-2802

ROBOTIC CRANE

TECHNOLOGY

Shipbuilding, aircraft manufacturing, and building construction

operations rely on cranes with a

single cable for lifting heavy

loads. The problem with this ap- proach is that the load is free to

rotate and swing with the slightest

side force. NIST has designed a crane that provides a very stiff

load platform that can be used to

lift heavy loads or as a base for mounting a conventional industrial robot. The design consists

of an equilateral, triangular platform suspended from six wire

cables. By adjusting the length of each cable from independently

controlled winches it is possible to

position the platform accurately.

As long as the cables remain in

tension, this configuration

provides a significant improvement in stiffness and positioning

capability over conventional

cranes.

Schematic of the Automated

Manufacturing Research

Facility.

NIST is building five testbed

systems to investigate the perform- ance of this crane design. These

consist of:

a full-scale model with a

9,072-kg capacity;

a !/4-scale model with a small

industrial robot mounted upside

down on the lower platform; an /^-scale model for performing stiffness, damping, and

stability measurements;

a single-cable, 1-D testbed for

developing real-time control

algorithms; and

a !/4-scale model bridge crane

with a servoed X-Y carriage.

CONTACT: Kenneth R. Goodwin

B124 Metrology

(301) 975-3421

30
RESEARCH

FACILITIES

AUTOMATED

MANUFACTURING

RESEARCH FACILITY

The Automated Manufacturing

Research FaciUty (AMRF) is a major national laboratory for technical work related to interfaces and standards for the next generation of computer-automated

manufacturing. The facility,

begun in 1981, was put into full

operation in 1986. A companion

installation, located in the adjacent instrument shop, serves

as a state-of-the-art production

facility, making use of the best commercially available

technology.

The workstations of the AMRF

are being used in active research

programs by NIST researchers, industrial research associates, guest

researchers, university personnel,

and scientists and engineers from

other government agencies.

CAPABILITIES: The facility currently supports research in machine tool and robot metrology, sensors and sensory processing, robot safety, robot control,

software accuracy enhancement of machine tools, process planning

and data preparation for machine

tools and robots, parts routing and

handling, real-time control of

robots and aggregations of devices, workstation control, cell

control, and materials-handling

control. It is particularly valuable

for studying interfaces between

control modules and among data

users. The AMRF is unique in the

opportunities it provides for studies of an integrated system of significant size.

The facility consists of a tworobot cleaning and deburring

workstation, inspection workstation, vertical machining

workstation, and two special project areas, which are occupied by

applications-oriented projects. Currently in the special projects areas

are an advanced deburring and

chamfering system, which will per- form production deburring of jet engine blades and discs, and an integrated turning workstation,

which machines threaded fasteners from difficult alloys. It will

be sent to the Portsmouth Naval

Shipyard upon completion.

Nearby are a manufacturing

systems integration (MSI) system

and an early-stage composites

manufacturing workstation. Using

the MSI system, researchers continue the study of AMRF control and data architectures, making

use of the shop floor facility for

validation of simulated results.

AVAILABILITY: Due to the nature

of the problems addressed, the AMRF is generally best suited for

research projects of an extended

nature. Most successful work to

date has involved a close working

relationship between NIST and

a collaborator for periods of

6 months to 1 year.

CONTACT: Philip N. Nanzetta B 112 Metrology

(301) 975-3414

ACOUSTIC ANECHOIC

CHAMBER

This facility is used to perform

acoustical measurements under

free-field conditions, usually at moderate to very small sound pressures. These measurements include calibrating the free-field amplitude and phase responses of sound transducers, such as microphones and loudspeakers,

and determining acoustic intensity in well-defined sound fields. The facility is a vibration-isolated shell-within-shell structure.

All interior surfaces of the inner

shell are covered with a sound-absorptive treatment consisting of

custom-designed, triple-density

wedge modules. The chamber

dimensions, measured wedge tip

to wedge tip, are 6.7 m x 10 m x

6.7 m, defining a volume of 450

A wire-mesh floor permits access to instrumentation within the chamber.

Accessories include signal, control, and power lines as well as instrumentation supports on all six

interior surfaces. Air-conditioning

ducts are acoustically treated and

vibration-isolated. Temperature

and humidity within the chamber

are independently controlled by

the heating, ventilating, and airconditioning system (HVAC).

CAPABILITIES: The chamber

provides a highly anechoic sound

field and a veiy small mechanical

ambient noise level. The wedge

modules are designed to absorb

99 percent or more of the normally incident sound energy at frequencies above 45 Hz. If increased

acoustical isolation from the HVAC

system and a uniform temperature

within the chamber are required

simultaneously, the air flow to the chamber interior can be turned off

while controlled air flow continues

between the inner and outer

shells.

APPLICATIONS: The chamber is used to calibrate and to characterize acoustical instruments and

their directionality under freefield conditions at moderate to

very small sound pressures, to measure non-linear distortions,

and to determine self-noise

equivalent free-field sound pressures. The chamber is used for

basic research aimed at developing methods for calibrating

microphones of standard and nonstandard geometries, for calibrating sound intensity probes and

other transducer arrays and instruments, and for determining acoustic intensity.

AVAILABILITY: This facility has

substantial potential for use by researchers in industry, universities,

and other government agencies.

Scheduling arrangements can be

made for collaborative programs

and individual research.

CONTACT: Victor Nedzelnitsky

(301) 975-6638

Edwin D. Burnett

(301) 975-6636

David J. Evans

(301) 975-6637 A 149 Sound

31 MANUFACTURING ENGINEERING
CHEMICAL SCIENCE

AND TECHNOLOGY

LABORATORY

The chemical-manufacturing, energy, health-care, biotechnology, food-processing, and materials-processing

industries all require accurate, high-precision

measurements for characterizing chemicals, controlling

production processes, and monitoring compliance with

health, safety, and environmental regulations. Collectively, firms in these U.S. industries perform about 250 million measurements daily. The Chemical Science and

Technology Laboratory (CSTL) develops the calibration

and measurement standards for a wide range of instruments used in measuring pressure, temperature, gas and

liquid flow rates, leak rates, and humidity. It also

produces Standard Reference Materials and Standard Ref- erence Data needed to achieve ever-lower detection limits

and to improve quality, productivity, and efficiency.

The laboratory maintains the national system of chemical

measurement and coordinates the system with measurement systems of other nations. It provides advisory and re- search services to other government agencies; conducts

basic and applied research in analytical chemistry, biotechnology, chemical engineering, and physical

chemistry; and conducts interdisciplinary research efforts

with other NIST laboratories in these areas.

Recent CSTL projects have explored new chemical

separation and purification methods and automated techniques for preparing protein crystals, DNA fragments, and

other samples essential to determining the three-dimensional atomic structure of biological compounds. Another

major initiative aims to develop reliable computer models

and simulations for studying and describing chemical

processes.

A newly formed consortium of U.S. businesses and

government agencies is developing a prototype automated

analytical chemistry laboratory. The modular system,

which will prepare samples, perform separations, and

assay the resulting compounds, is part of a larger effort to develop industry-wide standards for automated laboratory

equipment.

Contact: Harry S. Hertz

A309 Chemistry

(301)975-3145

COOPERATIVE

RESEARCH

OPPORTUNITIES

BIOTECHNOLOGY

PROTEIN

CHARACTERIZATION

BY TWO-DIMENSIONAL

ELECTROPHORESIS

NIST researchers are using a two- dimensional electrophoresis sys- tem to characterize proteins and

peptides. They are probing the influence of size, shape, and charge on migration characteristics in the

electrophoretic medium. Although

well-defined protein "markers,"

especially of high molecular

weight, are required to allow standardization of polyacrylamide gel

electrophoretic systems, charged

polymeric materials other than

proteins may be considered for markers. Because staining and

detection of such markers is of

special interest, the researchers plan to examine the mechanisms

of silver stains using neutron activation techniques.

Additional studies will be

directed toward understanding the

interactions of proteins with metal

ions.The researchers will use image processing by state-of-theart instrumentation to form meaningful databases. As part of this program, NIST plans to issue wellcharacterized mixtures of proteins

as Standard Reference Materials

that will be used to assess the

abilities of existing and new

electrophoretic techniques to

separate and detect proteins.

CONTACT: Dennis J. Reeder

A353 Chemistry

(301) 975-3128

32
DNA

CHEMISTRY

Working in several areas of DNA

chemistry, NIST scientists are

actively manipulating DNA to produce proteins, developing

methods for measuring DNA

damage on the molecular level, and developing methods for

characterizing DNA, including

profiling.

NIST scientists are developing

experimental methods to measure DNA damage in mammalian cells exposed to free-radical-generating

systems, such as ionizing radiation, elevated oxygen pressure,

redox-cycling drugs, and a number of carcinogenic compounds.

Free radicals produced in-vivo are thought to be mutagenic and carcinogenic. Measurement of DNA

damage at the molecular level in mammalian cells is a prerequisite

to understanding the chemical

mechanisms of damage by free

radicals. Techniques used for measuring DNA damage include

gas chromatography, mass

spectrometry, HPLC, and NMR

spectroscopy.

NIST scientists are working on new methods for DNA profiling,

ranging from developing wellcharacterized DNA fragment standards for restriction fragment

length polymorphisms to performing research for rapid determination of DNA profiles by polymerase

chain reaction amplification and

automated detection of fragments.

In addition, cooperative developResearch chemist Kristy

Richie uses an electrophoresis gel system to

analyze Standard Reference

Materials that will help

improve quality control for

DNA "fingerprinting"

techniques.

ment of STR (short term repeat)

technology and attendant stan- dards is sought.

CONTACT: Dennis J. Reeder

(301) 975-3128

M. Miral Dizdaroglu

(301) 975-2581

A353 Chemistry

RESONANCE

Programs are under way in which

NIST scientists are using nuclear

magnetic resonance (NMR)

spectroscopy to study simple peptides and proteins, aminoglycoside

and macrocyclic antibiotics, carbohydrates, glycoproteins, and DNA.

The studies are facilitated by re- search materials isotopically

labeled with carbon- 13 or

nitrogen- 15, which are prepared

by synthetic or biosynthetic

methods.

The researchers are making

extensive use of two-dimensional

NMR methods, including

homonuclear and heteronuclear

chemical shift correlation and

J-resolved techniques, nuclear

Overhauser measurements in the

rotating frame, and indirect detection. Measurements of chemical

shifts and coupling constants provide information on the structures, stereochemistry, and

conformations of biomolecules.

Determination of nuclear Overhauser effects and relaxation

times allows the imposition of

distance constraints for three- dimensional structure analysis

and characterization of molecular

dynamics, respectively.

In the future, researchers

plan to use three- and fourdimensional NMR techniques to

investigate higher molecular

weight biomolecules. Detailed

knowledge of the three- dimensional structures and conformations of the biomolecules is important to an increased understanding of biochemical reaction

mechanisms, enzyme specificity,

drug-protein/DNA binding, and

molecular-recognition processes.

CONTACT: Bruce Coxon

A353 Chemistry

(301) 975-3135

BIOPROCESS

ENGINEERING

MEASUREMENTS

NIST scientists are actively involved in the development of

theories, measurement methods,

models, and databases for upstream and downstream

bioprocessing.

To accurately measure cell

properties and product amounts

during fermentation for bioreactors—upstream processing

researchers are studying precision

thermodynamic measurements

and the development of sensor

technology. Downstream processing research includes the development of fundamental transport

data and experimental methods

and models for downstream

separation of proteins and other

biomolecules from complex mixtures. Among the methods under

study are aqueous two-phase partitioning systems, chromatography, and electrokinetic demixing technologies.

In the area of biothermodynamics, NIST researchers have

developed accurate and precise

microcalorimeters to measure the

heat released in enzyme-catalyzed

biochemical reactions of interest

to biotechnology. When coupled

with equilibrium measurements,

these measurements enable the

reliable modeling of the thermodynamics of these processes. These

data are used to predict reliably

the efficiency of biochemical

processes outside the normal meas- urement ranges for temperature,

pH, and ionic strength.

Light-scattering studies are being made on biomacromolecular solutions to characterize their transport and

thermodynamic properties. Models

and experimental methods,

needed to obtain the necessary

data, are being developed to characterize aqueous two-phase separation techniques. NIST scientists

are using small-angle neutron

scattering to characterize

chromatographic media in concentrated polymer solutions.

CONTACT: Stanley Abramowitz

A353 Chemistry

(301) 975-2587

ELECTRICAL

MEASUREMENTS IN

BIOREACTORS

Biological cells are known to be

electrically active as demonstrated

by the membrane potential

present in all living cells. To provide fundamental data for sensor development in bioreactors, NIST

researchers are developing meas- urement techniques for observing

electrical activity of cell suspensions. Both linear and non-linear

electrical responses are under investigation. The non-linear properties are especially interesting since

they are expected to originate

from the cell membrane.

33
COOPERATIVE RESEARCH OPPORTUNITIES

Theoretical investigations are

in progress to relate the observed

electrical behavior to the activity

of membrane transport proteins.

The researchers are working to

achieve a better understanding of

the coupling of applied electric

fields to membrane proteins,

which can lead to practical

schemes to influence the activity

of cells. Research areas include

electrical impedance measurements, study of microwave

propagation in cell suspensions,

electrostimulation of membrane

processes, and observation of

electrophoretic mobility with

dynamic light scattering. Additional work is planned to measure

the modulation of fluorescence

from membrane proteins by applied electric fields.

CONTACT: R. DeanAstumian

A353 Chemistry

(301) 975-5951

BIOSENSOR

TECHNOLOGY

Biosensors use a biocomponent for

the rapid, sensitive, and specific

determination of an organic or

biological compound. These devices, which can be utilized for online measurements in real time,

have potential for widespread

use in biomedical, clinical, en- vironmental, and industrial monitoring.

Basic problems associated with

biosensor technologies must be overcome, however, to ensure successful commercialization. NIST

scientists are examining the mechanisms of protein immobilization and stabilization on surfaces. Optical fiber techniques are

being developed for making nonintrusive, rapid and selective measurements. Fluorescence techniques, as well as Raman and

resonance Raman spectroscopy,

are used to determine the characteristics of amino acids, small peptides, and small organic molecules

as an aid to eventually providing

improved sensor specificity and

selectivity. Molecular diffusion,

rotational mobility, complexation,

and photochemical interaction

also are being examined.

NIST scientists are developing

amplification technologies, including liposome-encapsulated

molecules, multi turnover enzyme

reactions, and ion-exchange

polymer-modified electrodes. Such

methods and devices provide the

potential for extremely sensitive

devices.

CONTACT: Howard H. Weetall

A353 Chemistry

(301) 975-2628

CENTER FOR ADVANCED

RESEARCH IN

BIOTECHNOLOGY

At the Center for Advanced Research in Biotechnology (CARB),

jointly established by NIST, the

University of Maryland, and

Montgomery County, Md., researchers study protein structure/function relationships. They

are focusing on the measurement

of protein structure by X-ray crystallography and nuclear magnetic

resonance spectroscopy, and the manipulation of structure by

molecular biological techniques

including site-directed

mutagenesis. Protein modeling,

molecular dynamics, and computational chemistry are used to understand protein structure and

to predict the effects of specific

structural modifications on the

properties of proteins and enzymes. A variety of physical

chemistry methods are used to measure and analyze structural

changes, activities, and thermodynamic behavior of proteins

under investigation. CARB maintains state-of-the-art facilities for

crystallography, NMR spectroscopy, molecular biology, and

physical biochemistry. Its computer facilities include a minisupercomputer, several highresolution graphics workstations,

and access to the NIST Cyber 205

supercomputer.

CONTACT: Gary L. Gilliland

9600 Gudelsky Dr.

Rockville, Md. 20850

(301) 251-2244

34
Top left. Research chemists

Anne Plant and Steven

Choquette Investigate the

optical characteristics of

fluorescent molecules in order to increase the

specificity and sensitivity

of biosensing devices.

Bottom left. Student

Jennifer Schwarz grows

protein crystals at the Center for Advanced Research

in Biotechnology (CARB).

CHEMICAL

ENGINEERING

SEPARATIONS

Separation and purification are

critical steps in the manufacture

of chemical products using exist- ing and emerging process technologies, such as energy

production or environmental

protection. Separation processes

affect both the economies of

production and the fundamental

ability to produce a product of

desired form or purity. NIST is

creating an engineering science

base in membrane-based

separations.

Left. Travis Gallagher,

NIST/National Research

Council post-doctoral fel- low, displays the threedimensional image of a

protein molecule on a computer screen at one of the

interactive color graphics

workstations at CARB.

In the membrane area, NIST

scientists are studying gas separations, biomolecule transport and

adsorption, and reactive membranes; in the area of gas

separations, researchers are investigating novel facilitated transport

membranes for use in acid gas removal and air separations. Reactive membrane systems are being

studied for trace component

removal and for gas cleanup/

recycle applications. In an interdisciplinary project, researchers are examining the adsorption of

biological macromolecules to

ultrafiltration membranes, with

the objective of developing better

predictive models for fouling, flux

decline, and chromatographic applications. Other study areas include pervaporation membranes

for close boiling mixtures and

composite and polysaccharide

membranes for small biomolecule

separations.

CONTACT: John J. Pellegrino

Div. 832

Boulder, Colo. 80303

(303) 497-3416

REFRIGERATION

Cooling superconducting

electronics, magnetic devices, and

highly sensitive infrared detectors

requires specialized refrigerators

capable of reaching cryogenic

temperatures. Other applications,

such as satellite cooling or gas

liquefaction, demand long-term

reliability and maintenance-free

operation. Advances in the 1980s

led to widespread interest in many

regenerative-cycle refrigeration

systems for these applications, in- cluding the use of pulse-tube

refrigerators. NIST is the world

leader in pulse-tube refrigeration

research and is developing extensive engineering databases for

these devices and other

regenerator applications.

In pulse-tube studies, NIST

scientists have developed the

orifice pulse-tube refrigerator

(OPTR), which has reached

temperatures of 60 K in a single

stage. Using thermoacoustic

drivers (TADs) in place of mechanical compressors, an OPTR

was designed with no moving

parts. A patent. Strategic Defense

Initiative Office (SDIO) innovative

technology award, and an R&D

100 award have been received for

this device, called a TADOPTR.

Recently, the TADOPTR was

proposed for liquefaction of

natural gas at remote well sites, where about 30 percent of the gas produced would be burned to run

the TAD, providing cooling to liquefy the remaining 70 percent.

Substantial research efforts have been applied to the development of improved regenerators for

refrigeration systems. NIST researchers have assembled the

world's largest database for adsorption of low-temperature gases on

carbon. NIST computer models of

regenerator performance are the

only optimization tools available

to designers of regenerators.

CONTACT: Ray Radebaugh

Div. 832

Boulder, Colo. 80303

(303) 497-3710

CHEMICAL

KINETICS AND

THERMODYNAMICS

CHEMICAL AND

BIOCHEMICAL

THERMODYNAMICS

NIST researchers have developed

precision oxygen combustion

calorimeters to measure the enthalpy of combustion, from which

enthalpy of formation can be

derived, for samples varying in mass from 10 mg to 2.5 kg. These

instruments are used to characterize thermodynamic properties

for species of interest in biochemistry, organic chemistry (including strained species), phosphorous

chemistry, and heterogeneous fuel

technologies. The measurements

also serve as the basis for Standard

Reference Materials and Standard

Reference Data for a variety of

technologies, including energy. The researchers maintain

several data centers that evaluate

thermodynamic data in inorganic,

organic, and aqueous chemistr}'.

They examine existing data, extrapolate these data to temperatures

outside the range of measurement,

create algorithms for data evaluation and manipulation, and

produce reliable estimation

schemes for predicting the properties of species for which measure- ments are not available. Current

interests include the technological

problems of combustion, nuclear

waste disposal, and atmospheric ozone depletion and the prediction

of the formation properties of organic species in the gaseous, liquid, solid, and aqueous phases.

CONTACT: Sharon Lias A260 Chemistr)'

(301) 975-2562

35 CHEMICAL SCIENCE AND TECHNOLOGY
COOPERATIVE RESEARCH OPPORTUNITIES

CHEMICAL KINETICS

The chemical kinetics program at NIST provides reliable chemical

kinetics data, measurement

methods, and theoretical models.

Applications of this research include combustion, new chemical

technologies, the chemistry of the upper atmosphere and other

planetary atmospheres, effects of

ionizing radiation on materials,

solar energy conversion, biotechnology, flue-gas cleanup

chemistry, acid rain, toxic waste

incineration, coal conversion, and

analytical applications of kinetics. Among the experimental projects under way at NIST are pulse

radiolysis of aqueous solutions

and kinetic mass spectrometric

studies (Fourier transform ion

cyclotron resonance, highpressure mass spectrometry, tan- dem mass spectrometry) of the

kinetics and thermochemistry of ion/molecule reactions and

ion/molecule clustering processes.

Researchers also are studying

free-radical kinetics using heated

single-pulse shock tubes, flash

photolysis kinetic absorption

spectroscopy and a flash photolysis resonance fluorescence technique, vacuum ultraviolet laser

photolysis with kinetic absorption

detection, and high-temperature

reactors. Resonance enhanced

multiphoton ionization (REMPI)

spectroscopy is used to provide new, previously unobtainable data

about the electronic structures of a

wide variety of free radicals. REMPI procedures also lead to

very sensitive and selective schemes for the optical detection

of the radicals. An important focus

of the kinetics program is the production of databases of

evaluated chemical kinetic data,

as well as the design of databases

and relevant software.

CONTACT: Sharon G. Lias A260 Chemistry

(301) 975-2562

INORGANIC

ANALYTICAL

RESEARCH

ATOMIC SPECTROSCOPY

Atomic spectroscopy methods are probably the most widely used

analytical techniques in industry

today. Considerable research is required, however, to keep up with

the changing needs of industry.

At NIST, research in atomic

spectrometry is focused on several

different areas. For instance, researchers are working to improve

the analytical capabilities of direct

current plasma and inductively

coupled plasma, as well as ex- perimenting with the glow dis- charge as an atom reservoir.

Additional research concerns

the use of spark sampling for the

direct analysis of solids, the continued development of laser- enhanced ionization in flames,

and the use of uv-Vis Fourier trans- form spectroscopy for the purpose

of optical line assignments of atomic transitions in commonly

available atom sources. X-ray

fluorescence is used for homogeneity testing and certification of a wide variety of metals,

ceramics, and other materials.

NIST scientists also are developing a series of neutral density filters that can be issued as Standard

Reference Materials for verifying

the accuracy of the transmittance

and absorbance scales of

ultraviolet, visible, and

near infrared absorption

spectrophotometers.

CONTACT: Robert L. Watters B222 Chemistry

(301) 975-4122

ANALYTICAL MASS

SPECTROMETRY

Analytical mass spectrometry has

played a key role in industries,

such as the semiconductor industry, that require accurate measurements of trace elements in raw

materials, products, and product

containers. The NIST inorganic mass spectrometry program is concerned with developing analytical

capabilities for making highly accurate determinations of trace inorganics using stable isotope

dilution and highly precise measurements of isotopic compositions,

as well as highly accurate measurements of absolute isotopic compositions to redetermine atomic

weights.

Areas of research include

instrumentation in thermal

source, inductively coupled plasma source, and ionization and

chemical separations at the trace

level using chromatography and

other techniques. Methods are developed for generating and

maintaining pure reagents and a

clean environment to decrease

limits of quantitation.

CONTACT: John D. Fassett A21 Physics Bldg.

(301) 975-4109

INORGANIC

ELECTROANALYTICAL

RESEARCH

Electroanalytical research is vital

to the development of methods

and materials for environmental

and clinical determinations. A

broad range of electroanalytical

and chromatographic techniques,

such as voltammetry, coulometry,

and ion chromatography, are used

by researchers at NIST for analysis

and research. Research on standardization of pH and electrolytic

conductance leads to the certification of new classes of Standard Ref- erence Materials.

CONTACT: William F. Koch

A349 Chemistry Bldg.

(301) 975-4141

ACTIVATION ANALYSIS

Nuclear methods of analysis provide unique approaches to quantitative analysis. In this research,

methods of nuclear analysis are

investigated utilizing the 20-MW

NIST research reactor. All areas of

the technique are researched, in- cluding the capabilities of cold- neutron activation, the use of monitor activation, radiochemical

separations, the determination of new mathematical procedures for

the resolution of gamma spectra,

the development of prompt

gamma activation techniques, the

use of charged-particle activation

techniques, and neutron depth

profiling.

CONTACT: Robert R. Greenberg

B108 Reactor Bldg.

(301) 975-6285

36
ORGANIC ANALYTICAL

RESEARCH

LIQUID

CHROMATOGRAPHY

ELECTROCHEMISTRY

Although hquid chromatography

(LC) is one of the most widely

used analytical techniques in industrial laboratories, its use can

be made even more widespread by

improvements in detection

methods. NIST researchers are working to develop novel ap- proaches for the electrochemical

detection of organic analytes

separated by liquid chromatography. For this technique to be

applied most effectively, the

electrode reaction mechanisms of

the compounds to be detected must be investigated using techniques such as cyclic and reversepulse voltammetry, coulometry,

and LC/ultraviolet spectroscopy.

Ongoing NIST work focuses on

the use of differential pulse and

dual-electrode detection, as well

as the development of single- and

array-microelectrode detectors. Researchers also are developing new

liquid chromatographic separations employing specific chemical

interactions, including chelation,

ion-pairing, charge transfer complexation, and acid-base

equilibria.

CONTACT: William A. MacCrehan

B158 Chemistry

(301) 975-3122

CAPILLARY

ELECTROPHORESIS (CE)

The exciting new technique of

electrophoresis in small-diameter

capillaries provides tremendous

opportunity for basic research into

the fundamental properties and

interactions of ions and neutral molecules. The association of analyte ions via simple electrostatic attraction, or more stable complexation, may be directly

studied by the effect on the

electrophoretic mobility of the

ions. Hydrophobic interactions

between neutral molecules and

charged micellar surfactants can

be investigated using micellar

electrokinetic capillary electrophoresis (MECE).

Through the use of electrolyte

modifiers such as urea and

methanol, MECE can be extended

to very non-polar molecules. Surfactants with more specific interactive character, such as aromaticity

and chirality, need further exploration. Other "physical" additives

also promise to increase the applicability of CE. Soluble polymeric gels can be used to provide

molecular weight discrimination

for biomolecules, where differences in charge may be too small to

allow direct CE separation.

Detection in CE is also a hot research area. The small sample size and capillary dimensions make

sensitive detection difficult.

Electrochemical detection in CE

by the use of microelectrodes does

not suffer from the dimensional

liabilities normally associated

with the use of small capillaries.

Using knowledge gained from the

recent exploration of oxidative

detection via carbon fiber and

platinum electrodes, researchers

should also be able to carry out

reductive detection at mercury

film electrodes. Sensitive optical

CE detection using axial absorbance, as well as laser-source ther- mal lens and fluorescence modes

are of current interest at NIST.

CONTACT: William A. MacCrehan

B158 Chemistry

(301) 975-3122

BIOANALYTICAL SENSORS

Biosensors are a new generation of

analytical devices with the potential for widespread use in biomedical and industrial monitoring

applications. Biosensors will

incorporate the latest advances in biotechnology to provide high

specificity and sensitivity. Biologically derived substances have great

value as components of sensing devices because of their binding

specificity, the strength of their interactions, and their potential for

use in conjunction with a wide

variety of amplification schemes.

Immunological, enzymatic, and

receptor-ligand interactions are being explored as the basis for

analytical measurement.

NIST researchers are using a

variety of optical techniques for

detection. Detection can be based on changes in size and rotational

mobility of analytes or binding

agents upon interaction, or it can

be the result of enzymatic activity

that occurs due to analyte binding, causing enhanced fluorescence or absorbance signals.

Amplification can be achieved

with release to liposomeencapsulated molecules or multiturnover enzyme reactions. Combining high specificity for

analytes with amplification

provides the potential for extremely sensitive devices.

CONTACT: William A. MacCrehan

B158 Chemistry

(301) 975-3122

SUPERCRITICAL FLUID

EXTRACTION (SFE)

NIST researchers are studying the

elucidation of the basic

mechanisms responsible for

analyte release in supercritical

fluid extraction processes. They

are designing experiments to deter- mine the role of pressure, temperature, and extractant fluid composition on the equilibrium

and kinetic processes of analyte

release from both simple model

and complex environmental

matrices.

Research in this area also en- compasses the practical application of analytical SFE to a wide

variety of sample matrices; the modeling of the analyte-trapping

process and concurrent design/

optimization of trapping media;

hardware and software development for automated extraction sys- tems for on-line chromatographic

analysis; investigations of inter- mediate analyte class separations

based on solid phase adsorbents,

following the extraction; and the

design of expert systems for the

optimization of SFE system perfor- mance. Analyte/matrix combinations being studied include

polycyclic aromatic hydrocarbons

and polychlorinated biphenyls in such matrices as sediments, soils, and air particulate matter; fatsoluble vitamins in foods and

serum; and drugs of abuse in body

fluids and hair.

CONTACT: Stephen N. Chesler

(301) 975-3102

William A. MacCrehan

(301) 975-3122

B158 Chemistry

LABORATORY

AUTOMATION AND

ROBOTICS FOR

ORGANIC ANALYSIS

NIST has joined with industry' ;md

other government agencies in a

cooperative project to develop

automated analytical devices for organic analysis based on new

chemistries and apparatus, :is well

as on laboratoiy robotic systems.

37 CHEMICAL SCIENCE AND TECHNOLOGY
COOPERATIVE RESEARCH OPPORTUNITIES

One project focuses on the development of an on-line system for extraction of solid samples (using

supercritical fluids and volatile

liquids) with deposition onto a

short chromatographic column,

followed by selective elution for

conventional chromatographic

analysis. In a second project, researchers are studying the use of a

state-of-the-art laboratory robotic

system for automated sample

preparation of samples for clinical and environmental analysis.

CONTACT: Stephen N. Chesler

(301) 975-3102

William A. MacCrehan

(301) 975-3122

B158 Chemistry

Gary W. Kramer

(301) 975-4132

A343 Chemistry

SUPERCRITICAL FLUID

CHROMATOGRAPHY

Supercritical fluid chromatography (SFC) in both capillary and

packed columns has been shown

to offer several advantages when

compared with liquid and gas chromatography for highefficiency separations of nonvolatile, reactive, or thermally

labile molecules. NIST scientists

are investigating the variables that

influence retention, selectivity,

recovery, and efficiency of SFC

separations; the use of SFC as an

analytical technique for providing

high-efficiency separations and accurate quantitative analysis of complex mixtures; and the use of

supercritical fluids for extraction

of solid and liquid samples emphasizing on-line extraction and

analysis of micro samples.

CONTACT: Stephen A. Wise

(301) 975-3112

Lane C. Sander

(301) 975-3117

B158 Chemistry

FUNDAMENTAL

CHEMICAL AND

PHYSICAL PROCESSES

IN CHROMATOGRAPHY

Solute retention in chromatographic systems is the result of a complex assortment of molecular

interactions between the solute,

the stationary phase, and the

NIST has organized a consor- tium of industry and government researchers to develop

a prototype automated analytical chemistry laboratory.

When completed, the modular system will perform the

major steps of a chemical

analysis: sample preparation (dissolving by microwaves, as shown in photo),

separation, and detection.

mobile phase. The diversity of

these interactions can be used to optimize separations for different

classes of compounds by varying

separation parameters, such as stationary phase and/or mobile

phase composition, and column

temperature. An understanding of

these fundamental retention mechanisms facilitates the optimization

of separations in gas chromatography (GC), liquid chromatography (LC), and supercritical fluid chromatography (SFC). Recent LC research has focused on the design of chemically

bonded stationary phases (such as monomeric and polymeric Cig

phases and charge transfer

phases), which offer unique

capabilities for the separation of

isomeric compounds and com- pound classes. Polycyclic aromatic

hydrocarbons have been used as model solutes for investigating

retention mechanisms. Since these compounds are highly isomeric,

retention effects resulting from differences in solute shape can be isolated by studying isomer sets. Molecular modeling of solutes and stationary phase species holds

the potential to provide further insight into retention mechanisms.

Similar approaches can be taken

to characterize retention processes

in GC and SFC. A comparison of

the retention behavior for isomer

sets in GC, LC, and SFC may prove

useful in developing a unified understanding of chromatographic

retention processes.

CONTACT: Stephen A. Wise

(301) 975-3112

Lane C. Sander

(301) 975-3117

Michele M. Schantz

(301) 975-3106

B158 Chemistry

38
TRACE ORGANIC

ANALYSIS USING

HIGH-RESOLUTION

CHROMATOGRAPHY

NIST research in high-resolution

chromatography is focused on the development of gas chromatography (GC) and liquid chromatography (LC) methods for the determination of individual

organic compounds in complex

mixtures. Research areas in GC

include:

development of systematic

chromatographic approaches for sample preparation/cleanup and

analyte preconcentration prior to GC analysis;

development of multidimensional chromatographic procedures using stationary phases of

differing selectivity;

use of simultaneous multiple

and/or selective detection systems

(such as mass spectrometric,

electron capture, and flame

photometric detectors); and

development of on-line extraction and analysis of solid microsamples. Recent activities have emphasized the measurement of trace

levels of environmentally significant compounds, including

polychlorinated biphenyls and

polycyclic aromatic hydrocarbons,

in natural matrices such as sedi- ment, tissue, and airborne particulate matter. Using LC, researchers vi^ill

focus on the following approaches

to analyzing complex mixtures:

solid-phase extraction on short columns as an isolation/

cleanup/preconcentration step; development of multidimensional

LC procedures (multidimensional)

to isolate and quantify selected compounds; selective detection sys- tems (such as uv, fluorescence.

electrochemical, mass spectrometric, chemical derivatization);

and the development of microcolumn LC procedures.

CONTACT: Stephen A. Wise

(301) 975-3112

Michele IVl. Schantz

(301) 975-3106

B158 Chemistry

METHODS AND

STANDARDS FOR DRUGS

OF ABUSE TESTING

To reduce the use of illegal drugs,

particularly in work-related activities, many employers are now

performing drug tests on

employees and prospective

employees. Most of these tests involve analysis of urine samples for

traces of drugs or metabolites. Be- cause tests used to screen urine

samples for drugs are subject to

cross-reactivity from legal substances, it is strongly recom- mended, and in many cases mandated, that all positives from

the screening procedure be subjected to confirmatory analysis by

gas chromatography/mass

spectrometry (GC/MS). The GC/MS

methods are used not only to confirm the presence of drugs but also

to quantitatively determine if concentrations of the drugs are above

specified cutoff levels. Laboratories

performing these confirmatory

analyses must ensure that their methods produce accurate results. To support accuracy in drug

testing, NIST scientists are developing a series of urine-based Standard Reference Materials with

appropriate concentrations of

drugs of abuse. Drug levels are certified by a combination of two independent methods, one of which

is generally GC/MS. Research is

ongoing to develop alternate methods to complement GC/MS.

Considerable attention is now

focused on an alternate matrix for drug testing. Human hair provides a long-term record of drug use, in

contrast to urine which provides a

record of only the previous 48

hours to 72 hours. NIST scientists

are investigating analytical

aspects of hair analysis for drugs

of abuse. Research areas include

the extraction of drugs from hair,

measurement methods, the effects

of hair treatments on drug levels, and differentiation between hair

externally contaminated with

drugs and hair with drug levels

acquired through internal use.

CONTACT: Michael J. Welch

8158 Chemistry

(301) 975-3100

MASS SPECTROMETRY

OF BIOMOLECULES

Major advances in mass

spectrometry have improved its

capabilities for characterizing

biomolecules. Techniques such as

fast- atom bombardment,

electrospray, matrix-assisted laser

desorption, and others permit the

accurate determination of molecular weights of peptides and

small proteins previously unmeasurable by mass spectrometry.

Molecular weights greater than

look daltons are now being deter- mined with accuracies far exceeding those of other techniques.

Advances in structural determinations of biomolecules include the

use of collision-induced dissociation and photodissociation for determining sequence information

for peptides and oligonucleotides.

Considerable attention now is

focused on coupling these new

mass spectrometric techniques

with developments in capillary

electrophoresis and microscale

liquid chromatography.

Scientists at NIST are investigating these new techniques to understand their capabilities and

apply them to biomolecule characterization. They are particularly

interested in applying these tech- niques to the quantitative analysis

of species not previously amenable

to mass spectrometric analysis.

These capabilities should result in

the development of reference materials to support industries involved

in biotechnology and biomedical

research.

CONTACT: Michael J. Welch

81 58 Chemistry

(301) 975-3100

TRACE GAS

MEASUREMENT

TECHNIQUES

Accurate measurement of gaseous

species is of great importance to many industries for applications

ranging from quantification of

pollutant and toxic gas emissions

to the quality control of products.

The validity of data derived from

such measurements is tied directly

to the availability of useful gas measurement techniques and to

the degree of understanding of

their capabilities and limitations. Although a variety of techniques

have been applied to trace gas

analysis, more research is needed

to improve the present state of the

art. This research is particularly

important because of the growing

need for the analysis of specific

gas species in multicomponent

gaseous mixtures; it also is necessary' to extend accurate analyses to below the parls-per-million and

parts-per-billion levels.

39 CHEMICAL SCIENCE AND TECHNOLOGY
COOPERATIVE RESEARCH OPPORTUNITIES

Current NIST research focuses on new detection systems using

chemiluminescence, electrochemistry, infrared diode laser systems, capillary gas-liquid and

gas-solid chromatography coupled

to mass spectrometry, and isotopedilution mass spectrometry.

Institute scientists also are ex- amining the use of class-specific

detectors for gas chromatography

and evaluating electronic circuitry

to optimize signals and reduce instrumentation noise and drift.

CONTACT: William D. Dorko

B158 Chemistry

(301) 975-3916

INSTABILITY OF

COMPRESSED GAS

MIXTURES

Inorganic and organic compressed

gas mixtures are employed extensively throughout industry to

calibrate equipment used to assess

the quality of products and the

effectiveness of emission controls. Although the stability of these mixtures is critical to their successful

use, a number of instances have

been noted in which instability

has been observed, particularly in mixtures containing low levels of

reactive gaseous species, such as nitrogen oxides, sulfur dioxide,

and hydrocarbons.

The reasons for instability may

differ somewhat for various

gaseous species, but they are related to at least two possible

phenomena: gas-phase reactions

and gas-metal interactions with

the internal surface of the

cylinder. NIST researchers are

working to improve the understanding and predictability of

these phenomena. Their tech- niques involve those employed in

surface science studies and other

approaches, such as Fouriertransform infrared, diode laser, and other spectroscopies; mass

spectrometry; metal analysis;

trace water and oxygen analysis;

chemiluminescence analysis; and

the use of specifically doped mixtures and homogeneous gas phase

kinetics.

CONTACT: William D. Dorko

B158 Chemistry

(301) 975-3916

PROCESS

MEASUREMENTS

FLOW MEASUREMENT

RESEARCH AND

STANDARDS

The accelerating costs of scarce

fluid resources—particularly

petrochemical fluids—are caus- ing increased concerns about the performance levels of flow meters. Improved flow measurement

traceability needs to be established

and maintained so that realistic,

quantified data are generated on a continuing basis to assure practical fluid measurements at satisfactory, specified levels of perfor- mance. To achieve the desired

flow measurement traceability,

NIST is designing transfer standards to link the performance

of calibration facilities to

appropriate national reference

standards.

Because of the importance of

these measurements, transfer stan- dards need to be designed so that high levels of confidence can be

placed in them and their perfor- mance. The new transfer standards will be rigorously evaluated

against NIST fluid flow calibration standards. As part of the

evaluation, the appropriate range

of calibrations will be done on the developed standards so that perfor- mance levels can be assured at

specified levels. Current fluid- metering research programs use

laser Doppler velocimetry (LDV)

techniques to focus on the

pipeflows produced by conventional pipeline elements and by

standard flow conditioning elements. New experimental

programs are feasible using LDV

or other anemometry or flowvisualization techniques to study

other flows. NIST also has computational capabilities to model

numerically a number of closed conduit flow fields.

CONTACT: George E. Mattingly

105 Fluid Mechanics

(301) 975-5939

HIGH-TEMPERATURE

REACTORS

The chemical and associated industries produce enormous

amounts of byproducts. To avoid

wasting industrial resources and

polluting the environment, the impact of these byproducts must be

minimized. The solution of the problem lies in: minimizing waste

at the source by modifying industrial processes; recovering energy and chemicals for reuse; and

converting pollutants to acceptable species. For all of these solutions, thermal treatments offer the

most promising approach. Hence,

there is urgent need for detailed mechanistic elucidation of fundamental thermal processes, such

as pyrolysis and oxidation, that govern chemical conversion and

destruction of both model compounds and actual industrial

byproducts.

NIST maintains two instru- mented facilities that are exceptionally promising for efficient

pyrolytic and oxidative destruction

of a wide variety of chemical compounds: a fluidized bed reactor and a plug-flow reactor designed

for long residence times (seconds)

at elevated temperatures. The research centers on kinetic studies,

both global and mechanistic, of

destruction of model compounds

representative of major industrial

byproducts, the most prominent of which are chlorinated hydrocarbons and nitrogen-containing

species (amines and nitrocompounds, for example). The scientists are investigating the effects of

temperature, pressure, residence

time, and composition of reactor

fluids on destruction efficiency of

the model compound, as well as formation and disappearance of

intermediate products. Diagnostic

instrumentation includes both online sampling with subsequent

analysis by several analytical techniques (GC, MS, and FTIR) and insitu optical systems.

CONTACT: Andrej Macek

B312 Physics

(301) 975-2610

40
CHEMICAL SENSOR

RESEARCH

To understand the performance of

thin-film and chemical sensors, NIST scientists are conducting research aimed at improving their

accuracy, stability, selectivity, and

response, as well as developing

concepts for new measurement

techniques. Activities incorporate

adhesion, oxidation, interfacial

diffusion, surface adsorption and

desorption, and phase morphology

to investigate mechanisms of chemical sensing. Analytical

methods are used to relate the

structure and composition of sens- ing devices to fabricating

parameters and performance, and

for development of mechanistic

performance models. Research

areas include thin-film thermocouples and resistance devices,

moisture and pH sensors, and gas- phase chemical detectors based on

tin and other metal oxides.

Fabrication facilities available for

this research are rf and dc sputtering for both alloy and reactive

film deposition and gas reactors. The researchers also are investigating the feasibility of thin-film

systems as improved chemical sensors. Their research activities employ an array of surface characterization techniques to determine

the electronic properties of films

and single crystals for dielectric

strength and surface conductance.

Among the techniques used are X-ray and uv photoemission and

thermal desorption spectroscopies,

SIMS, and in-situ electrical measurements. Recent research activities have focused on the use of

spontaneously organized

monomolecular films for sensing

of chemical and biochemical

materials.

CONTACT: Kenneth G. Kreider

(301) 975-2619

Stephen Semancik

(301) 975-2606

Michael J. Tarlov

(301) 975-2058

A303 Physics

CHEMISTRY OF

SUPERCRITICAL WATER

OXIDATION PROCESSES

Supercritical water oxidation

(SCWO) is a new technology with

high promise as a safe, efficient

process for the minimization and

destruction of hazardous materials. It is a totally contained process that takes place in water above

its critical point, that is, at pressures greater than 22 MPa and

temperatures above 374 °C. Under

these conditions, many reactions

proceed unusually rapidly producing benign end-products carried

in the output water stream. Industrial implementation of SCWO

has lagged, in part because of an

inability to prescribe the process

variables, such as the temperature,

pressure, flow rates, and concentration of oxidants, required for safe,

efficient waste destruction. These,

in turn, demand understanding of fundamental thermodynamic and

kinetic processes in supercritical

media.

NIST researchers are seeking to

supply both the understanding

and data necessary to support reliable process modeling for SCWO.

The experimental work centers around reactors for studies of

chemical kinetics and durability

of materials, as well as a unique

flow reactor, which provides optical access for in-situ measure- ments of density, chemical species.

temperature, and product/reactant

concentrations. The researchers

currently are studying the ammonia destruction reactions as

functions of temperature, pressure, and added oxidant.

CONTACT: Gregory]. Rosasco

(301) 975-4813

Andrej Macek

(301) 975-2610

B312 Physics Bldg.

CHEMISTRY OF

HIGH-TEMPERATURE,

GAS-PHASE SYNTHESIS

OF MATERIALS

The semiconductor, coatings, and

ceramics industries require highperformance thin films, particles,

and fibers. This demand for materials with micro-engineered

mechanical, electrical, and optical

properties has placed greater emphasis on the development of new

processing methods and on the need for increased fundamental

understanding of materialsfabrication processes. NIST researchers are seeking an understanding of hightemperature materials synthesis in

a fast-flow reactor that provides

reaction temperatures in excess of 1500 K and residence times as

short as 10 ms, allowing extension

of conventional chemical kinetics

to temperature regimes representative of the chemistry relevant

to materials processing. The reactor has provision for molecularbeam sampling of gas-phase

species, including clusters, with

subsequent mass spectrometric

analysis. It also is equipped with

optical excitation and diagnostic

probe beams.

Currently, NIST scientists are

researching the homogeneous

(gas-phase) and heterogeneous

(thin-film and cluster/aerosol)

chemistry of silicon oxide. They

are comparing measurements of

species and growth kinetics to the

predictions of chemical reaction

and fluid flow models developed

for the process. This approach

identifies rate, purity, or defectlimiting steps in the process.

CONTACT: Michael R. Zachariah

B320 Physics

(301) 975-2063

DYNAMIC PRESSURE AND

TEMPERATURE RESEARCH

U.S. industry increasingly relies on

real-time monitoring of process

parameters, particularly temperature and pressure, to produce efficiently a desired end-product, to warrant safe operation, and to

assure equity in commerce. This

trend is pervasive in the chemical

and materials-processing industries, as well as in energy and

raw materials production and

transfer. NIST has a research pro- gram and is developing a test

facility to provide a reliable basis

for the evaluation and calibration

of transducer dynamical response

functions. The research seeks to develop a primary standard for dynamic temperature and pressure based on the fundamental properties of the molecular constituents

of a dynamical system. Information about the molecules is accessed via laser-optical diagnostic

techniques, and measurement

times of the order of 10 ns at ac- curacy levels of 5 percent appear

feasible. Through the use of these measurement techniques, an accurately characterized dynamical

source will be developed. This reference source and its ;issocialed

41 CHEMICAL SCIENCE AND TECHNOLOGY
COOPERATIVE RESEARCH OPPORTUNITIES

measurement system will provide

industry with a means for assuring

the accuracy of transducers used

to measure time-varying temperature and pressure.

CONTACT: Gregory]. Rosasco B312 Physics

(301) 975-4813

CHEMICAL-VAPOR

DEPOSITION REACTION

KINETICS AND

FLOW MODELING

Chemical-vapor deposition (CVD)

is an important process used to grow thin films in the manufacture of microelectronics devices,

as well as to produce highperformance coatings. CVD involves complex gas-phase

chemistry, surface chemistry, and mass and heat transport processes. These highly coupled processes

control the quality, uniformity,

and yield of the deposited layers.

NIST researchers are developing

and testing numerical models that can be used to design and control CVD processing reactors. These

models account for gas-phase

chemistry, particle formation,

heat and mass transport, and surface deposition leading to the for- mation of thin films. The modeling effort is co- ordinated with a measurement

program to supply the required

chemical kinetics and materialsgrowth information and to

validate the modeling results in a

materials-synthesis flow reactor. The measurement program

includes optical and mass

spectrometric diagnostics of the

gas phase and post-production

evaluation of particle and film

growth.

An interactive, graphics-based

chemical kinetics program has

been developed. Researchers are

constructing a supporting thermochemical and kinetics numerical

database, and they are developing

two-dimensional heat and mass

transport models, which simulate

reactor geometries relevant to

practical devices.

CONTACT: Donald R.F. Burgess

(301) 975-2614

Ronald W. Davis

(301) 975-2739

8320 Physics

PARTICULATE AND

DROPLET DIAGNOSTICS

IN SPRAY FLAMES

To minimize the cost of highpriced fuel, U.S. industry needs to

obtain maximum energy output

from fuel combustion. NIST

researchers are tackling this problem by attempting to improve combustion efficiency. The researchers

are studying the dynamics of spray flames to investigate droplet

vaporization, pyrolysis, combustion, and particulate formation

processes and to delineate the effect of chemical and physical

properties of fuels on the above

processes. The research results will

provide an experimental database,

with well-defined boundary conditions, for developing and validating spray combustion models.

The experiments are being carried out in a spray combustion

facility, with a moveable-vane

swirl burner, which simulates

operating conditions found in

practical combustion systems. A

combination of non-intrusive

probing techniques is used to obtain comprehensive data on spray combustion characteristics, including soot particle and droplet size, number density and volume fraction, gas composition, and velocity

and temperature fields.

Currently NIST scientists are

focusing their efforts on laser scattering and laser Doppler

velocimetry measurements to determine the correlation between

droplet size and velocity distributions, respectively, in both lowtemperature and burning sprays.

CONTACT: Hratch G. Semerjian

B308 Physics

(301) 975-2609

TEMPERATURESENSOR

RESEARCH

Improved industrial processes and

sophisticated scientific research

require temperature sensors that

cover wider temperature ranges with better accuracy and precision

than previously required. For example, the degradation of ther- mocouples exposed to high

temperatures for extended periods

of time represents a serious impediment to temperature measure- ments in jet engines, furnaces,

and so forth. NIST has several projects under

way to test and improve the perfor- mance of currently available sensors, including thermocouples,

and use resistance thermometers

of various types. The temperature

range covered by these projects extends from about 0.2 K to 2100 °C. NIST has excellent temperature

calibration facilities, an auto- mated laboratory equipped to

evaluate thermocouples at high

temperatures, several laboratories equipped for work on resistance thermometers, and a laboratory to

evaluate industrial grade thermometers. NIST is planning a series

of new materials and techniques

to provide highly precise and accurate temperature measurements.

CONTACT: B.W. Mangum

B122 Physics

(301) 975-4808

SURFACE AND

IVIICROANALYSIS

SCIENCE

MICROBEAM

COMPOSITIONAL MAPPING

Interpreting the relationship be- tween the physical and chemical

microstructure of materials is important in understanding their macroscopic behavior and in ex- tending their in-service perfor- mance. Conventional microbeam

techniques for elemental/

molecular compositional analysis on the micrometer scale, such as

the electron microprobe and ion

microscope, have been restricted

to quantitative analysis at individual locations. Mapping of the

distribution of constituents has

been possible only at the qualitative or semiquantitative level. However, recent NIST research developments have led to the production of the first truly quantitative elemental compositional

maps. Quantitative compositional

mapping with the electron microprobe has been demonstrated down to levels of 0.1 weight

percent, while quantitative isotope

ratio measurement in images has

been demonstrated with the ion

microscope. Current research activities at NIST include extending compositional mapping to analytical

electron microscopy, laser Raman

microanalysis, and laser microprobe mass analysis. Potential

projects could involve applying

the compositional mapping instru- ments to materials characterization problems, developing new techniques for compositional

mapping on other microanalysis

instruments, and investigating

42
basic topics in elemental and

molecular quantitative analysis

with microbeam instrumentation.

Among the equipment available at NIST is an electron microprobe, an analytical scanning electron

microscope, 200- and 300-kV

analytical electron microscopes, an ion microscope (secondary ion mass spectrometry, SIMS), a timeof-flight SIMS, a laser microprobe mass analyzer, a laser Raman

microprobe of NIST design, and

extensive computer facilities, in- cluding image processing.

CONTACT: Dale E. Newbury

A113 Chemistry

(301) 975-3921

ATMOSPHERIC AND

CHEMOMETRIC RESEARCH

Current regional and global concerns with the impact of human

activities on environmental con- tamination and wastes, atmospheric pollution, and potential

effects on health and climate

make it imperative to determine

with a high degree of accuracy the

individual sources of the noxious

species. State-of-the art research,

pioneered at NIST, makes possible

unique source identification by application of the most advanced

microchemical and isotopic

analytical techniques, including

accelerator mass spectrometry and

high-precision gas isotope ratio mass spectrometry.

Complementing advanced

isotopic-chemical characterization of atmospheric gases and particles is basic research in chemometrics, which represents

the synthesis of chemical

knowledge and measurement with

modern statistical and computational methods. Work in this area

is directed toward improving the

quality of chemical measurements

generally through advanced

design, measurement and data

analysis quality assurance, and

graphical multivariate data

exploration.

CONTACT: Lloyd A. Currie

B364 Chemistry

(301) 975-3919

Top. Chemical engineer Joe

Magee prepares a simulated

natural gas mixture for a Standard Reference Material to be used for precise

density measurements.

Bottom. Studies conducted

by research engineer Gary

Presser in the spray combustion facility are designed to provide more efficient use

of both conventional and al- ternative fuels.

THERMOPHYSICS

PROPERTIES OF FLUIDS

Therraophysical properties data

are essential for the design and

operation of many chemical

processes, such as supercritical

extraction. To obtain these data,

NIST scientists are using three new

phase equilibria apparatus for

studies at elevated temperatures: one makes VLE measurements on

carbon dioxide-hydrocarbon sys- tems and refrigerant-hydrocarbon

systems; the second is a dew/bubble point apparatus extending to 800 K; and the third employs a

palladium-silver membrane to measure the fugacity of hydrogencontaining mixtures.

Five exceptional instruments

are available for making PVT,

PVTx, and heat capacity measure- ments on pure fluids and fluid

mixtures: an isochoric PVT apparatus, a Burnett apparatus, a combined Burnett/isochoric PVT

apparatus, a magnetic suspension

densimeter for P\T and PVTx

measurements, and an instrument

to measure constant volume heat

capacity. Facilities also exist to determine properties along the two-phase coexistence line of pure

fluids and mixtures and to make

sound speed measurements.

NIST researchers also can

devise techniques to characterize

fluids and fluid mixtures when the

temperatures, pressures, and times

involved can result in reactions

during the measurement process.

CONTACT: William M. Haynes

Div. 838

Boulder, Colo. 80303

(303) 497-3247

Michael R. Moldover A 105 Physics

(301) 975-2459

43 CHEMICAL SCIENCE AND TECHNOLOGY
COOPERATIVE RESEARCH OPPORTUNITIES

THERMOPHYSICAL AND

SUPERCRITICAL

PROPERTIES OF MIXTURES

PROPERTIES OF

ATMOSPHERICALLY SAFE

REFRIGERANTS

Chlorofluorocarbons (CFCs) have

been used widely for the past

50 years as refrigerants; as foam

in building insulation, furniture,

and car seats; and in many other

Chemist Lloyd Weber

measures chemical and

physical properties of alternate refrigerants. The goal

is to help industry find effective replacements for

chlorofluorocarbons or CFCs, which break down the

Earth's ozone layer.

applications. Recent evidence has

shown, however, that CFCs are breaking down the ozone layer

that protects the Earth from harmful levels of ultraviolet radiation.

Alternative chemicals must be

found to replace the existing fluids

within the next decade. For this

to be achieved, an accurate knowledge of their thermophysical

properties is required. NIST has a

research program designed to provide these data to industry, ultimately in the form of interactive computer codes. The research includes extensive experimental

measurements on pure fluids and

mixtures, including PVT, PVTx, vapor pressure, saturation density,

heat capacity, thermal conductivity, viscosity, sound speed, and

surface tension. The program also

includes substantial effort in

modeling fluid properties and in developing equations of state.

CONTACT: Richard F. Kayser

A105 Physics

(301) 975-2483

PRESSURE STANDARDS

Achieving better understanding

and control of the pressure meas- urement process will lead to better

quality control in the manufacture of new materials and better

design and performance of

transducers for thousands of applications in modern technology.

The measurement of pressure from sub atmospheric to 689 MPa

and above with uncertainties of

tens to hundreds of parts per million is essential in modern technology.

The most fundamental instru- ment at these high pressures is the deadweight piston gauge. In the

piston gauge, a force generated in

a working fluid acts against the

surfaces of a piston and against

the walls of a cylinder that confines the piston. At high pressures,

the materials undergo significant

distortion, which leads to limitations and uncertainties in the area on which fluid is acting. The fluid

interacts with the side of the piston, creating upward forces that

are difficult to interpret. NIST

scientists are using various tools

finite-element analysis to characterize distortion, better hydrodynamic measurement and modeling of the annular region through

which the fluid flows, and improved piston gage designs—to understand these effects.

CONTACT: Charles D. Ehrlich

A45 Metrology

(301) 975-4834

VACUUM AND LEAK

STANDARDS

IVIany industries depend on accurate vacuum (pressure) and

leak measurements for research and development and for process and quality control. NIST develops

and maintains pressure and vacuum standards from above at- mospheric pressure to ultrahigh vacuum; leak or flow standards

are operated from 10"^ to below

10'^ std cc/s. Facilities include five

ultrahigh vacuum systems; two low-range flowmeters; high-ac- curacy mercury manometers; pressure and vacuum control systems;

and vacuum, electronic, data acquisition, and data analysis equip- ment.These facilities and measure- ment capabilities enable researchers to develop improved

measurement techniques and

equipment and to investigate the performance of vacuum and pressure equipment, specifically

mechanical pressure gauges, momentum transfer gauges,

ionization gauges, standard leaks,

and residual gas analyzers. In addition, NIST plans to use this measurement capability to investigate properties of materials and

physical phenomena of fundamental interest. Among the planned

projects is the development of reference standards for the transition regime between low pressures measured by mechanical or

electromechanical gauges and

pressures measured by vacuum

technology devices. The development of accurate methods to measure and characterize

ultrahigh vacuum systems is also under investigation.

CONTACT: Charles R. Tilford A51 Metrology

(301) 975-4828

Chemical process technology requires accurate knowledge of

various thermophysical properties

of pure, polyfunctional chemicals

and their mixtures. NIST research

focuses on the most important of

these properties—equilibrium

phase composition, density, and

enthalpy. NIST researchers are

developing predictive methods for

the properties of chemically dissimilar compounds, especially

complex mixtures and aqueous

solutions. Another project is aimed

at developing accurate predictive

models for the thermo-dynamic

and transport properties of near

critical and supercritical mixtures.

This work includes PVTx and VLE

measurements on mixtures containing carbon dioxide,

halogenated hydrocarbons, and

similar supercritical solvents. Other experimental work involves

using supercritical chromatography to measure diffusion coefficients in supercritical mixtures

and theoretical studies to focus on

applying extended corresponding

states to supercritical systems.

CONTACT: Thomas J. Bruno

Div. 838

Boulder, Colo. 80303

(303) 497-5158

J.M.H.L. Sengers

A121 Physics

(301) 975-2463

44
RESEARCH

FACILITIES

WATER FLOW

MEASUREMENT FACILITY

The NIST water flow measurement

facilities are used to establish,

maintain, and disseminate

flowrate measurements, standards,

and data for the wide range of conditions needed by U.S. industry. Industry requests include flow meter

calibrations, round robin testing

programs to establish realistic

traceability chains in the form of

flow measurement assurance programs, data-generation

programs for industrial groups

and trade associations, and

testbeds for carrying out industrial

research programs focused on flow

measurement topics.

CAPABILITIES: Water flow

facilities enable flowrates up to 40,000 liters/min in pipe sizes that range up to 500 mm in diameter.

Maximum operating pressure is

1 MPa. Flowrate determination

schemes use static and dynamic

gravimetric systems.

APPLICATION: These facilities are

used to establish and maintain the

national bases for the liquid

flowrate measurement systems.

The end result is orderliness in the marketplace, both domestically

and internationally, for U.S. industries involved in the custody

transfer and/or process control of

valuable fluid resources and products. Potential users include the National Aeronautics and Space

Administration, the Department of

Defense, the oil and gas industries,

the chemical and related industries, and the power and

energy-generation industries.

AVAILABILITY: The facilities

are available upon request to U.S.

industry, other government agencies, and academia for collaborative research projects and

calibrations.

CONTACT: George E. Mattingly

105 Fluid Mechanics

(301) 975-5939

FLum^^mT

RESEARCH FACILITY

The NIST Fluid Metering Research

Facility combines primary calibration techniques with the capability

to conduct detailed surveys of fluid

velocity profiles in temperaturecontrolled water flows using laser Doppler velocimetry (LDV).

LDV is a non-intrusive tech- nique for determining the fluid

velocity at a particular location in

the flow. It enables pipeflows to be

surveyed for a wide range of

piping configurations in pipe sizes up to 20 cm in diameter. Temperature control enables stable fluid and flow conditions to be established and maintained for extended test periods. The primary

calibration technique uses

dynamic gravimetric methods to determine accurately the bulk

liquid flowrate.

CAPABILITIES: Water flowrates up

to 240 liters/min in a range of pipe sizes up to 20 cm in diameter can be produced. Maximum

operating pressure is 0.5 MPa, and

temperature can be stabilized in

the range from l6 °C to 30 °C.

APPLICATIONS: This facility is used to conduct calibrations,

special fluid measurement tests,

or selected research programs on flow topics. An industrygovernment consortium currently

supports a research program on

flowmeter installation effects, and

the U.S. Navy is sponsoring a

series of tests to assess the perfor- mance of selected flow transfer

standards' in a range of non-ideal

installation conditions.

The facility is used to generate

critical databases used to initiate

or update the national standards on generic fluid metering topics.

These standards are used for accurate custody transfer of fluid

resources or products in the domestic and international marketplace

or for process control in chemical

manufacturing processes. Among

the potential users of the facility

are the Department of Defense, the

National Aeronautics and Space

Administration, the oil and gas industries, the engine manufacturing and testing industries, and

the energy-generation industries.

AVAILABILITY: These facilities

are available upon request to

U.S. industry, other government

agencies, and academia for collaborative research projects or

calibrations.

CONTACT: George E. Mattingly

105 Fluid Mechanics

(301) 975-5939

NITROGEN FLOW

MEASUREMENT FACILITY

The nitrogen flow measurement

facility is a mass-based reference system capable of both liquid and

gas flow measurement. Well instru- mented for temperature and pressure, the facility is adaptable and

capable of a variety of piping ar- rangements. Located completely

indoors, it is not subject to en- vironmental changes.

CAPABILITIES: When configured

for gas flow measurements, the

facility has a flow rate range of

0.5 kg/s to 2.4 kg/s. In this mode,

the nitrogen gas is at pressures of approximately 4 MPa and temperatures of approximately 288 K. The

facility has a flow rate range of

0.05 kg/s to 10 kg/s when set up

Mechanical engineers

George Mattingly (right) and

T.T. Yeh (center), with technician Boyd Shomaker,

study flow-measuring devices using laser Doppler

velocimetry at the NIST

fluid metering research

facility.

45 CHEMICAL SCIENCE AND TECHNOLOGY
RESEARCH FACILITIES

n

f" -3

for liquid flow measurements. Liquid nitrogen can be at pressures up to 0.7 MPa and temperatures

between 75 K and 90 K in this configuration. This continuous flow

facility permits dynamic mass flow

measurements. For volume flow

measurements, density is deter- mined by making pressure and

temperature measurements and

calculating density from an equation of state.

APPLICATIONS: The nitrogen flow

facility can be used for testing a

variety of flow measurement instrumentation, including flowmeters, temperature sensors,

pressure sensors, and densimeters.

The ability to operate the facility

at stable conditions for long

periods of time permits testing of instrumentation stability. The

ability to vary system parameters

permits testing of instrument

sensitivity.

AVAILABILITY: Collaborative or in- dependent programs for this test

facility can be arranged. The

facility must be operated by NIST

staff.

CONTACT: Blaine R. Bateman

Div. 832

Boulder, Colo. 80303

(303) 497-5366

NEUTRON DEPTH

PROFILING FACILITY

The neutron depth profiling

(NDP) facility uses a neutron beam for non-destructive evaluation of elemental depth distributions in materials. Working with

the Institute's 20-MW nuclear reactor, researchers use the technique

to provide concentration profiles

for characterizing the nearsurface regime of semiconductors,

metals, glasses, and polymers to

depths of several micrometers. The

facility uses filters and collimators

to produce a high-quality neutron beam with good thermal neutron

intensity and minimum con- tamination with fast neutrons and

gamma rays. An aluminum target

chamber is used to contain the samples in a vacuum, and a full

array of electronic components is

available for data acquisition and

analysis.

CAPABILITIES: With the thermal neutron beam provided by the

reactor, depth profiling can be

carried out with sensitivities ap- proaching 10^^ atoms/cm^. A

single analysis produces a profile

typically 5 |J-ni to 20 |im deep

with a resolution of better than

30 nm. Once calibrated with the

appropriate elemental standard,

the concentration scale is fixed in- dependently of the sample cornSchematic of the Nitrogen

Flow IVIeasurement Facility.

position. Elements that do not produce charged particles under

thermal neutron irradiation contribute no interference.

APPLICATIONS: Applications of NDP include range measurements

for boron implanted in Si, GaAs,

and MCT; observations on nearsurface boron in glasses; lithium

concentration profiles in lithium

niobates and aluminum alloys;

measurement of helium release in

single-crystal nickel to investigate

the He-trapping phenomena; and

measurement of high-dose

nitrogen implants in steels.

AVAILABILITY: The facility is

available to qualified researchers on an independent or collaborative basis with NIST staff.

CONTACT: R. Greg Downing

B125 Reactor

(301) 975-6286

46
PHYSICS

LABORATORY

Attending to the long-term needs of many U.S. hightechnology industries, NIST's Physics Laboratory conducts

basic research in the areas of quantum, electron, optical,

atomic, molecular, and radiation physics. This research is complemented by work in quantum metrology and efforts

to improve the accuracy and precision of time and frequency standards.

Much of the laboratory's research is devoted to over- coming the barriers to the next technological revolution,

in which individual atoms and molecules will serve as the

fundamental building blocks of electronic and optical

devices. Manufacturing products based on ultrasmall,

atomic-scale systems will require entirely new measurement techniques. To develop the necessary measurement

capabilities, laboratory scientists are using highly specialized equipment, such as polarized electron microscopes,

scanning tunneling microscopes, and synchrotron radiation sources, to study and manipulate the behavior of individual atoms and molecules.

They are investigating how atoms and molecules aggregate into clusters and microstructures and how these

microstructures behave on surfaces and in solids. With

lasers and other advanced spectroscopic methods, scientists have trapped atoms and ions, induced unusual quantum phenomena, and measured chemical reactions on

material surfaces over time spans as short as a few

hundred quadrillionths of a second, the time frame for a single molecular vibration.

In support of industries ranging from photography to aerospace to lighting, the laboratory is working to improve

optical measurement techniques for a diverse range of

applications, including remote sensing, advanced colorgraphic imaging systems, and optically pumped atomic

clocks. Complementing research fosters the development

of emerging X-ray technologies, such as X-ray lithography

for the semiconductor industry and X-ray imaging.

Contact: Katherine B. Gebbie

B160 Physics

(301) 975-4201

COOPERATIVE

RESEARCH

OPPORTUNITIES

ELECTRON AND

OPTICAL PHYSICS

UV OPTICS

TESTBED

The emerging field of high reflectance, normal incidence, soft X-ray/extreme ultraviolet (xuv)

optics has a wide range of applications. The ability to produce highquality images at wavelengths

below 40 nm has allowed construction of xuv solar telescopes with

unprecedented resolution; xuv

microscopes able to study living

biological samples with submicron resolution; and xuv

photolithographic systems that

will produce the next generation

of integrated circuits. NIST has initiated an xuv

multilayer characterization facility at the SURF II electron storage

ring, which is available to all researchers on a cooperative basis. The present facility is capable of measuring the reflectance or trans- mission of xuv optics (such as mirrors, filters, and gratings) as a

function of wavelength, angle of

incidence, and position on the

optic from 8 nm to 60 nm. NIST is

constructing a new facility that

will extend measurement capabilities to shorter wavelengths, larger

substrates, and more highly

curved optics and at the same time

increase resolution and accuracy. An optical testbed also is being

constructed to measure the imaging properties of individual optics

and entire optical systems. The

first element of this testbed will be

a quasi-real-time imaging device

with a resolution goal of 25 nm.

CONTACT: Richard N. Watts A253 Physics

(301) 975-6892

ATOMIC

PHYSICS

VACUUM ULTRAVIOLET

RADIOMETRY

As part of its research to understand and measure various forms

of radiation, NIST is conducting vacuum ultraviolet studies involving radiation damage, polymerization of organic molecules, and

solar simulation. NIST scientists have worked with researchers from

industry to develop and test vacuum ultraviolet instrumentation, new spectrometer designs,

and detector systems, especially for

flight in space. They also have collaborated on special sources, narrow-band filters, and lasers. NIST scientists are interested in doing cooperative research in

several other areas, including

studying hollow cathode lamps,

laser plasmas, and sparkdischarge light sources as secondary standards. State-ofthe-art radiometric facilities and

advanced optical equipment are

available at NIST for these studies.

CONTACT: J. Mervin Bridges A 167 Physics

(301) 975-3228

CHARACTERIZATION

OF LOW-TEMPERATURE

PLASMAS

The properties of low-temperature

plasmas play a key role in the

processing of materials such as semiconductors. Proper characterization of these phisnuus is essential to develop accurate plasma

diagnostics and useful plasma

models for specific applications. At

47
COOPERATIVE RESEARCH OPPORTUNITIES

NIST, plasma discharges are characterized utihzing optical emission spectroscopy, laser-induced

fluorescence, laser scattering, and

optogalvanic methods. Modeling

of the plasma is also an integral

part of this characterization.

Discharge sources include lowpressure rf plasmas, stabilized

arcs, glow discharges, heat pipes

with laser resonance ionization,

and inductively coupled plasmas.

An extensive array of laboratoiy equipment is available to accomplish this characterization,

including several Nd:YAG pumped,

high-resolution (<0.1 cm'') dye

lasers; Ar ion-pumped dye and

ring dye lasers; a Fizeau wavemeter; a high-throughput

(f/4), high-resolution (<.001 nm)

spectrometer with an automated

intensified diode array detector; a 80-MHz quadrature He-Ne laser

interferometer; uv spectrometers;

grazing incidence spectrometers;

laboratory computers; and miscellaneous optics. The principal

quantities measured are particle

density distributions—both

spatially and temporally—for

electrons, atoms, ions, and

molecules. Also included are

electric-field distributions,

electron and ion temperatures,

and non-equilibrium phenomena.

CONTACT: James R. Roberts

AI67 Physics

(301) 975-3225

EBIT FACILITY FOR

RESEARCH ON HIGHLY

IONIZED ATOMS

NIST's new electron beam ion trap

(EBIT) source provides many

opportunities for definitive measurements aimed at a basic understanding of plasma processes and

atomic structure. Ions can be

generated over a wide range of

species and charge states (ultimately up to fully stripped

uranium). Ions are radially

trapped and probed with a monoenergetic electron beam. Electrostatic end caps confine the ions

axially. A large magnetic field is

applied by a superconducting magnet to pinch the electron beam to high density and provide additional radial trapping. The carefully controlled conditions in EBIT

allow scientists to unravel complex collision processes and measure spectra to very high accuracy. Highly charged ions can

be produced at low temperatures

and observed in fluorescence with

adequate brightness. The ion

temperature can be further

lowered by evaporative cooling

techniques. A variety of instru- ments are available to characterize and probe the trapped ions,

including X-ray spectrometers and

a new laser system.

CONTACT: James R. Roberts

(301) 975-3225

John D. Gillaspy

(301) 975-3236

A 167 Physics

RADIOMETRIC

PHYSICS

LUMINESCENCE

SPECTRAL RADIOMETRY

Luminescence techniques have

broad application in virtually

every scientific field, including

radiation measurement, remote

sensing, quantitation of biomolecules by intrinsic luminescence and immunoassay

techniques, and characterization

of laser, semiconductor, and super- conductor materials. The accurate

spectral radiometric quantitation

Above. Physicist James

Roberts observes the optical emission from a plasma

discharge generated in a radio-frequency reference

cell. Right. Physical scientist Stephen Ebner analyzes

data from the NIST Low

Background Infrared Radiation Facility where blackbody, infrared sources are

calibrated. These sources,

in turn, are used to calibrate infrared detectors.

of light emission is an exacting

task requiring painstaking

radiometric measurements and

knowledge of the fundamental

chemical and physical processes

represented by these radiative transitions. Standard lamps, both

radiance and irradiance, and

silicon detector radiometry provide

the accuracy base for the spectral

and quantum efficiency measurements. Luminescent phenomena

under investigation at NIST are

photo-, chemi-, thermo-, electro-, and bio-luminescences. NIST researchers are conducting luminescence radiometric research in the

near-ultraviolet, visible, and nearinfrared spectral regions and are

developing accurate standards and

measurement procedures for these

regions. Facilities available for

this research include various laser and lamp sources, the NIST refer- ence spectrofluorimeter, and a lowlight-level spectroradiometer now

under construction.

CONTACT: Ambler E. Thompson

B306 Metrology

(301) 975-2333

THERMAL

RADIOMETRY

NIST researchers are investigating

the use of thermal imaging cameras as a temperature-measuring

tool. These devices may prove to

be very useful in determining the

quality of products and in investigating changes in different

48
processes. Research projects

involve the development of largearea blackbodies, use of Pt-Si as

detector standards, and the characterization of thermal imaging

cameras. Equipment available includes several heat-pipe blackbodies, a Pt-Si camera, and an

infrared radiometer.

CONTACT: Robert Saunders

A221 Physics

(301) 975-2355

UV RADIOMETRY

The measurement of terrestrial

solar irradiance in the uv-b

spectral region is being investigated by NIST researchers in

order to provide improved tech- niques and standards in this

region. Their work is of importance not only to scientists studying biological effects but to

researchers investigating the aging of materials by uv light.

Specific projects include the development of a reference

spectral, radiometer, broadband

detectors, and source standards in

the region. A high-accuracy

spectrometer, standard detectors,

and standard sources are available.

CONTACT: Robert Saunders

A221 Physics

(301) 975-2355

SPECTRAL

RADIOMETRY

Research and development

programs at NIST span a broad

spectrum of activities associated

with the measurement of optical

radiation, including spectral

radiance measurements and new

techniques for spectrophotometric

measurement of dense optical

media. These activities cover the

ultraviolet spectral region from

200 nm to the far infrared region

and include the development of appropriate detector methodology to perform the measurements and relate them to the U.S. radiometric

measurement base. Specific re- search and development projects

involve low-background infrared

calibrations in a cryogenic en- vironment, solid-state photodiode

metrology, applications of detector metrology to all areas of radiometry, development of an absolute cryogenic radiometer, and

application of laser heterodyne

technology to optical density

measurement.

Several well-equipped

laboratories for optical measure- ments in the uv and visible

spectral region are available for

use, and new facilities are being

developed that will enable scientists to research both detector development and optical properties of materials in the infrared

spectral region.

CONTACT: Albert C. Parr B306 Metrology

(301) 975-3739

INFRARED SPECTRAL

RADIOMETRY

NIST researchers are developing

devices and techniques for highprecision measurements of radiant

power in the 2 \xm to 30 |im

spectral region to enable characterization of infrared spectral

sources, optical components and

detectors. Novel experiments using

these capabilities will investigate

physical and chemical processes

in materials and molecular structures. State-of-the-art radiometers,

a cryogenic blackbody with multiple apertures, lead salt lasers,

spectral instrumentation, and

solid-state infrared detectors are

being acquired for experiments. A

unique low background infrared

radiation (LBIR) facility is dedicated for this research and development effort.

Ancillary research projects in

progress are measurements of optical density of filters using laser heterodyne technology and deter- mination of spatial uniformity

and linearity in the response of infrared detectors. Collaborative research opportunities exist in

optical properties of materials and

molecular structures in the infrared spectral region and in detector development.

CONTACT: Raju Datla

A221 Physics

(301) 975-2131

BIDIRECTIONAL

SCATTERING METROLOGY

The bidirectional characterization

of optical scatter from surfaces is a

useful diagnostic in evaluating ele- ments contained within large optical systems that require the minimization of scattered light.

This information is needed for the development of ring-laser gyroscopes, telescopes, and superpolished mirrors. It is also used for

the characterization of materials

for use in stray light reduction in thermal control and inspection

processes in optical manufacturing settings. NIST research projects involve the development of a

multiangle scattering reference instrument and the development of measurement methodologies and

Standard Reference Materials for

the spectral range from the

ultraviolet to the infrared region.

CONTACT: JackJ. Hsia

B306 Metrology

(301) 975-2342

QUANTUM

METROLOGY

STUDY OF ATOMIC

STRUCTURE OF MATTER

WITH X-RAYS

X-ray spectroscopy provides infor- mation on electronic structure and on the local atomic structure

of atoms in matter. A synchrotron

radiation beamline has been constructed by NIST scientists at the

National Synchrotron Light

Source, providing the highest flux,

intensity, and energy-resolving

power of any existing beamline in

the X-ray energy range from

500 eV to 5000 eV. NIST equipment complements the

synchrotron radiation instrumentation. X-ray absorption spectros- copy techniques, such as X-ray

absorption near-edge structure and extended X-ray absorption

fine structure, have been used to determine the atomic structure of

metals, semiconductors, polymers,

catalysts, biological molecules,

and other materials of interest to

industry. Researchers also use

X-ray emission spectroscopy, X-ray

photoelectron spectroscopy, and

Auger electron spectroscopy to

probe the electronic structure of

solids, liquids, or gases. The X-ray standing-wave technique uses interference between incident and diffracted X-rays to determine the precise location of

impurities or imperfections within

a crystal or at its interfaces. The

technique can be used with semiconductors or optical ciystals,

growth of overl avers on ciystals,

and the structure of catalysts supported on cr\'stal substrates. In addition, evanescent X-rays, which

49 PHYSICS
COOPERATIVE RESEARCH OPPORTUNITIES

penetrate only a few nanometers

from an interface, can be controlled to study chemical composition in the vicinity of an interface. NIST scientists recently

pioneered a new technique, diffraction of evanescent X-rays, which

combines and extends the

capabilities of the X-ray standing- wave method and experiments

based on evanescent X-rays. The

synchrotron radiation beamline

provides an ideal facility for applying these techniques.

CONTACT: Richard D. Deslattes Al4l Physics

(301) 975-4841

IONIZING

RADIATION

RADIATION PROCESSING

To enhance quality-control

methods used in industrial radiation processing of foods and in the production and use of medical

devices, electronic components,

and polymers, NIST researchers

are developing standardization

and measurement assurance methods related to industrial highdose applications of ionizing

radiation. As part of this program.

Institute scientists are investigating radiation chemical

mechanisms and kinetic studies

applied to chemical dosimetry sys- tems in the condensed phase, including liquids, gels, thin films,

and solid-state detectors. They also plan to examine sensor materials, such as doped plastics, solid-state matrices, fiber

optics, organic dye solutions, semiconductors, scintillators, amino

acids, metalloporphyrins, and organic or inorganic radiochromic

and luminescent aqueous solutions and gels. A number of

analytical methods will be used,

including transmission and

fluorescence spectrophotometry,

electron spin resonance

spectrometry, and chemiluminescence spectrophotometry, as well

as optical waveguide analysis,

microcalorimetry, pulse radiolysis,

laser-induced photochemistry, and

conductivity measurements.

Various X-ray and gamma-ray

sources and electron accelerators with energies in the 0.1-MeV to 10-MeV range are used in this work. Conventional ultraviolet,

visible, and infrared spectrophotometers and spectrofluorimeters, high-intensity

gamma-ray sources, pulsed and

continuous beam electron accelerators, and organic-chemical

analytical equipment are also

available.

CONTACT: William L. McLaughlin

C229 Radiation Physics

(301) 975-5559

INDUSTRIAL

RADIOLOGIC IMAGING

The use of penetrating radiation

for imaging is one of the most

powerful investigative techniques

available to industry for maintaining or improving the quality of

products. Designers, aware of this,

are creating components that

facilitate such non-destructive testing. Research is under way at NIST to allow better quantification of radiographic images. Particularly relevant to image

evaluation are computer-based sys- tems that permit pseudo three- dimensional images and the implementation of image processing on these or traditional images

in real time or near real time.

Physicist Charles Olck

aligns an X-ray detector for

characterizing a multiplefocal-spot tomographic

X-ray source. Such sources can be used to produce

three-dimensional dental images that may soon improve

selection of appropriate

treatments for periodontal

disease.

NIST research focuses on

image processing for improved imaging of low contrast for noisy images; adaption of tomographic

equipment to industrial needs and

measurement of the performance

characteristics of such systems;

and development of reliable tech- niques for image storage and

retrieval. Available equipment includes X-ray sources, low-energy

electron accelerators, gamma-ray

sources, and state-of-the-art

radiologic imaging devices.

CONTACT: Charles E. Dick

C229 Radiation Physics

(301) 975-5580

NEUTRON FLUENCE

MEASUREMENT AND

NEUTRON PHYSICS

NIST researchers are studying industrial applications of neutron

fluence and dose determination in

the neutron energy region from

thermal to 20 MeV. They are

developing effective methods to

transfer personnel protection tech- nology to the private sector. This

research provides a basis for standardizing personnel protection

control procedures in nuclear reactor and high-energy accelerator

operations. Specific research involves the measurement of reference standard neutron reaction

cross sections; characterization of

reference fission deposits; development of neutron detectors with

fast timing; and calibrations using

standard neutron and gamma-ray

fields. Equipment available

includes a 100-kV ion generatorbased 2.5-MeV neutron source, a 3-MV pulsed positive-ion accelerator, and a 20-MW nuclear

reactor.

CONTACT: Oren A. Wasson

C229 Radiation Physics

(301) 975-5567

50
TIME AND

FREQUENCY

FREQUENCY, TIME,

AND PHASE NOISE

MEASUREMENT

Advancements in communication

and navigation systems require

atomic oscillators with increased

performance and reliability. NIST

has several programs aimed at providing advanced frequency

standards with the potential for

benefiting commercial atomic

standards. NIST scientists currently are working on an optically

pumped cesium-beam standard

that should significantly surpass

the performance of standards

based on magnetic-state selection and detection. Their studies on ion

storage and radiative cooling are

exploring the potential for standards operating at accuracy levels

of 1 part in 10^^ and beyond.

Aerospace systems often require extreme phase stability, which has

led to a need for high-quality

phase noise characterization of

amplifiers, frequency multipliers,

oscillators, and other electronic

components. NIST has initiated a program to develop methods for measuring phase noise in such

components over a broad fre- quency range (into the millimeter

range). The work will involve primarily the two-oscillator technique, but other techniques will be

studied. Requirements for synchronization (time) and syntonization

(frequency) of broadly dispersed

sets of nodes for communication,

navigation, and other electronic

systems are increasing significantly. Because of the inherent

reliability, simplicity, and low cost

of using satellite transfer, NIST is studying several possible ap- proaches for using this technique.

The NIST time scale and reliable

ties to many other international

timing centers provide the basis

for performance analysis of these

time-transfer techniques. In addition, the Institute is equipped with

Global Positioning System

receivers. Earth communication

terminals, and automated systems

for statistical analysis of system

performance.

CONTACT: Donald B. Sullivan

Div. 847

Boulder, Colo. 80303

(303) 497-3772

QUANTUM PHYSICS

LASER STUDIES OF

SEMICONDUCTOR

MATERIALS

Optical/laser probing of the gas phase species involved in the molecular beam epitaxial (MBE)

growth of III-V semiconductor materials is an area of high potential

relevance for standards and technology. Work under way has

demonstrated sensitive, direct

laser detection methods for study

of Ga and In atoms and arsenic

species during GaAs growth. It will

soon be possible to consider minor

dopant species such as phosphorous and impurities, for example, carbon monoxide. With the

incorporation of non-invasive

Electrical engineer John

Lowe adjusts a laser system

for NIST-7, the latest

generation in a series of ex- tremely accurate atomic

clocks developed at NIST.

laser probes into advanced generations of MBE machines, researchers will be able to carry out

in-situ diagnostics to quantify and

characterize the growth process, to provide optical feedback for adjustment of species concentrations,

and to determine the purities of

materials used during semiconductor fabrication.

In related experimentation,

laser vaporization of thin films is used to produce sources of translationally energetic species for etching and deposition studies. Thermal chlorine molecules

produce little or no etching of

silicon materials, whereas etch

rates increase dramatically with

increasing kinetic energy, with an

apparent threshold. New research

will also explore the kinetic energy dependence of film growth by

using velocity selected beams of

refractory materials and insulators.

CONTACT: Stephen R. Leone

JILA

Boulder, Colo. 80303

(303) 492-5128

LASER

STABILIZATION

Many sensitive and sophisticated

applications of lasers depend on

the laser's spectral coherence,

frequency stability, and lowintensity noise. NIST scientists have been working on laser intensity stabilization, laser frequency

linewidth reduction with active

control techniques, and several methods for producing quantitative laser frequency scans. Two new systems have been

developed. One, based on optical

51 PHYSICS
RESEARCH

FACILITIES

sideband production by broadband

microwave phase modulation of

the laser, allows scans over a GHz

range, with inaccuracy below

10 kHz. The other scan technique

utilizes a novel interferometer/

phase-locked rf system. The system

maps optical frequency change

into the corresponding phase

change of an rf signal suitable for

control, stabilization, and scanning. Another NIST system under

development works entirely externally to a continuous-wave laser

to shift the output laser frequency

and reduce the intensity in a controlled manner.

CONTACT: John L. Hall

JILA

Boulder, Colo, 80303

(303) 492-7843

SILICON

THIN FILMS

Thin films of amorphous silicon

are used in photosensitive devices,

displays, and in photovoltaic cells.

Scientists are examining physical

and chemical mechanisms involved in discharge and thermal

chemical vapor deposition (CVD)

production of such films. A scan- ning tunneling microscope is used

to examine in situ the morphology

and chemical character of asdeposited films. All electronics,

vacuum, and gas-handling ap- paratus necessary for producing

and diagnosing discharge and

thermal CVD films under controlled conditions are available.

CONTACT: Alan C. Gallagher

JILA

Boulder, Colo. 80303

(303) 492-7841

SYNCHROTRON

ULTRAVIOLET

RADIATION FACILITY-II

The Synchrotron Ultraviolet Radiation Facility-II (SURF-H) is a 300-MeV electron storage ring that

radiates synchrotron radiation

which is highly collimated, nearly

linearly polarized, and of calculable intensity. Seven beamlines

are available, and a users' pro- gram is in operation. SURF-II is

well-suited for studies in

radiometry; atomic, molecular,

biomolecular, and solid-state

physics; surface and materials

science; electro-optics; and surface chemistry and radiation effects on

matter. Special facilities are available for developing and testing

soft X-ray optics and optical

devices.

CAPABILITIES: The typical storage

ring electron beam current is 200 mA at 284 MeV. The photon

intensity in the region 60 nm to 120 nm is about 3 x lo'^ photons

per second per milliradian of orbit

for an instrumental resolution of

0.1 nm. Experiments can be conducted conveniently throughout

the wavelength range 4 nm to 1000 nm, from the soft X-ray

region to the infrared. A normal

incidence, a grazing incidence.

and several toroidal grating

monochromators are available to

disperse the radiation. A large,

ultrahigh vacuum spectrometer

calibration chamber, 1.2 m x

1.2 m X 2.5 m and accessible through a clean room, is available

for radiometric applications in a

clean, vacuum environment. A

6.65-m, normal-incidence vacuum spectrometer, with resolving power of about 300,000, is

available on a beamline dedicated

to high-resolution vacuum

ultraviolet radiation research.

APPLICATIONS: The continuous

radiation from SURF-II is used as

a national standard of spectral irradiance for radiometric applications and for fundamental

research in the following areas; atomic and molecular absorption spectroscopy;

optical properties of materials;

electron density of states in

solids;

surface characterization;

photoelectron spectroscopy;

molecular kinetics and excitation and ionization dynamics; and

radiation interactions with matter (such as lithography,

radiation damage, dosimetry,

photobiology).

AVAILABILITY: Beam time on

SURF-II is available to any

qualified scientist if beamline vacuum requirements are met and

scheduling arrangements can be

made. Proposals should be submitted for NIST review before use

of the facility is desired. Informal

contact is also encouraged.

CONTACT: Robert P. Madden

B119 Radiation Physics

(301) 975-3726

LOW-BACKGROUND

INFRARED RADIATION

FACILITY

In the Low-Background Infrared Radiation Facility (LBIR), radiant

background noise levels less than

a few nanowatts are attained in a

large (60-cm-diameter x 152-cmlong) vacuum chamber by cooling

internal cryoshields to temperatures less than 20 K using a closedcycle helium refrigerator system.

An absolute cryogenic radiometer

(ACR) of the electrical substitution type that operates at 2 K to 4 K is housed in the chamber.

CAPABILITIES: The ACR is a broadband detector with a flat response from the visible to the long

wavelength infrared spectral

A schematic of the

Synchrotron Ultraviolet

Radiation Facility-II.

52
region. It can measure power

levels of 20 nw to 100 |iw at its 3-cm-diameter aperture within an

uncertainty of less than 1 percent.

The ACR has a resolution of 1 nanowatt, and its time constant is about 20 s.

APPLICATIONS: This unique

facility can be used to measure

total radiant power from sources such as cryogenic blackbodies. Ongoing improvements will allow

measurement of the spectral distribution of radiation from sources and characterization of infrared

detectors and optical components.

AVAILABILITY: The facility is

operated by NIST staff in support

of user infrared calibrations. It is

available for collaborative research by NIST and outside scientists in areas of mutual interest.

CONTACT: Raju Datla

A221 Physics

(301) 975-2131

ELECTRON

PARAMAGNETIC

RESONANCE FACILITY

NIST is leading a national and

international effort in electron paramagnetic resonance (EPR)

dosimetry for measuring ionizing

radiation. Paramagnetic centers (molecules/atoms with unpaired

electrons) are produced by the action of radiation on materials. In

the EPR experiment, irradiated

materials are placed in a magnetic field and electron spin transitions are induced by an

electromagnetic field of the appropriate frequency (typically

GHz). EPR is used as a nondestructive probe of the structure and concentration of paramagnetic centers. The centers created

by ionizing radiation are proportional to the absorbed dose and

Top right. Physical scientist

Jacqueline Calhoun makes

an activity measurement of a gamma-ray-emitting

sample by placing it in the

NIST "47i"y ionization Chamber." Bottom right. Precise

measurements of absorbed

radiation dose for industrial

and medical applications can be made at the NIST

Electron Paramagnetic

Resonance Facility. Here,

physical science trainee

Francoise Le inserts a bone

fragment into the sample

chamber.

provide a sensitive and versatile measurement method.

CAPABILITIES: The EPR dosimetry

facility is supported by a state-ofthe-art X-band EPR spectrometer

capable of measuring radiation effects on a wide range of materials

from inorganic semiconductors to

biological tissues. The recently

upgraded data acquisition system

provides full computer control of

all spectrometer functions, including real-time spectral display and

rapid acquisition scan to analyze

rapidly decaying signals. The data

acquisition system is interfaced

with an advanced data analysis

station for data manipulation and

is capable of simulating and

deconvoluting multicomponent

spectra.

APPLICATIONS: EPR dosimetry is

operable over several orders of magnitude in absorbed dose

(10"^ Gy-10^ Gy) and impacts

many facets of society and industry. Areas of impact include:

Radiation Protection/Accident

Dosimetry. Using biological

tissues (bone, tooth enamel) or

inanimate materials (clothing),

retrospective dose assessment and

mapping can be accomplished.

Clinical Radiology. Ionizing

radiation doses administered in cancer therapy can be measured

for external beam therapy using

dosimeters of crystalline alanine

(an amino acid) or validated for

internally delivered bone-seeking

radiopharmaceuticals using bone

biopsies.

Industrial Radiation Processing.

Routine and transfer dosimetry for

industrial radiation facilities can

be performed using alanine dosimeters, as well as post-irradiation

monitoring of radiation-processed

meats, shellfish, and fruits using

bone, shell, or seed.

The EPR facility also serves as a fully functional materials research facility for analyzing radiation effects on semiconductors,

optical fibers, functional

polymers, and composites.

AVAILABILITY: The EPR facility

is available for collaborative research by researchers from industry, academia, and other

government agencies under the

supen'ision of NIST staff.

CONTACT: Marc F. Desrosiers

C229 Radiation Physics

(301) 975-5639

53 PHYSICS
RESEARCH FACILITIES

RADIOPHARMACEUTICAL

STANDARDIZATION

LABORATORY

Radioactivity measurements for

diagnostic and therapeutic

nuclear medicine in the United

States are based on measurements

at NIST. Activity measurements for

the gamma-ray-emitting

radionuchdes are made using the NIST "471" Y

ionization chamber.

The calibration process also includes identification of radionuclidic impurities by germanium

spectrometry. Recent development

work has focused on therapeutic

nuclides for nuclear medicine,

radioimmunotherapy, and bone

palliation.

CAPABILITIES: The radiopharmaceutical standardization

laboratory provides calibration service for the gamma-ray-emitting

radionuclides and is available for

technical users who must make

measurements consistent with national standards or who require

higher accuracy calibrations than

are available with commercial

standards. NIST also undertakes basic research to develop new methods of standardizing radionuclides for

diagnostic and therapeutic applications. These studies include

measurements of decay-scheme

parameters, such as half lives and

gamma-ray emission probabilities, and identification of

radionuclidic impurities.

AVAILABILITY: The customer has no direct use of the facility. NIST

staff can provide calibration services for the gamma-ray-emitting

radionuclides that comply with

the specifications as stated in NIST

Special Publication 250-10.

Research associates of the United

States Council for Energy Awareness distribute radiopharmaceutical Standard Reference Materials.

CONTACT: Jacqueline M. Calhoun

Cll4 Radiation Physics

(301) 975-5538

MAGNETIC

MICROSTRUCTURE

MEASUREMENT FACILITY

The magnetic microstructure of

materials can be measured with

very high spatial resolution by a

technique called scanning

electron microscopy with polarization analysis (SEMPA). An

ultrahigh-vacuum electron microscope has been modified so secon- dary electrons from the sample can be analyzed for their electron

spin polarization. This allows for

a measurement of the surface magnetism with moments both in

the plane and perpendicular to the plane of the sample.

CAPABILITIES: SEMPA allows the simultaneous observation of surface microstructure and surface magnetic domains at a resolution

of 0.05 \im, using an innovative,

extremely compact electron spin

detector invented at NIST.

APPLICATIONS: This unique

measurement facility can be

used for research in magnetic thin

films, high-coercivity magnetic

materials, high-density magnetic

storage media, and other advanced magnetic materials.

AVAILABILITY: These facilities are

available for collaborative research by NIST and outside scientists in areas of mutual interest on

a time-available basis.

CONTACT: Robert J. Celotta B206 Metrology

(301) 975-3710

Using a scanning electron

microscope with polarization analysis, physicist

Mike Kelley examines magnetic microstructures of

magnetic materials such as

the recording media used in computer disks.

54
MATERIALS SCIENCE

AND ENGINEERING

LABORATORY

Covering all classes of advanced materials, as well as

conventional structural materials, the laboratory's

research programs address the full range of issues in

materials science and engineering—those related to design, synthesis, processing, performance, instrumentation, and analysis and modeling. A unifying aim is to acquire the knowledge and tools needed for intelligent

manufacturing methods with real-time automated process

controls.

Separate research initiatives address ceramics, metals,

polymers, composites, and superconductors. This re- search supports U.S. industry efforts to develop reliable,

low-cost manufacturing methods for producing tailormade materials and products with superior properties.

Through laboratory-organized consortia and one-to-one

collaborations, NIST's materials scientists and engineers

work closely with their counterparts from U.S. industry.

For example, one consortium is developing a computercontrolled system for intelligently processing rapidly

solidified metal powders. The research involves development of an integrated system to control particle size in

real time. Other collaborations are developing nondestructive evaluation sensors for aluminum and steel

processing.

The Materials Science and Engineering Laboratory is also

strengthening its research relationships with manufacturers of high-technology products, the major users of advanced materials. On the basis of discussions with U.S.

microelectronics firms, it has launched new programs to improve materials for semiconductor packaging.

Contact: Lyie H. Schwartz

B309 Materials

(301) 975-5658

COOPERATIVE

RESEARCH

OPPORTUNITIES

INTELLIGENT

PROCESSING

OF MATERIALS

INTELLIGENT SENSORS,

CONTROLS, AND

PROCESS MODELS

Advanced materials are capable of providing outstanding properties,

but they generally require unusual

processing operations and tend to

be expensive. Intelligent process- ing offers the potential to design

and produce materials with substantially improved quality,

reduced lead time, and increased

flexibility in production.

Intelligent processing incorporates four principal elements in- cluding materials processors,

non-destructive evaluation sensors

that can measure physical and

mechanical characteristics of

materials in real time during processing, rigorous models to describe

the materials production process, and expert systems to control the production process in real time

through integration of sensors and

process models.

Research sponsored by the Office of Intelligent Processing of

Materials is directed to process

models, sensors, and intelligent

control systems. Research topics

include processing modeling, sensing and control of the production

of metal powders by high-pressure

gas atomization, measurement

and control of steel sheet texture, magnetic methods for measuring

An ultrasonic sensor developed by physicist Ray

Schramm can be embedded

in train tracks to detect

cracks in railroad wheels as

a train rolls by.

55
COOPERATIVE RESEARCH OPPORTUNITIES

mechanical properties, ultrasonic

measurement of interfaces,

powder-particle-size sensing, inspection of electronic components.

X-ray radioscopy standards,

fluorescence spectroscopy in polymers processing, magnetic

resonance imaging and ESA for ceramic processing, eddy-current

sensing in metals and composites,

and laser ultrasonic methods.

CONTACT: H. Thomas Yolken

John P. Gudas

B344 Materials

(301) 975-5727

CERAMICS

CERAMIC

PROCESSING

Sintering of ceramics is a complex

process that involves the interaction of many different processing

variables. The influence of these

processing variables on sintering cannot be determined simply by

measuring final density or some

other end-point property. Chemical composition of the ceramic

powders is known to be of major

importance and, under certain

conditions, can mask effects of most other processing variables. NIST scientists are investigating

the effect of trace levels of impurities using clean-room processing to produce, compact, and

sinter ultrahigh purity ceramics.

Results from this research will enhance investigations of other

processing variables, including

particle size, shape, agglomeration, compaction method, and

atmosphere under controlled composition conditions. The data can

be used to design better models for

microstructure evolution during

sintering. Use of predictive

models, in conjunction with other

ongoing efforts to produce unique

compositions and phases, can lead

to new advanced ceramic materials with unique microstructures

and properties.

CONTACT: John E. Blendell A215 Materials

(301) 975-5796

TRIBOLOGY

OF CERAMICS

Researchers in the NIST ceramics

tribology program are investigating the fundamental mechanisms

of friction and wear of advanced

Top left. Research chemist

Pu Sen Wang uses a nuclear

magnetic resonance instrument to determine the distribution of water and other

chemicals in a silicon

nitride slurry, a ceramic

material used to form advanced automotive engine

components. Top right. This

electrokinetic sonic amplitude instrument has been

adapted by NIST scientists

to measure the homogeneity

of ceramic slurries. Bottom.

Materials research engineer

Mark Austin uses an X-ray

diffraction apparatus at cryogenic temperatures to study phase transitions

in a high-temperature

superconductor.

materials and lubricants and are developing test methods for evaluating the performance of

these materials. The program's

primary focus is on the characterization of the interfacial phenomena that occur when two

solid surfaces interact. Research

activities include analysis of chemical reactions and formation

of tribochemical films, physical

and mechanical behavior of surface films, and deformation and

fracture processes leading to wear and failure. Tribology

laboratories consist of state-of-theart tribometers, such as hightemperature (1000 °C) wear

testers, and analytical instruments, such as time-resolved

micro-Raman laser systems,

which can be used for cooperative

research with industry and other

federal agencies.

NIST researchers are compiling

data in the form of "wear maps"

and computerized data, and are

studying the mechanisms for wear

of structural ceramics at elevated

temperatures, self-lubricating

metal-matrix and ceramic-matrix

composites, and wear-resistant

coatings.

CONTACT: Stephen Hsu

A256 Materials

(301) 975-6120

ELECTRO-OPTIC

CRYSTALS

Imperfections in highly perfect

crystals typically limit their performance in high-technology

applications, such as optical communications and optical signal

processing. In particular, limitations in the perfection of electrooptic and photorefractive

materials, such as lithium niobate

and bismuth silicon oxide, have
inhibited the development of optical switches and modulators.

NIST researchers are investigating crystal perfection at a unique,

monochromatic X-ray topography

facility at the NIST/Naval Research Laboratory beamlines on

the high-energy ring at Brookhaven National Laboratory's National Synchrotron Light Source

in New York. Conducted jointly

with growers of high-quality crystals, current studies are expected

to improve substantially the quality, and hence the performance, of

these crystals.

CONTACT: Bruce W. Steiner

A256 Materials

(301) 975-5977

MECHANICAL PROPERTIES

OF CERAMICS

Several long-term programs are

being conducted at NIST on the

fracture, creep, and creep rupture

of monolithic and composite

ceramics. Researchers, for example, are examining the effect of

veiy near surface forces on the

fracture properties of monolithic

ceramics. These forces have been

measured for mica, sapphire, and

fused silica surfaces, using a

crossed cylinders apparatus. A second program uses an indentation strength procedure to

determine the fracture toughness

(R-curve) behavior of monolithic

alumina ceramics and to relate

the R-curve to the specific

microstructure of the material.

In-situ microscopic observations of

crack growth demonstrate the

presence of grain bridging and

frictional sliding in the crack

wake as a significant source of

material toughening.

A program in composites is aimed at determining the effects

of the fiber/matrix interface on

fracture behavior of these materials. An instrumented microindenter is available to measure

the fiber/matrix interface

strengths. Researchers also are investigating the stresses developed

in composites during conventional

sintering processes to determine

methods of reducing these stresses through the use of fiber coatings—thus minimizing or eliminating cracking of the matrix as densification proceeds.

High-temperature deformation

and fracture behavior of ceramics

are other areas of research. Creep

and creep rupture of several

varieties of siliconized SiC have

been investigated and their behavior related to differences in

microstructure, particularly grain

size. Research continues on

whisker-reinforced Si3N4 and

AI2O3, SiC, and other hightemperature materials. Facilities

exist for performing creep measurements in tension, compression,

and flexure at temperatures up to

1800 °C. The tensile creep apparatus is almost completely

automated, and measurements are made using a laser-imaging technique. Displacement measure- ments are accurate to ±1 |im at

1500 °C.

CONTACT: Joseph A. Carpenter

A256 Materials

(301) 975-6119

CERAMIC PHASE

EQUILIBRIA

Ceramic phase equilibria studies

at NIST involve complementary research activities in experimental,

theoretical, data evaluation, and

compilation aspects of ceramic

phase equilibria. The dataevaluation and compilation work

is carried out under the joint

American Ceramic Society/

NIST program to provide industiy

and others with a comprehensive

database of up-to-date, critically

evaluated phase-diagram information. Ceramic phase diagrams

are also being determined experimentally for systems of technical importance, such as

high-transition-temperature

ceramic superconductors.

CONTACT: Stephen Freiman

A256 Materials

(301) 975-5761

CERAMIC

CHEMISTRY

NIST scientists are investigating

low-temperature synthetic ap- proaches to both oxide and nonoxide ceramic powders and

coatings. They are using novel

chemistry and techniques to solve

the problems of generating

homogeneous, multicomponent

materials with predictable and optimal properties. The researchers

are studying the following materials: high Tc ceramic superconductors; ultrafine ceramic powders

with high-electrical conductivity;

ceramic coatings with selected optical, electronic, or structural

properties; ultrafine magnetic

composites; ceramic whiskersceramic matrix composites; and

ultrafine, pure oxide powders.

Depending upon requirements of

the study and the powder, synthesis is carried out either in small

bulk reactors or in a flow reactor. The researchers are examining

the relationship of process conditions to surface chemistry of the

powder, particle size and shape,

the phases formed during thermal

treatment of the powder, and

properties of the powder or

sintered ceramic, such as electrical conductivity. Coupled with the powder synthesis is the development of characterization methods

involving nuclear magnetic

resonance spectroscopy.

CONTACT: Joseph R. Ritter

(301) 975-6106

Pu Sen Wang

(301) 975-6104

A256 Materials

MATERIALS

RELIABILITY

NON-DESTRUCTIVE

EVALUATION

NIST scientists are developing

acoustic and electromagnetic sensors for material characterization,

including electromagneticacoustic transducers (EMATs)

,

arrays of piezoelectric polymers,

and eddy-current and capacitive

probes.

EMATs are used for noncontacting applications, where it

is not possible to have an intervening material couple sound from

transducer to specimen. For example, an EMAT embedded in a

rail is used to inspect railroad

wheels for cracks in a roll-by

mode. Researchers are investigating the possible use of EMATs at

the input to an automated press

shop, where automobile body parts

are formed. Formability me;isurements could be made on moving

sheet, and materials with improper formability would be

rejected from the production line.

57 MATERIALS SCIENCE AND ENGINEERING
COOPERATIVE RESEARCH OPPORTUNITIES

Acoustic arrays are useful in medical imaging, where their unique advantages allow suppression of artifacts to give better image quality. Research is being

conducted by NIST to use these

techniques to characterize composites. Various types of arrays are being constructed and interfaced with signal processing devices. NIST scientists have developed

eddy-current probes and techniques for detecting and sizing

small defects that could prove to

be critical in aircraft and other

structures. Capacitive probes are being investigated as a noncontacting means to monitor

sintering of ceramics, with possible use for quality control of substrates for semiconductor devices.

CONTACT: Alfred V. Clark

Div. 853

Boulder, Colo. 80303

(303) 497-3159

THERMOMECHANICAL

PROCESSING

Metals producers and manufacturers rely heavily on pilot-scale

or production facilities for the development of new alloys or new

manufacturing schedules. This is not only expensive but can also

yield unreliable results. These

processing problems can be alleviated by using a more economical, versatile, and reproducible

Above right. A computer

model created by NIST materials scientists describes in three-dimensions the flow

of a polymer into a mold

containing reinforcing

fibers. Right. Improved un- derstanding of flow properties in molds like this one

will help manufacturers

produce strong, lightweight

automobile frames more

efficiently.

laboratory facility. Controlled

thermomechanical processing

offers the opportunity to produce

superior steels at lower cost due to

the elimination of post-heat treat- ment—an energy-intensive

process. NIST scientists and engineers

have designed and built a computerized, laboratory-scale, hot- deformation apparatus that can

simulate manufacturing processes, such as forging and plate

rolling, and measure important

properties incurred during processing. The apparatus can be used

to study static and dynamic recrystallization, high-temperature

deformation resistance in terms of

a true stress-strain curve at highstrain rates, and phase transformation characteristics. The apparatus

is used to characterize directly

cooled forging steel during simulated forging operations in an at- tempt to develop optimized steels and forging procedures.

CONTACT: Yi-Wen Cheng

Div. 853

Boulder, Colo. 80303

(303) 497-5545

CRYOGENIC

MATERIALS

Comprehensive low-temperature

facilities are available to conduct

both characterization testing and

fundamental studies on the mechanical and physical properties of high-strength structural alloys, high-conductivity metals and

superconductors, metal and

polymer-based composites, and

polymer foams.

Properties studied include

tensile strength, compression,

fatigue, creep, fracture toughness,

stress relaxation, elasticity

(ultrasonic), and thermal expansion. Strain sensitivities of lO"'' at

liquid helium temperature (4 K)

are now possible, permitting

precise low-temperature

microstrain measurements. Researchers are assembling equipment to permit load capacities of

5 MN for testing at 4.2 K.

CONTACT: Nancy I. Simon

Div. 853

Boulder, Colo. 80303

(303) 497-3687

WELDING QUALITY

RESEARCH

The integrity of welded joints is a

primary concern in the design and

fabrication of engineering structures. Researchers at NIST are investigating ways to improve the

fracture resistance of weldments

and are assessing weld quality by

non-destructive evaluation (NDE)

techniques. Specific goals of the research are to improve fracture toughness in the heat- affected zone of steel weldments and in the weld metal of materials for lowtemperature service and to im58
prove the soundness of welds

through increased understanding

of the metal transfer process in arc

welding. In addition, the researchers are applying fineresolution NDE techniques to

evaluate solder joints in printed

circuit boards for the electronics

industry. NIST scientists have

developed techniques to reduce

porosity in aluminum weldments,

to reduce spatter in gas metal arc welding of steels, and to predict accurately the ferrite number in

stainless steel welds. The NIST welding and NDE

laboratories house equipment for

shielded metal arc, gas metal arc, and gas tungsten arc welding;

radiographic and penetrant techniques for non-destructive evaluation of weldments; and a precision

power supply, high-speed photography, and laser-shadow techniques for metal-transfer studies.

CONTACT: Thomas A. Siewert

Div. 853

Boulder, Colo. 80303

(303) 497-3523

POLYMERS

PROCESSING SCIENCE

FOR POLYMER

COMPOSITES

Fiber-reinforced composites offer,

along with other advantages, versatility in processing combined

with high strength and stiffness at low weight. For the current growth

in the production of these materials to continue, however, more

rapid and reliable processing is

needed.

NIST researchers are developing new measurement tools to

characterize the starting materials

for composite processing and to

study in the laboratory the chemical and physical changes that occur during processing. The

scientific understanding that can be generated with these tools

will facilitate both advances in processing methods and implementation of on-line control and automation.

The infiltration of a resin into a fiber preform during processing

is the critical step in composite

fabrication by liquid molding.

Test methods to characterize the

resistance of the preform to resin

infiltration have been developed.

NIST is working with several companies including the Automotive

Composites Consortium (Ford,

General Motors, and Chiysler) to

characterize this resistance in a

variety of materials and use the

results in computer simulation

models to optimize the liquid

molding process.

In addition, NIST is developing measurement techniques to monitor the chemical, morphological, and molecular

changes that occur during processing. The program currently has

10 different spectroscopic,

dielectric, thermal, and mechanical techniques available for process monitoring, and others are under development. This diversity

of tools provides a unique

capability for evaluating and

calibrating new measurement

methods, for developing process

models, and for analyzing model

resin systems.

For example, through cooperative projects with NIST, several industries have selected and

developed monitoring methods for

their particular problems.

CONTACT: Donald L. Hunston

A209 Polymer

(301) 975-6837

POLYMER

STRUCTURE

Knowledge of the relationships be- tween mechanical properties of polymers and polymer structure is important to the design and processing of materials for optimal per- formance. Researchers at NIST are

studying semicrystalline polymers,

polymer glasses, elastomers,

molecular composites, and fibers

to develop improved models of mechanical behavior, characterize

structure from the atomic- to

fine-texture level, and elucidate

relationships between mechanical

performance and structure. NIST scientists use a variety of

techniques to characterize the

structure of polymers in the solid

state. Nuclear magnetic resonance

spectroscopy is used to determine

molecular orientation, molecular

dynamics, and microstructure on

the 1-nm to 10-nm scale.

Microstructural information is deduced from C-13 lineshapes obtained with magic angle spinning

or by proton "spin diffusion" experiments in which domain-size

information is inferred from the

rates at which proton magnetization diffuses in the presence of magnetization gradients. Fourier

transform infrared spectroscopy

helps to determine molecular architecture, orientation, and

molecular processes, such as meas- urement of the amount of chain

scission associated with mechanical deformation of polymers.

Microstructural features, including spherulytic morphologies,

lamellar texture, fiber structures, and ciystallization habits, are

elucidated through optical and

electron microscopic studies of

polymers.

NIST scientists are examining

the relationships between

mechanical performance of polymers and fine structures by investigating the morphological

changes that polymers undergo

when they are deformed. Wideand small-angle X-ray diffraction

techniques, which include the use

of position-sensitive detectors, are

also used in these investigations.

CONTACT: Bruno M. Fanconi

A309 Polymer

(301) 975-6770

DENTAL AND

MEDICAL MATERIALS

Modern dental and medical materials utilize numerous substances

in an array of combinations.

NIST has a comprehensive pro- gram aimed at increasing basic

understanding of the causes for

failure or poor performance of

these materials, proposing and

testing new material systems, and

transferring the resultant science

and technology to industry. The

program has the active participation of researchers from the American Dental Association, the

National Institute of Dental Research, dental industries, and

universities.

Researchers are working in a number of areas. For example, in

a tribology study, scientists are ex- amining wear and degradation of

materials in various environments. In addition, improved

resins are being synthesized to produce polymers that have improved properties, such as wear

resistance, higher strength, resistance to oral fluids, or X-ray

opacity. Researchers have

developed an in-mouth shield

for cancer patients undergoing

radiation therapy to protect

healthy tissues from secondaiy

59 MATERIALS SCIENCE AND ENGINEERING
COOPERATIVE RESEARCH OPPORTUNITIES

radiation emitted from metallic

restorations.

In an effort to improve the

strength of dental systems, different combinations of materials

are being designed and tested, including resin-matrix composites

and ceramic-metal, metal-cement,

cement-tooth, and compositeadhesive-tooth materials. New

monomers are being synthesized,

which are designed to reduce

polymerization shrinkage and/or

improve the degree of wear. Unique methods for determining

the effectiveness of coupling

agents and curing efficiency are being explored. Weibull statistical

analysis is employed to identify

the weakest links, and finite- element analysis is applied to

define stress states within systems.

CONTACT: John A. Tesk

Al43 Polymer

(301) 975-6801

ELECTRICAL AND OPTICAL

PROPERTIES

NIST is conducting a number of

studies on the electrical properties

of polymers. The research focuses on dielectric measurements,

fundamentals and applications of

piezoelectric and pyroelectric

polymers, measurement of space charge distribution within

polymer films, and electro-optic

properties of polymers.

Scientists have developed in- strumentation and data analysis

techniques to measure the

dielectric constant and loss of polymer films over a frequency

range of 10"^ Hz to 10^ Hz in less than 30 minutes. These developments make it possible to follow changes in the dielectric spectrum

as a function of time, processing

conditions, or other parameters.

The toughness, flexibility, lowdielectric constant, and an acoustic impedance close to water make

piezoelectric polymers ideal for many transducer applications.

NIST researchers have considerable experience with the fundamental properties of polymers

such as polyvinylidene fluoride and its copolymers and can work

with industry to develop

transducers for novel applications

or to assist in measuring the

properties of new piezoelectric

polymers or composites.

The scientists also have

designed instrumentation and

data analysis techniques to measure the charge or polarization distribution across the thickness of a polymer film by analyzing the transient charge response

following a pulse of energy on one

surface of the film. This technique

has been used to detect the

presence of non-uniform electric

fields in the poling of piezoelectric

polymers and currently is being

used to investigate the role of

space charge in the dielectric breakdown of polymer insulation. Organic molecules with highly

delocalized Ti-conjugated

electrons offer great potential in

the field of non-linear optics due

to their relatively large secondorder susceptibilities and their picosecond response times. The

orientation and stability of orientation of polar groups in polymers

containing these molecules are being investigated by measure- ments of dielectric properties and

polarization distributions.

CONTACT: George T. Davis

B320 Polymer

(301) 975-6725

MOLECULAR

NETWORKS

Thermoset resins are used extensively in practical applications,

especially polymer-based composites. However, knowledge of the

basic structural entity of these

resins, for example, their molecular network structure, is

very limited. NIST researchers have developed a neutronscattering technique that can be

used to determine quantitatively

characteristics of the network, in- cluding the average distance be- tween crosslinks, the rigidity of the

network, the molecular weight distribution between crosslinks, and

the topological heterogeneity of

the network structure.

Current NIST research focuses on developing correlations among

chemical compositions, processing

conditions, and resulting network

structure for epoxy-type polymers.

To establish processing-structureproperty relationships, these

materials are then evaluated to determine performance properties,

such as fracture behavior.

The neutron-scattering tech- nique also is being used to study

how the molecular network

deforms when the material is

placed under load. These studies

help industry by providing

guidelines for designing and

processing polymers for optimal

performance.

CONTACT: Wen-li Wu

A209 Polymer

(301) 975-6839

POLYMER

BLENDS

Blending polymers has become an

effective method for producing

high-performance engineering

polymers. The fundamental data

required to design a manufacturing process include the equilibrium phase diagram, the

energetic interaction parameter

(compatibility) between the blend

components, diffusion coefficients,

and the interfacial tension. At NIST, small-angle neutron

scattering has been used to measure the interaction parameter

and phase diagram of polymer

blends. NIST scientists have

developed forced Rayleigh scattering and temperature-jump lightscattering techniques to measure

polymer-polymer diffusion and

other parameters that control phase separation kinetics and

morphology.

Currently, researchers are testing various kinetic theories of phase separation and late-stage

coarsening and are studying the

control of morphology and

mechanical properties of microphase-separated polymer

blends. As part of this program,

they are working with industry to

study the homogenization and

phase coarsening of rubber blends.

CONTACT: Charles C. Han

B210 Polymer

(301) 975-6771

FLUORESCENCE

MONITORING

NIST researchers are using fluorescence spectroscopy to characterize

structural and dynamic properties

of polymers and to monitor the behavior of polymer flows during

processing.

Fluorescence quenching is

employed, for example, to monitor

the uniformity of mixing in polymer blends and in particlefilled polymer melts. Excimer

fluorescence is used to monitor

the cure of thermoset resins, to

60
detect crystallization and glass

transition temperatures, and to measure the temperature of polymers during processing.

Fluorescence anisotropy is used to measure molecular orientation

and to monitor the non- Newtonian flows of polymer

solutions and melts.

For polymer processing and

composites monitoring, optical

fibers are used to transmit fluores- cence and excitation light energy

between the processed polymer

and light source and detection

equipment. Well-equipped

laboratories containing laser light

sources, spectrofluorimeters and

a nanosecond spectrofluorimeter

are available for carrying out this

research.

CONTACT: Francis W. Wang

B320 Polymer

(301) 975-6726

METALLURGY

METALLURGICAL

PROCESS CONTROL

SENSORS

Special facilities at NIST enable

researchers to develop advanced

measurement methods and standards for application in process modeling and control for intel11

ligent processing of materials.

Measurement methods available

include ultrasound, eddy currents, and acoustic emission. In particular, non-contact ultrasonic

facilities featuring high-intensity

pulsed lasers and electromagnetic

acoustic transducers have been

designed.

Coupled with state-of-the-art

materials-processing equipment

and expertise, these facilities offer

a unique opportunity to ascertain

feasibility and develop prototype

specifications for a wide spectrum

of sensor needs, including the measurement of internal temperature, phase transformations,

surface-modified layers, porosity,

grain size, and inclusion/

segregate distributions.

CONTACT: Leonard Mordfin

B144 iVIaterials

(301) 975-6168

CORROSION DATA

PROGRAM

Corrosion is a major limiting factor in the service life and cost of many products, plants, and equipment. The costs of metallic corrosion to the U.S. economy are

estimated to be $218 billion in

1989 dollars, $33 billion of which

could be saved by using existing

technology.

The National Association of

Corrosion Engineers (NACE) and

NIST have joined together in a collaborative NACE/NIST Corrosion Data Program to reduce the enor- mous costs of corrosion. The focus

of this program is to establish an

evaluated corrosion database that can be accessed easily by computer

using intelligent interfaces to obSchematic of the Supersonic Gas Metal Atomizer.

tain data in a number of graphical, tabular, or textual formats. The researchers are developing

evaluation methodologies and a

prototype database for areas covering thermodynamic and kinetic

corrosion data. NIST scientists are emphasizing interactions with industry both to help set priorities

for data projects and as a source of

corrosion data for the database.

CONTACT: David B. Anderson

A109 Materials

(301) 975-6026

CORROSION

MEASUREMENTS

Electrochemical measurements

can give important information

about the chemical processes causing the corrosion and the rate of

corrosion as well as its forms,

whether uniform or localized. Researchers at NIST are determining

current and potential and their

variations with time, measuring

the frequency spectrum of the

ac impedance of corroding

electrodes, and detecting and

analyzing random fluctuations of

electrical parameters.

Electrochemical methods for measuring corrosion rates offer

the possibility of tracking the process in a non-destructive way and

assessing the effect of various en- vironmental variables. Other

electrochemical techniques can

shed light on the kinetics of the

corrosion reactions and on the

critical factors that may contribute either to catastrophic

failures or corrosion prevention.

CONTACT: Ugo Bertocci B254 Materials

(301) 975-6017

61 MATERIALS SCIENCE AND ENGINEERING
COOPERATIVE RESEARCH OPPORTUNITIES

FIELD CORROSION

OF METALS

The corrosion of metals in natural

and manmade environments is

very costly to industry and government. For several years, NIST researchers have been involved in developing methods for measuring

the corrosion of metals in field

conditions, such as steel piling in

soil and seawater, electric utility

lines in soil, and most recently,

steel in concrete. To measure the corrosion of

reinforcing steel in concrete

bridge decks, NIST scientists have

developed a small, portable computer system. With this system,

scientists are able to use

electrochemical techniques nor- mally limited to the laboratory to measure the corrosion. This new

approach, which allows faster, more accurate corrosion measurements, can be used to evaluate the

effectiveness of protection systems

in place. The system has been applied to several bridges in Maiyland and Washington state.

CONTACT: Edward Escalante

B254 Materials

(301) 975-6014

STEEL SLAG

THERMOCHEMISTRY

Thermochemical databases and

models are needed by the U.S. steel

industry for the design of new or improved steel-making processes. To design such processes, NIST researchers are involved in three programs: measuring refractory

and slag thermochemical equilibria; evaluating the scattered

literature data; and developing

computer models that relate ex- perimental data to industrial conditions. Unique experimental

facilities are available at NIST for

measuring key phase equilibria

and kinetics.

CONTACT: John W. Hastie B 106 Materials

(301) 975-5754

ENVIRONMENTALLY

INDUCED FRACTURE OF

ADVANCED MATERIALS

Corrosive reactions between the environment and advanced materials can dramatically alter the

fracture resistance of the material.

To assist in the development of ad- vanced materials, NIST scientists

are studying the mechanisms by

which environments can induce

crack propagation at stresses well below those which cause normal

fracture.

Researchers are developing ex- perimental techniques to evaluate

and quantify the susceptibility of

different types of advanced materials. Experiments are being conducted to investigate the mechanisms of hydrogen absorption, dissolution, and environmentally induced cleavage on different

types of materials, specifically lowdensity, high-strength Al-Li alloys;

intermetallic compounds; and

composites as well as simple

model systems.

CONTACT: Richard E. Ricker

B254 Materials

(301) 975-6023

MAGNETIC

MATERIALS

As part of the NIST program in magnetic materials, researchers

are studying the magnetic

properties of alloys and their

relationship to metallurgical

structure. Nanocomposites,

composition-modulated alloys.

high-temperature superconductors, metallic glasses, and

icosahedral crystals are among the

materials being investigated. The

magnetic properties are characterized by ac and dc (VSM and

SQUID) magnetic susceptibility

measurements, magnetocaloric

properties, Barkhausen noise,

magneto-optic Kerr effect, ferro- magnetic resonance and

Mbssbauer effect observations.

Applications are made to nondestructive evaluation.

CONTACT: Lawrence H. Bennett B152 Materials

(301) 975-5966

VAPOR-DEPOSITED

THIN FILMS

Obtaining new fundamental understanding of the detailed physics

and chemistry of thin-film formation from high-temperature vapor

sources is an objective of NIST researchers. This effort is currently

developing a laser-produced vapor

deposition facility, with measure- ment access for a variety of existing vapor diagnostics facilities. These in-situ facilities include

high-pressure sampling molecular

beam mass spectrometry, optical

multichannel emission spectroscopy, laser-induced fluorescence

spectroscopy, and optogalvanic effect spectroscopy. These diagnostic

techniques provide time-resolved,

species-specific gas-phase compositions during the gas transport

process.

In addition, film characterization facilities, including

magneto-optical Kerr effect, SEM

and TEM-based X-ray analysis,

and Auger/ ESCA are available.

Current plans are to extend measurements on film-producing en- vironments to conventional

sputtering conditions as well.

Films of current interest include

electronic, magnetic, and high Tc

materials.

CONTACT: John W. Hastie

BIO6 Materials

(301) 975-5754

REACTOR RADIATION

NEUTRON

NON-DESTRUCTIVE

EVALUATION

Neutron radiography has been a

well-established tool for nondestructive evaluation (NDE) for some time. More recent neutron

applications in NDE include neutron diffraction for texture and

residual stress determination. All

three of these specialties are available for cooperative research and

development at the NIST reactor.

In general, these techniques

parallel their X-ray counterparts;

however, in certain cases (such as where hydrogenous components

are critical, or subsurface texture

or residual stress distributions are

sought) X-rays do not provide the needed sensitivity or penetration.

NIST scientists are collaborating with scientists from the Smithsonian Institution to continue the examination of art works by neutron autoradiography. The

technique has also been applied to

industry-related problems, and efforts are being made to extend its

capabilities to, for example, cold neutron radiography. NIST and

Department of Defense (DOD)

scientists are continuing a

cooperative development and application of neutron diffraction to

62
texture and residual stress characterization. Texture studies have

centered on copper, tantalum, and

uranium-alloy components for a

variety of DOD end-items; recent work has included ceramic super- conductors. Neutron residual

stress studies have included components made of the above metals,

ceramics, fiber-reinforced ceramic

composites, and steel.

CONTACT: Henry J. Prask

(301) 975-6226

Chang S. Choi

(301) 975-6225

AlOO Reactor

NEUTRON

SPECTROSCOPY

The vibrational dynamics and

diffusion of hydrogen in metals

and molecular species in hetero- geneous catalysts, clays, and other

layered materials are studied at NIST with inelastic and quasielastic neutron scattering. The

results of this research reveal the bonding states and atomic-scale

interactions and diffusion paths in such materials. Recent progress has allowed in-situ spectroscopic

studies of hydrogen and molecular

species down to 0.1 of an atomic

percent.

These measurements can provide direct information, for ex- ample, on the molecular processes

that affect reaction and selective

release of chemicals in industrial

catalysts and on the local trapping

and clustering of hydrogen in metals and semiconductors, which

cause embrittlement, corrosion, or changes in electronic properties.

Collaborations with researchers from outside laboratories also include studies of the dynamics of atoms and molecules in molecular

solids, alloys, and zeolites.

For the above research, the equipment available includes

three-axis neutron crystal

spectrometers and time-of-flight

spectrometers for inelastic scattering, which along with neutron diffractometers, measure structural and dynamic processes in the time

regime from 10""''

s to 10"^^ s. In the Cold Neutron Research

Facility, two new very-highresolution inelastic scattering

spectrometers will be available.

Controlled temperature (0.3 K to 1300 K) and pressure devices are

available for changing sample

environments.

CONTACT: J. Michael Rowe

(301) 975-6210

John J. Rush

(301) 975-6231

AlOO Reactor

SMALL-ANGLE

NEUTRON SCATTERING

Small-angle neutron scattering

(SANS) is used to characterize submicron structural and magnetic

properties of materials in the size regime from 1 nm to 100 nm.

The SANS diffraction patterns

produced by structural features in

this size regime—for example, by

small precipitates or cavities in metal alloys, by micropores or

cracks in ceramics, by colloidal

suspensions and microemulsions,

or by polymers and biological macromolecules—can be analyzed to

give information on the size and

shape of the scattering centers as

well as their size distribution, surface area, and number density.

This detailed microstructure infor- mation is often a key to the prediction or understanding of the performance or failure modes of

structural materials and materials

processing conditions.

This five-detector, liighresolution tliermal neutron

diffractometer allows for ac- celerated data collection on

the crystal structures of

high-temperature superconductors, metals, and other

materials in powdered form.

A number of scientists from the chemical, communications, advanced materials, and aerospace

industries are already engaged in SANS research at NIST.

In the Cold Neutron Research

Facility, 30-m and 8-m SANS

spectrometers are operational,

with a second 30-m nearing completion. These world-class SANS in- struments will significantly

enhance resolution and sample

throughput. Computer-automated

equipment is available for maintaining samples at temperatures

from 4 K to 700 K and in magnetic

fields up to 20 kilogauss. To extract structural information from

the data, the researchers analyze

SANS patterns with an interactive

color graphics system and related programs.

CONTACT: Charles J. Glinka

AlOO l^eactor

(301) 975-6242

NEUTRON DIFFRACTION

Precise information on crystal

structures in solids is often a key

to understanding or improving the

properties of modern materials

and creating new materials with

specific properties. Many important materials, for example,

ceramics, catalysts, and rapidly

solidified alloys, often can be obtained only in powdered form. In

addition to single-crystal diffraction, state-of-the-art capabilities

are in place at NIST for measuring

and analyzing the crystal and

magnetic structure of polycrystalline materials by neutron diffraction. Both single-crystal and

multidetector, high-resolution

powder diffractometers are

available. NIST researchers continue to develop improved methods for accurate structure refinement. A

major effort currently is under

way in relating atomic arrange- ment, including defects, to super- conducting properties in high Tc ceramic superconductors. In addition, a number of industrial scientists are collaborating with NIST

staff in neutron diffraction studies

of inorganic catalysts, new kinds

of ionic conductors for small batteries and fuel cells, improved

ceramics for microcircuit substrates and engine components,

and high-performance lightweight

alloys for advanced aircraft.

CONTACT: Edward Prince

(301) 975-6230

Antonio Santoro

(301) 975-6232

AlOO Reactor

63 MATERIALS SCIENCE AND ENGINEERING
RESEARCH

FACILITIES

NEUTRON

REFLECTOMETRY

The importance of thin films,

layer structures, and interfaces has

grown significantly in the last few

years in a number of applications

areas. Analogous to electromagnetic radiation, neutrons can

undergo specular reflection at surfaces, and because neutrons can

distinguish between different

isotopes of the same element

(such as hydrogen and

deuterium), can penetrate to focus on subsurface interfaces, and are

sensitive to magnetic properties of

materials, they provide an important complement to other surface

probes.

Thermal neutron reflectometiy

and grazing-angle diffraction are

currently available at the NIST

reactor. For the former, reflectivities as low as 2 X lO"'' have

been measured, which is competitive with any neutron reflec- tometer in the world. Reflect- ometiy studies at NIST and else- where include superconducting

and magnetic layers, magnetic

multilayers, polymer interfaces,

and solid-liquid interfaces. An even more sensitive instru- ment is being constructed in the Cold Neutron Research Facility.

Neutron grazing-angle diffraction

is a very new technique—first demonstrated at NIST. With this approach, lattice spacings of planes with normals parallel to

the sample surface are determined

to depths of -10 nm.

CONTACT: Charles F. Majkrzak

AlOO Reactor

(301) 975-5251

NIST RESEARCH

REACTOR

The NIST research reactor (NBSR)

is a national center for the application of reactor radiation to a

variety of problems of national

concern. A wide variety of internal and external programs have

benefited from the broad range of

capabilities available to researchers from industry, universities, and government

laboratories.

CAPABILITIES: The NIST reactor

is an enriched-uranium, D2O

cooled and moderated reactor, with a peak thermal core flux of 4x10^ neutrons/cm^-s. The core comprises 30 fuel elements of a

unique, split-core design, in which

nine radial beam tubes "look" at a 17-cm gap between fuel-element

halves. A large-volume cold

source, two tangential and one

vertical beam tube, a thermal

column, several vertical thimbles,

and four "rabbit" tubes complete

the configuration. The reactor

operates continuously, 24 hours a

64

i
day on monthly cycles, followed by

approximately a week of shutdown

for refueling and maintenance.

The NBSR utilizes the flux

available in a very efficient manner through relatively short coreto-instrument distances and

large-diameter beam tubes. As a

result, the flux on the sample for

certain instruments is comparable

to that at other major research

reactors of higher power and peak

core flux. The experimental facilities in

the reactor hall are used for; neutron scattering and

diffraction; neutron radiography;

Left. Schematic of the NIST

20-megawatt research reactor and its associated thermal neutron instruments.

Below. The thermal neutron

ref lectometer shown here

produces high-resolution

information on structures

of multilayer coatings, magnetic films, liquid-solid in- terfaces, and other

surfaces.

trace analysis and depth

profiling; neutron dosimetry and stan- dards development;

fundamental neutron physics;

irradiations; and

isotope production.

Sample environments for low

and high temperature, low and

high pressure, and high magnetic

fields are routinely available. Online graphics, plotting, and data

fitting are available via personal

computers, Macintoshes, MicroVAXs, and a DEC 5810.

Elastic Scattering. Four beam

ports are dedicated to elastic scattering studies. A high-resolution

powder diffractometer is installed

at beam tube 1 (BT-1). The existing diffractometer is a fivedetector system arranged with 20°

spacing between detectors so that a complete diffraction scan (-10°

to 110°) is made by incrementing

the detector system through 20°. The wavelength is set at 0.154 nm,

and collimations as low as lO'-lO'-

10' are available. In late 1991 or

early 1992, a 32-detector diffractometer will replace the current instrument. It will provide three monochromator positions, each

set at 0.154-nm wavelength but at

different take-off angles to allow

maximum flexibility in selecting

the optimal resolution function

for a given measurement. Collimations down to 7'-20'-7' are

planned.

A triple-axis spectrometer with a four-circle goniometer is installed at BT-6 and is used primarily for residual stress and texture measurements, although inelastic

scattering experiments also can be

performed. This spectrometer is

typically operated in the elastic

scattering mode without an

analyzer for texture studies and

with the analyzer for residual

stress measurements. Incident

energies are continuously variable

with 2eM's from 20° to 75° available. Beam sizes up to 30 x 50

mm^ and down to 2 x 2 mm^ (for

residual stress studies) are utilized. Single-crystal structure deter- minations are performed on this

instrument while the new diffractometer is being completed.

A new thermal-neutron reflectometer, in which the incident

beam can be polarized and the

spin state of the reflected beam

analyzed, is operational on BT-7.

In this reflectometer, the polychromatic beam first passes through a pyrolytic graphite (PC)

filter to suppress the higher-order

wavelengths that would also be

reflected by the vertically focusing

PG monochromator set for a principal wavelength of 0.235 nm. For

collimations of -1° preceding and

1' following the monochromator,

respectively, the wavelength resolution AX,/X, -0.01, and the actual

flux on the sample is -5 x 10^

neutrons/cm^-s. Two %e detectors

are incorporated: one for

reflectivity measurements, the

other for grazing-anglediffraction experiments. Polarization of the incident beam is accomplished in transmission by one or more polarizing Fe-Si

supermirrors deposited on singlecrystal Si substrates. Because the reflectivities of the

polarizing supermirrors are not

unity for the unwanted spin state,

two or more supermirrors are used

in series. Reflectivities down to about 2 X 10'^ with a signal-tonoise ratio of about 1 have been

measured.

Inelastic Scattering. Three

triple-axis inelastic scattering

spectrometers are operational.

The BT-4 instrument employs two

remotely selectable, verticalfocusing monochromator crystals

(pyrolytic graphite and Cu), which

provide incident energies from

3 meV to 300 meV continuously. It

is capable of elastic-peak resolution down to 0.04 meV and also can be used in the "invertedfilter" mode for energy-loss

spectroscopy of vibrations in the 15meV to 280 meV range. The

BT-9 spectrometer offers variable

incident energy in the 5 meV to

50 meV range and collimations

down to 10'-12'-12'-l6'. The BT-2 instrument has both

triple-axis and polarized-beam

(up to 96 percent) capabilities.

Either a pyrolytic graphite or a

Heusler-alloy monochromator,

each vertically focused, are available, with remotely insertable cold

beryllium or pyrolytic graphite filters. Built-in guide fields and spin

rotators and collimation as low as

10'-S'-S'-20' are available.

65 MATERIALS SCIENCE AND ENGINEERING
RESEARCH FACILITIES

Elemental Analysis. Neutron

activation analysis is performed

utilizing the clean room for sample preparation, NBSR

irradiation facilities, semi-hot

and warm radiochemistry labs, and state-of-the-art radiationcounting labs. Development of methodology has aimed at

accuracies and sensitivities over

concentrations of 10'"^ percent to 100 percent.

Radiochemical separations for

specific elements and multielement analysis at the ultratrace

level are available. A thermal neutron-capture

prompt-gamma activation

analysis facility is operational,

with a neutron fluence of 5 x 10^

n/cm^-s in a 2-cm-diameter beam.

A thermal neutron depthprofiling facility is installed on

BT-3 for non-destructive deter- mination of near-surface elemental depth distributions in a variety

of materials. Sensitivities ap- proaching 10^^ atoms/cm^ with a

spatial resolution of better than

30 nm for depths of 5 |im -20 |im

are achievable.

Neutron Standards and

Dosimetry. A number of neutron

fields for standards and dosimetry

are available. These include a Cf

fission source, a U cavity fission

source, the thermal column beam,

an intermediate energy standard neutron field, and 2-, 24.5-, and

l44-keV filtered beams.

Irradiation Facilities. Four

pneumatic tubes for 40-cm^

"rabbits" with fluence ranges of 3x lo" to2x lo'Vcm -sfor irradiations of seconds up to hours

are available. The cadmium ratio range for these facilities is 4 to 3000 (Au). For long irradiations

6- and 9-cm-diameter in-core

thimbles are used. These are D2O

filled with fluences of 2-4 x 10^^

n/cm^-s.

Neutron Radiography. Radiography facilities are available at a

highly thermalized beam of the thermal column. Fluences range

from 10 to 10 n/cm -s, depending on resolution, with a Cd ratio

of 500:1, and an L/D ratio adjustable from 20:1 to 500:1. The

diverging beam is 25 cm in diameter at the image plane 2 m

from the reactor face. Facilities for autoradiography have also been

developed.

APPLICATIONS:

Structural and Spectroscopic

Studies of Magnetic Materials. Recent efforts have focused on

rare-earth compounds, amorphous magnets and spin glasses,

superconductors, magnetic

bilayers, and hydrogen in metals. Molecular-System Studies. These range from determination

of crystal dynamics in condensed

systems as complex as catalysts

and military "energetic" materials, to characterization of phase

transitions and translationrotation interactions in ionic

crystals.

Crystallographic Studies. Such

studies have ranged from development of analytical techniques in

single-crystal structure refinement

and (powder) total-profile refine- ment to a host of structure determinations. The latter include

ceramics (such as high-Tc super- conductors and ionic conductors),

alloys, zeolites, minerals, energetic, biological materials; and

structural studies focused on the

elucidation of phase transition mechanisms.

Thermal Neutron Reflectometry.

This is a relatively new capability

which already has produced very important results in studies of

supermirrors, thin films, and interfacial structure characterization.

Elemental Analysis Programs.

Examples include: studies in en- vironmental chemistry, nutrition,

biomedicine, energy and

electronic devices—with emphasis on Standard Reference Materials

for these applications. Neutron Dosimetry Studies.

Specific projects include: neutron

fluence standards for power reactor pressure vessel irradiation surveillance, ultralight mass assay for commercial track recorder detectors, absolute fission-rate measurements, and development of thermal neutron beam monitors.

Non-Destructive Evaluation

(NDE). Neutron radiography

capability has proven to be a very important complement to X-ray

radiography for applications

where light-element localization

is necessary, particularly in the

presence of heavy elements.

Neutron-induced autoradiography

has been applied primarily to ex- amining works of art. Diffraction

facilities are being used for texture

characterization and residual

stress determination for a variety

of metallurgical and ceramic

hardware.

AVAILABILITY: There are 25

thermal-neutron facilities at the NBSR, which provide about

125,000 instrument hours per

year. In 1990 over 450 researchers from 15 NIST divisions, 19 other

federal organizations, 90 U.S.

industrial and university

laboratories, and 34 foreign

laboratories utilized the facilities,

either collaboratively with NIST

staff or independently.

CONTACT: J. Michael Rowe

AIO6 Reactor

(301) 975-6210

COLD NEUTRON

RESEARCH FACILITY

The NIST Cold Neutron Research

Facility (CNRF) is the first in the

United States devoted exclusively

to cold neutron research. The

facility provides U.S. researchers prime access to a key tool of modern materials science. When

fully complete in 1993, the

$30-million project will provide

15 new experimental stations for

use by U.S. researchers, with

66
capabilities currently unavailable

in this country.

The facility is focused on the

cold source, a block of D2O ice

(with 8 percent H2O added) cooled

to 30 K to 40 K by recirculating

helium gas. The cold source is viewed by one port inside the reactor hall and seven neutron guide

tubes. The guide hall and associated office and laboratory

space has more than tripled the workspace available at NIST for neutron beam researchers.

CAPABILITIES: Instruments currently in operation include: Small-Angle Neutron Scattering

(SANS). The NIST/Exxon/University of Minnesota 30-meter SANS

will be the first to use a doubly

curved mirror as a focal element

in a long flight path to provide angular resolution and beam intensities that compare favorably with

any SANS instrument in the world. Two large-area position-sensitive

detectors will provide exceptional

sensitivity to materials structures ranging from roughly 1 nm to 500 nm. A second 30-meter SANS

scheduled for completion by early

1992—will be one of two instru- ments in the NSF/NIST Center for High-Resolution Neutron Scatter- ing (CHRNS). Polarized neutron

capabilities are planned for both

instruments.

Far left. An interactive

color graphics program used

by materials scientist John

Barker displays 30-m SANS

data in real time. Left. The

30-m small-angle neutron

scattering spectrometer at

the CNRF is operated jointly

by NIST, Exxon, and the

University of Minnesota.

Below. Schematic of current

and planned instrumentation at the Cold Neutron Research Facility.

Depth Profiling Instrument. With a measured chemical sensitivity 20 times that of the existing NIST thermal-beam

instrument, this station features automated sample handling; near

real-time spectral processing;

goniometer positioning of sample

and detectors; and sample

temperature control. Increased

signal intensity will permit multidimensional imaging of elemental

distributions and profiling of

nuclides with absorption crosssections for charged particle emission of less than 1 barn. Prompt-gamma-ray activation

analysis. Providing greater sensitivity for this method than any

other existing instrument in the

world, this equipment provides

unique measurements of chemical

elements, such as hydrogen, that

are difficult to detect by other means. Fundamental Physics Station.

Available for use only in collaboration with the NIST fundamental

physics research group, an end

67 MATERIALS SCIENCE AND ENGINEERING
RESEARCH FACILITIES

guide position physics station currently is instrumented for a new

measurement of the lifetime of the

neutron. Instruments planned for completion between 1992 and 1993

include: neutron reflectometer;

grazing-incidence

diffractometer;

triple-axis spectrometer;

spin-polarized inelastic neutron

spectrometer (SPINS);

time-of-flight spectrometer;

back-reflection spectrometer;

spin-echo spectrometer; and

neutron interferometer.

APPLICATIONS: The unusual sensitivity and range of measure- ments possible at the NIST CNRF

provide applications in materials

structures, materials dynamics,

chemical analysis, and neutron

physics. Currently operational in- struments are used to study

microstructures in metals,

ceramics and colloidal mixtures;

molecular geometry of polymer

and biological macromolecules;

chemical composition of semiconductors, high-tech materials, airpollution filters, and other

samples; and neutron decay rates.

AVAILABILITY: The CNRF operates

as a national facility open to all

qualified researchers. NIST

develops experimental stations for

use by the general U.S. research community. Two-thirds of the

available time on these stations

will be allocated by a Program Advisory Committee (PAC) on the

basis of scientific merit of written

proposals. The PAC is appointed by

NIST with a majority of members

chosen from outside NIST.

The second mode involves Participating Research Teams

(PRTs), which are developing the remaining stations. The PRTs are

responsible for design, construction, and maintenance of the

facilities in return for threefourths of the available time. The

remaining time will be allocated

by the PAC. The NSF/NIST

(CHRNS) instruments constitute a

special PRT in which all allocatable time will be available to

the research community through

the proposal review/PAC system. For all instrumental stations,

instrument-responsible scientists

will be designated to assist users in performing their experiments.

CONTACT: J. Michael Rowe

AlOO Reactor

(301) 975-6210

METALS PROCESSING

LABORATORY

The metals processing laboratory

at NIST contains special facilities

for the production of rapidly

solidified alloys, including equipment for gas atomization and

electrohydrodynamic atomization

to produce rapidly solidified alloy

powders, melt spinning to produce

rapidly solidified alloy ribbons,

and electron beam surface melting to produce rapidly solidified

surface layers. Hot isostatic pressing equipment is available for consolidating alloy powders.

CAPABILITIES:

Gas Atomization. The gas atomization system can be used to produce up to 25 kg of rapidly

solidified alloy powder per batch

while maintaining a controlled at- mosphere throughout the atomizing and powder handling process.

High-energy gas (Ar, He, or N) impinging on a liquid metal stream

breaks up the liquid into small

droplets, which solidify rapidly.

Cooling rates are up to 10^ K/s. The atomized powder, entrained

in the gas flow, is collected in removable, vacuum-tight canisters. Electrohydrodynamic Atomization. In the electrohydrodynamic

atomization system, a liquid

metal stream is injected into a

strong electric field. The field

causes the stream to disintegrate

into droplets, which solidify rapidly to produce extremely fine (<1 |im diameter) alloy powder.

Powder produced by this process is

well-suited for studying solidification dynamics. As the system is

presently configured, small quantities for microscopic examination can be produced from alloys with

melting points up to 900 °C.

Melt Spinning. Melt-spinning

techniques can be used to produce

rapidly solidified alloys in ribbon

form. Because of the high cooling

rates (up to 10^ K/s) with this method, amorphous alloys as well

as crystalline alloys can be

produced. Ribbons up to 3-nim

wide and 0.05-mm thick can be

produced in quantities of several grams per batch. Materials with a

wide range of melting points, from

aluminum alloys to super-alloys,

have been produced.

Electron-Beam Surface Melting.

An electron-beam system, which

provides surface melting and subsequent rapid resolidification of

surface layers, can be operated in

either a pulsed or continuous

mode. The electron beam can be

focused to a spot less than 1 mm

in diameter and deflected at frequencies up to 5 kHz. Hot Isostatic Press. A hot

isostatic press (HIP) with

microprocessor control of the

temperature-pressure-time cycle is

available for consolidation of powder or compacted powder shapes.

The HIP has a cylindrical working

volume 15 cm in diameter and 30

cm high. The maximum working

pressure is 207 MPa. The molybdenum furnace has a maximum

heating rate of 35 K/min and is capable of maintaining 1500 °C.

AVAILABILITY: These facilities are

designed to produce alloy research samples that otherwise are difficult for users to obtain. Typically, industrial companies or

universities send workers to NIST

to participate in preparing alloys

of special industrial and scientific

interest for further analyses in

their home laboratories and to

collaborate with NIST scientists in

investigations of generic relationships between processing conditions and resulting alloy

microstructures and properties.

CONTACT: John R. Manning

A153 Materials

(301) 975-6157

POLYMER COMPOSITE

FABRICATION FACILITY

The composite fabrication facility

permits the preparation of wellcontrolled polymer composite

samples for scientific studies and

the evaluation of results from

NIST's processing science pro- gram in a realistic fabrication

environment.

CAPABILITIES: The facility involves five major components and

associated support equipment: a

prepregger to prepare sheets (up

to 180 cm X 30 cm) of unidirectional fiber coated with resin; a

fully computerized autoclave

68
capable of temperatures up to

535 °C and pressures up to 3-6 MPa; an automated hydraulic

press (temperatures up to 535 °C)

with water-cooled platens for

rapid, controlled cooling; a

unidirectional flow facility for

characterizing the permeability of

fiber preforms in all three directions; and a specially designed two- component pumping system for

fabrication of samples by resin

transfer molding and for conducting flow visualization

experiments.

APPLICATIONS: The facility can

be used to study a variety of questions, such as the details of resin

flow and void formation during

processing and the influence of

processing conditions, fiber orientation, and fiber-surface treat- ments on performance.

AVAILABILITY: Used by NIST staff

in an active research program on

polymer composites, the facility is

available for collaborative studies

with industry, academic institutions, and other government

agencies.

CONTACT: Donald L. Hunston

A209 Polymer

(301) 975-6837

POWDER

CHARACTERIZATION AND

PROCESSING LABORATORY

Advanced ceramics are manufactured by the consolidation of fine powders. Researchers at NIST are working to develop the scientific foundation needed for improving

reproducibility and reducing the

cost of producing ceramic components. The powder characterization facility offers

specialized instrumentation for measuring physical properties,

phase composition, and surface chemical properties. In addition,

facilities exist for processing and

synthesizing ultrapure powders.

CAPABILITIES:

Physical Properties Measure- ment. Particle size distribution,

specific surface area, specific

gravity, and porosity are some of

the major physical properties for which instrumentation is available. Powder size distribution can

be determined by gravity sedimentation followed by X-ray absorption, centrifugal sedimentation,

light diffraction, and photon correlation spectroscopy. The size

range of these instruments covers

0.03 |im to 200 |J,m. Each instru- ment works in a specific range

and provides the data in the form

of a discrete size range. The particles are examined directly by the

application of scanning and transmission electron microscopy of

particles as small as 0.001 |J.m.

Surface and Interface Chemistry

Measurements. The surface and interface characterization of powders contributes to the knowledge

base of the surface interactions of

particles in contact with solvents.

As the particles become smaller,

their surface characteristics be- come more significant. MicroRaman and Fourier transformed

infrared spectroscopy are used to

study surface composition, and

electrophoretic mobility and

acoustophoretic mobility are used

to study modification to the powder surface as a result of an interaction with a solvent. Phase Composition. Since most

of the ceramic powders undergo

phase transformation during densification, understanding the phase changes in specific densification environments is an active part of NIST research. The

Siemens high-temperature X-ray

diffractometer has a temperature

range from room temperature to 3000 K and a position sensitive

detector. In addition, sintering can be carried out in oxygen-free

argon or nitrogen environments.

Solid-State Imaging. The solidstate nuclear magnetic resonance (NMR) spectrometer/imager carries out measurements in chemical shift, nuclear spin density,

relaxation times, and imaging of NMR active nuclear distribution. Ceramic powder slurries, green

bodies, and dense ceramics can be

analyzed for identification of

impurities, chemical state, and

composition distribution by nondestructive evaluation. In addition, the NMR can determine

amorphous phase content of the

powders.

Powder Synthesis. The ability to

synthesize powders of controlled

characteristics is needed to

develop a powder-processing

knowledge base. The fine-powder

synthesis facility consists of a chemical flow reactor for controlled synthesis and inert atmosphere chambers. A solution

atomizer is available to generate

polydisperse aerosols in the range

0.01 |im to 1.0 |im, as is a spray

dryer to form monodisperse ag- glomerates in the range 0.5 |J.m to

100 )im.

Colloidal Suspensions Preparation. Colloidal processing of ceramic powders has emerged as an attractive technology for producing defect-free ceramics.

However, some major issues still remain to be addressed, including

the lack of characterization techniques for slurries that contain

high concentrations of solids and

scientific understanding of limitations in the preparation of such

slurries. The powder processing

laboratory consists of an acoustophoresis instrument, a rheometer,

a high-energy agitation ball mill,

and slurry consolidation equipment. These techniques are used

to study interface chemistry, flow

behavior, size reduction, morphology modification, and densification of polydisperse particles and

similar processes resulting from interactions between the particles

and their environment.

AVAILABILITY: These facilities are

used primarily to support NIST research programs using ceramic

powders. They are available for

collaborative or independent work

by qualified government, industry,

or university personnel with

preference given to projects related

to ceramics research. CONTACT: Subhas G. Malghan

A256 Materials

(301) 975-6101

69 MATERIALS SCIENCE AND ENGINEERING
RESEARCH FACILITIES

MECHANICAL BEHAVIOR

LABORATORIES

Mechanical property measurement

facilities at NIST permit characterization of all mechanical

properties over a wide range of

force levels and temperatures.

CAPABILITIES: Conventional

mechanical property measurements, such as yield and ultimate

strengths, elongation, and reduction of area, can be made at temperatures ranging from 4 K

(produced by immersion of the specimen in liquid helium in a

cryostatted test apparatus specially

designed for this purpose) to 2800 K (produced by testing in a vacuum furnace heated by

tungsten elements). Equipment

for measuring fracture toughness

over the same temperature range

is used. Material fatigue resistance can be characterized in a variety

of ways—including fatigue crack

growth, load- and straincontrolled, random-load, or conventional rotating beam—at temperatures from 4 K to 600 K. Narrow and wide-plate be- havior characteristics, such as in crack arrest testing, are studied

using computer-assisted data acquisition and reduction equip- ment. Up to 100 strain gage

channels are available, as well as

capabilities for capacitance and

strain-gage extensometers and

full-field video optical strain data

measurement (photoelastic and

moire interferometry). High-speed

digital oscilloscopes are used to

record strain patterns produced by

rapidly moving cracks (1000 m/s)

in crack arrest tests. Special test re- quirements, including dynamic

tear, drop weight, torsion, and impact, can be met using existing

facilities. Complete metallographic and hardness characThe mechanical properties

of structural alloys,

superconductors, polymer

composites, and other materials are measured at cryogenic temperatures by

physical scientist David

McColskey.

terizations of specimen materials

are available. The high-load mechanical test- ing machine has a force capacity

of 50 MN in compression and

25 MN in tension. Servo-hydraulic

tension-compression machines are

available in a range of load

capacities and actuator travel

rates; the maximum load capacity

is 4 MN and the maximum dis- placement rate is 50 cm/s. These

smaller machines are used routinely for measuring fracture and

fatigue properties in liquid

helium. Two screw-driven tensile machines have capacities of up to 100 kN for tensile testing in liquid

helium.

AVAILABILITY: These facilities are

available to guest researchers for

collaborative programs. NIST

routinely performs research on

these facilities for outside sponsors.

CONTACT: J. David McColskey

Div. 853

Boulder, Colo. 80303

(303) 497-5544

SMALL-ANGLE X-RAY

SCATTERING FACILITY

Small-angle X-ray scattering

(SAXS) is a technique in which a highly collimated beam of X-rays

(wavelength range 0.7 angstrom

to 3 angstroms) is used to probe

the structure of materials on the

size scale of 0.1 nm to 100 nm.

Materials exhibiting structure in

this size range include polymers,

biological macromolecules,

ceramics, metals, and alloys. The

small-angle scattering patterns can be analyzed to characterize

the size and shape of the scattering centers as well as their spatial

distribution and surface area. Data obtained from these experiments are complementary to data

obtained from other diffraction

studies and from morphological

studies using electron microscopy.

CAPABILITIES: The NIST 10-m

SAXS camera uses a 12-kW rotating anode X-ray generator as a

source of X-rays. The target is

usually copper X{Ka) = 1.54, but

additional wavelengths are available. The collimation path is

defined so as to permit a 10' nm'

resolution in reciprocal space at

the surface of a two-dimensional

position-sensitive proportional

detector. The collimation path

and the scattered beam path are

evacuated, and all elements of vacuum operation. X-ray optical

configuration, sample selection,

and calibration are computer controlled. Image data are collected by a minicomputer, and an associated VAX/730 computer supports a complete repertory of

software for displaying, analyzing,

and modeling the results. Sample chambers are being

developed for measurements at high temperatures and to deform

specimens during measurement.

70
APPLICATIONS: The SAXS tech- nique is used to study molecular

conformation, microphase

domain structures, crystallization

phenomena, network formation,

craze initiation, void distribution,

and similar phenomena resulting

from fluctuations in electron density within a material. Such studies are currently of broad interest

in all areas of materials science.

AVAILABILITY: This facility is

operated by members of the NIST

staff in support of their active research program in polymeric

materials. It is available for use by

researchers from industry,

academia, and other government

agencies on either a collaborative

or independent basis.

CONTACT: John D. Barnes B2 10 Polymer

(301) 975-6786

MATERIALS SCIENCE

X-RAY BEAMLINES

NIST operates two beamstations on the X23A port at the National

Synchrotron Light Source (NSLS)

Schematic of the NIST X-Ray

Beamline at the Brookhaven

National Synchrotron Light

Source.

at Brookhaven National

Laboratory in New York. The

light source provides an intense

continuous-spectrum beam of collimated and polarized X-rays

many orders of magnitude

brighter than the beams that conventional laboratory sources provide. These two beam stations offer

access to dedicated instrumentation for small-angle X-ray scattering. X-ray diffraction imaging

(topography) and extended X-ray

absorption fine structure.

CAPABILITIES: Small-angle

X-ray scattering can be carried

out in the photon energy range

from 5 keV to 1 1 keV. The mini2 1 mum wavevector is 4 x 10 nm"

and the wavelength resolution is AX/X = 10"^, enabling anomalous small-angle scattering with

excellent resolution. Diffraction imaging of single crystals and

powders is carried out with

monochromatic photons between

5 keV and 30 keV. An energytunable X-ray image magnifier

enables imaging of microstructure

down to less than 1 mm. The

energy-scanning experiments,

primarily EXAFS, also are per- formed over an energy range from

5 keV to 30 keV.

APPLICATIONS: Small-angle

scattering measurements on

ceramic and metallurgical materials are used to characterize the

microstructure in the 2-nm to l-jim size range as a function of

starting chemistry and processing

parameters. Scattering from a particular entity can be separated

from other scatterers in a complex

material using anomalous smallangle X-ray scattering. Diffraction imaging is used to study imperfections and strains in single crystals

and powder compacts. The structure of strained semiconductor interfaces and metal multilayers can

be studied using EXAFS. A combination of EXAFS and diffraction

will provide a capability for sitespecific local structure determination in crystals.

AVAILABILITY: Beam time is

available to qualified scientists

provided safety requirements are met and scheduling arrangements can be made. Proposals for collaborative use of the facility are

reviewed at NIST; proposals for in- dependent use of the facility

should be submitted to the NSLS.

CONTACT: Gabrielle G. Long

A 163 Materials

(301) 975-5975

Mom otS-iCiDMATaFi

X

71 MATERIALS SCIENCE AND ENGINEERING
BUILDING AND

FIRE RESEARCH

LABORATORY

Wlajor goals of the Building and Fire Research Laboratory

(BFRL) are to improve the productivity of the U.S. construction industry, which now faces stiff competition from

overseas firms, and to reduce the human and economic

costs resulting from fire, earthquakes, and other hazards.

Products of the laboratory's research include measurements and test methods, performance criteria, and

technical data that are often incorporated into building

and fire standards and codes. Staff members are involved

in more than 100 activities to develop voluntary standards. In addition, studies on fire science and engineering, building materials, computer-integrated construction

practices, and structural, mechanical, and environmental

engineering yield results presented in a form that industry can use.

For example, HAZARD I, a BFRL-developed computer program, models the behavior of building fires, helping engineers, architects, and others to anticipate and reduce

the potential for hazards. Another computer model simulates how microstructural defects can undermine the

structural integrity of concrete.

Laboratory personnel also conduct investigations at the scene of structural failures due to earthquakes, hurricanes, or other causes. The knowledge gained from these

investigations is applied to the laboratory's recommendations for construction practices to reduce hazards.

NIST scientists and engineers also use investigations of

major fires to advance their research and guide their

recommendations to policy-makers. Following the Persian

Gulf War, these researchers made measurements of combustion products released by the hundreds of oil well fires

raging In Kuwait. Such measurements will help determine

whether the burning of oil spills poses less environmental

damage than other clean-up methods.

Contact: Richard N. Wright

B216 Building Research

(301) 975-5900

COOPERATIVE

RESEARCH

OPPORTUNITIES

STRUCTURES

STRUCTURAL

ENGINEERING

Under the National Earthquake

Hazards Reduction Program, NIST

does research and development

work that is used in standards for

the seismic safety of structures. Experimental and analytical research is under way at NIST to

develop knowledge for design and

construction standards for new

and existing buildings and lifeline

structures. The work involves identifying mechanisms of failure and

establishing criteria to ensure

structural safety.

Current research addresses: a rational procedure to deter- mine the ultimate shear strength

of partially reinforced masonry

walls;

strength and ductility of connections in precast concrete

structures;

drift control criteria for flexible

frames;

evaluation criteria for baseisolation systems and test proce- dures for evaluating the response

of structures subjected to seismic

loading;

strengthening methodologies

for concrete frame structures; and

effects of subsurface conditions on ground motion.

Other structural research

includes:

studies of structural perfor- mance for development of standards and test methods for high-performance concrete in major construction applications;

techniques and instrumentation

for assessing the properties of

existing structures and for developing technical criteria and

methodologies for strengthening

and repairing existing structural members and systems; and

analytical and experimental

methods for identification of dynamic response characteristics

of flexible members and structural

networks.

CONTACT: H.S. Lew

BI68 Building Research

(301) 975-6061

72
BUILDING

MATERIALS

CEMENT

AND CONCRETE

NIST researchers are undertaking

research to develop a fundamental

understanding of the relationship

between chemistry, microstructure, and service life of concrete and other inorganic building materials. The goal of the program is

to be able to predict the behavior

of these materials and their service

lifetimes. The service life of concrete largely depends on the rate

of moisture ingress and of transport of dissolved salts and gases in

the pore system of concrete. Models are being developed to

consider service conditions, including composition of the environ- ment; the transport rate of

reactants by diffusion, convection,

and capillary forces; and reaction

mechanisms. Researchers are developing mathematical and

simulation models to predict the

relationships between pore structure and diffusion and permeability of concrete. Research projects include

development and validation of mathematical models of

microstructure development in cement pastes as the cement

hydrates, the effects of microstructure on permeability and fracture

of concrete, and mechanisms of degradation of concrete. Artificial

Physicist Edward Garboczi

worl(s on a computer model

tliat will simulate how the

microstructure of concrete

develops during the setting

process.

intelligence systems are being

developed for optimizing the selection of materials and for diagnosing the causes of material

degradation. The research is per- formed using a variety of techniques, including scanning

electron microscopy, computerized

image analysis, X-ray diffraction,

and thermal analysis.

CONTACT: James R. Clifton B348 Building Research

(301) 975-6707

MATERIALS

NIST is conducting basic and

applied research to develop

methodologies to aid in predicting

the service life of organic building

materials, such as protective coatings for steel, roofing materials,

and asphalt. The researchers are

investigating degradation

mechanisms, improving characterization methods, and developing mathematical models of the

degradation processes. Stochastic

models, which are based in

reliability theory and life-testing

analysis, are included in the modeling efforts for coatings and

roofing materials.

To help in understanding the mechanisms of degradation and

provide data for models, materials

are characterized in many ways,

including Fourier transform infrared spectroscopy, thermal

analyses methods, scanning

electron microscopy/energy dispersive X-ray, and visual and infrared imaging. Researchers also are

developing improved ways to characterize atmospheric environments in which these materials

often are used. Characterization of environmental parameters that cause degradation is needed to

link inventory data with service

life prediction.

CONTACT: Geoffrey Frohnsdorff

B368 Building Research

(301) 975-6706

BUILDING

ENVIRONMENT

LIGHTING

The NIST lighting program

focuses on fundamental measure- ments of interior luminance and

illuminance distributions, hght

fixture output, and the interaction

between lighting and HVAC

systems. A continuing challenge is

to develop metrics for lighting

quality that evaluate the combined effects of illuminance,

luminance, contrast, color rendering, lighting geometry, and

configuration.

Current research includes a major project on the measurement

and modeling of the interaction of

lighting and HVAC in a simulated

interior office module. This research will result in the development of a detailed computer

model for predicting the effects of

different types of lighting and

HVAC systems. Modifications will

be made to the facility in the near

future to study the effects of dimming, thermal mass, and external

solar conditions.

CONTACT: Belinda L. Collins

A3 13 Building Research

(301) 975-6455

INDOOR

AIR QUALITY

Measurement and testing procedures, technical data, and comprehensive indoor air-quality

models are being developed by

NIST researchers as part of a

multiyear program to improve

indoor air quality in buildings.

Experiments are being conducted

in several large buildings to

develop test methods to evaluate

how air moves into and within

large commercial buildings. The

researchers are developing comprehensive computer models to

predict pollutant levels from

sources introduced into buildings

from outdoor air and those

generated inside from sources as combustion equipment and floor and wall coverings.

The first phase of the research

is complete. Models exist that can

predict indoor contaminant levels

as functions of emission, dilution,

and intrabuilding air movement.

The models currently are being

extended to model reactive contaminants. Test procedures also

are being developed to evaluate

the effectiveness of various filter media for removing gaseous pollutants. A test facility for this purpose has been designed and

assembled. Test methods will be

developed for commercial gaseous

air filters and for those used in

residences.

CONTACT: Andrew K. Persily

A3 13 Building Research

(301) 975-6418

73
COOPERATIVE RESEARCH OPPORTUNITIES

REFRIGERATION

MACHINERY

NIST researchers are exploring the

use of refrigerant mixtures to improve the efficiency of refrigeration cycles and replace harmful

chlorofluorocarbon refrigerants

that are damaging the ozone layer

of the upper atmosphere. The researchers evaluate a wide variety

of refrigeration cycles by using a breadboard heat pump to "plug"

and "unplug" circuits and components. The breadboard heat

pump will be altered to test new

refrigeration cycles. This is based on the results of a theoretical

study being conducted to find the optimal combination of mixtures

and appropriate refrigeration

cycles for the best and most versatile performance.

The "best" of the advanced

cycles will be selected and equipment built and evaluated. A minibreadboard that will use a very

small charge will also be built so

that rare refrigerants of limited

production can be studied.

CONTACT: David A. Didion

B114 Building Research

(301) 975-5881

THERMAL

INSULATION

Researchers at NIST are developing basic data and simulation

models for heat, air, and moisture

transfer through building envelope components. They are

developing and validating a

theoretical model for moisture

transfer, completing research

required to develop a lowconductivity Standard Reference

Material (SRM), developing a ther- mal conductivity database for

chlorofluorocarbon (CFC) blown

Using sophisticated equipment sucii as tliis Fourier

transform Infrared microscope, NIST researcli

cliemist Eric Byrd develops

ways to predict tlie service

life of organic building materials, such as protective

coatings for steel, roofing

materials, and asphalt.

thermal insulation products, and

refining a dynamic test procedure

for building components.

A 1-m guarded hot plate is

used to develop SRMs; to deter- mine thermal conductivity values

for various materials, such as CFC-blown insulation; and to provide measurement services to manufacturers and researchers. A calibrated hot box is used to measure the steady-state and

dynamic performance of full-scale

wall systems.

CONTACT: A. Hunter Fanney

B320 Building Research

(301) 975-5864

BUILDING

CONTROLS

NIST research is fostering the development of more intelligent,

integrated, and optimized building mechanical systems. A

dynamic building/heating, ventilating, and air-conditioning control system simulation program is

used to study HVAC/control system

dynamics and interactions. An ex- panded building management and

controls laboratory is used to assist the building controls industry

in the development, evaluation,

and testing of communication

protocol standards for the open

exchange of information.

The application of knowledgebased systems to buildings is a new area of research. Plans call

for exploring how real-time

models, "tuning" techniques,

forecasting, optimal control

theory, and a rule-based expert sys- tem can be combined to evaluate

control system performance, make

control strategy decisions that optimize building performance, and

perform diagnostics to advise the

building operator or manager on

building operations, equipment

problems, or maintenance require- ments. Work has begun for the Department of Energy to develop an HVAC/building emulator/EMCS

tester, which will provide a method for evaluating application

algorithms.

CONTACT: George E. Kelly

B114 Building Research

(301) 975-5870

COMPUTER-INTEGRATED

CONSTRUCTION

NIST researchers are developing

rational techniques for defining

and testing computer representations of information needed

throughout the building process, from the conception of a building

to its demolition. The goal of the program is to develop validated

neutral data representations for

use in standards for accessing, ex- changing, and archiving information. As a corollary, the program

seeks to develop testing methods

that assure consistency, completeness, and correctness of information. The research draws on

evolving information technologies, including knowledge engineering and semantic modeling.

Subject areas for research include

standards and codes, engineering

drawings, and product data.

74
Past research has resulted in methodologies for representing,

analyzing, and expressing standards, and for interfacing standards to computer-aided design

systems. Recent research results

are being applied in the development and validation of national

and international standards for

product data, such as the Initial Graphics Exchange Specification

and the Standard for the Ex- change of Product IVIodel Data.

CONTACT: Kent A. Reed

B306 Building Research

(301) 975-5852

Using a small unmanned

blimp, NIST researchers

measure the combustion

products and the smoke

plume flow from crude oil spill fires. This study was

conducted by NIST at the

U.S. Coast Guard Fire and

Safety Test Detachment in Mobile, Ala.

FIRE SCIENCE

AND ENGINEERING

FIRE SIMULATION

This project is designed to provide

the expedient transfer of scientifically based technology from NIST

to the professional user community and to create a link be- tween NIST computer-based

activities and others doing similar

or complementary work. Over the

past decade, NIST researchers have

developed many computer models

of various aspects of fire. Researchers develop engineering sys- tems for design application as well

as expert systems, collect supporting data and programs, and

operate a working and training

laboratory dedicated to fire-safety

computations.

CONTACT: Harold E. Nelson

B250 Building Research

(301) 975-6869

FIRE

DYNAMICS

Predictive fire models need accurate representations of burning

objects. The most important of

these for residences are

upholstered furniture and wall

coverings. NIST researchers are using both laboratory experiments

and computer modeling to understand the processes that govern

these types of combustion. Algorithms are being developed and

validated for use in hazard

analysis.

CONTACT: Andrew J. Powell

B250 Polymer

(301) 975-6865

FIRE MEASUREMENT

AND RESEARCH

HAZARD

ANALYSIS

The United States has one of the

worst fire records in the industrialized world. NIST researchers are

helping to reduce the losses and

the cost of fire protection by

providing scientific and engineering bases needed by manufacturers and the fire protection

community. One project involves

the development of predictive,

analytical methods that permit the

quantitative assessment of hazard

and risk from fires. Researchers

base these methods on numerical

modeling but also include handcalculation methods for estimating hazards and design curves/

tables to be used by architects and

engineers. To ensure widespread

use, the necessary data must be

readily available, and data input

and presentation must be in terms

readily understandable by the

average professional. Thus, the

projects include a strong emphasis on state-of-the-art computer

graphics and computer-aided

design techniques.

CONTACT: Walter W. Jones A249 Polymer

(301) 975-6879

LARGE FIRES

Large fires, which result from industrial and transportation accidents or natural disasters, present

a hazard to the surrounding area. While these fires attract media and

public attention, very little is known about their characteristics,

including the chemical compounds that are released into the

atmosphere. NIST is researching

and measuring large fires to understand and predict the effect of

these fires in terms of fuel burning

rate, chemical compounds in the smoke plume, and the downwind

movement of the smoke plume, including particulate settling. As a

first step, NIST is measuring

smoke plumes from large, openair fires to help develop computer

models which can predict their

size and movement. Further fire dynamics research and advanced

computational fluid dynamics will

lead to methods capable of assessing the local impact of large fires.

These methods can be used by industiy in preplanning analysis for

potential accidents or as technical

support for emergency response.

CONTACT: David D. Evans A345 Polymer

(301) 975-6899

75 BUILDING AND FIRE RESEARCH
RESEARCH

FACILITIES

ADVANCED

FIRE SENSING

Fires that are detected and suppressed quickly do little damage.

NIST research is studying new

"fire signatures" that would

enable a new generation of detectors. The signals from these detectors would be electronically

analyzed to alert occupants or suppression devices, perhaps even

before flames exist. The research

also is intended to understand and

provide technology for avoiding

the high false alarm rate of current sensors.

CONTACT: Richard G. Gann

B250 Polymer

(301) 975-6866

SMOKE AND TOXIC

GAS PREDICTION

Most people who perish in fires die from smoke inhalation. Many are exposed to this smoke for longer

periods because the blackness of

the smoke impedes their escape from the burning building. NIST

research is developing the scientific base and the predictive

methods for the yields of carbon

monoxide (the predominant

toxicant) and soot. These require

improved knowledge of the chemical and physical processes in

flames, combined with the fluid mechanical processes that dominate air entrainment into fire plumes and the flow fields within

a compartment.

CONTACT: William M. Pitts B258 Polymer

(301) 975-6486

POLYMER COMBUSTION

RESEARCH

NIST is conducting research to

develop a scientific base for the

gasification and combustion of

natural and synthetic polymers,

particularly for the more applied

fire research activities. For ex- ample, NIST scientists are working on the kinetics and heats of combustion for wood, theoretical modeling of thermal degradation

of polymers, smoldering research,

and detailed degradation

mechanisms of polymers.

CONTACT: Takashi Kashiwagi

B258 Polymer

(301) 975-6699

LARGE-SCALE

STRUCTURES

TESTING FACILITY

The large-scale structures testing

facility consists of a universal testing machine (UTM) that may be

used with a 13.7-ni-high reaction

buttress equipped with a horizontal hydraulic ram of 4.5-MN

capacity. A combination of

horizontal and vertical forces may

be applied to large-scale

specimens.

CAPABILITIES: The UTM portion

of the facility is a hydraulically

operated machine of 53.4-MN

capacity and is one of the largest

in the world. It tests large structural components and applies the

forces needed to calibrate very

large capacity force-measuring

devices. It can apply compression

forces to column sections or fabricated members up to 18 m in

height. The reaction buttress will

resist horizontal forces to 4.5 MN

from floor level to 12.2 m high.

Flexure and tension specimens

may be subjected to forces up to

18 MN and 26 MN, respectively.

Two-m-thick test floors east and

west of the machine may be used

to tie specimens in place.

A servo system has been added

to the original manual controls of

the UTM. It may be programmed

by function generator or computer

to create any desired loading function using force, strain, or dis- placement as the variable. Loads may be applied to a specimen by both the UTM and

horizontal ram. A four-rail track

system equipped with low-friction

rollers has been used for concrete column tests. An "A" frame was

used to resist horizontal reaction

forces generated by the ram and was attached to the buttress at the

desired height.

APPLICATIONS: A testing program

was conducted to evaluate the per- formance of concrete columns

1.5 m in diameter and up to 9-1 rn

high. Another test series evaluated

fracture propagation in steel

plates 1 m wide and 0.1 m and

0.15 m thick. A third experiment

used the servo-control system

programming repeated loads applied to composite specimens.

Low-cycle fatigue tests, destructive or ultimate loads, earthquake

simulation in two dimensions,

and complex loading of components may all be accomplished

in this facility. Servo operation of

this machine creates a unique

potential for precisely controlled

very large forces applied to test components.

AVAILABILITY: This facility, which

must be operated by NIST staff, is

available for cooperative or independent research. Tests should be

arranged as far in advance as possible as special hardware may be

needed for specimen attachment.

CONTACT: H.S. Lew

Bl68 Building Research

(301) 975-6061

TRI-DIRECTIONAL

TEST FACILITY

The tri-directional test facility is a

computer-controlled apparatus

capable of applying cyclic loads simultaneously in three directions.

It is used to examine the strength

of structural components or as- semblages under the application

of a variety of loading phenomena, such as an earthquake or

wind. This is one of the largest

such facilities in the world, both

in terms of its high load capacity

76
and its capability to handle large,

full-scale specimens.

CAPABILITIES: The facility can

apply forces and/or displacements

in six directions at one end of a

specimen. The other end of a specimen is fixed. Specimens up

to 3-3 m high x 3 m in length or width may be tested. The six

degrees of freedom are translations and rotations in and about

three orthogonal axes. The forces

are applied by six closed-loop,

servo-controlled hydraulic actuators that receive instructions

from a computer. Operating under

computer control, the facility

simultaneously maintains control

of the load and/or displacements

in each of the three orthogonal

directions. Loads may be applied

up to 2,000 kN in the vertical and

about 890 kN in each of the two

horizontal directions.

APPLICATIONS: The test facility is

limited only by the size of the test specimen. Loads may be cyclic or

unidirectional depending on the

type of loading condition being

simulated. The facility is used to

study masonry shear walls subjected to reverse cyclic lateral loading and precast concrete connections also subjected to reversed

cyclic lateral loading. This facility

supports NIST's role in conducting

research for seismic design and

construction standards in the National Earthquake Hazards Reduction Program.

AVAILABILITY: The tri-directional

test facility is used by NIST staff in

a variety of NIST research projects and collaborative projects

with other agencies. It also is

available for independent research but must be operated by NIST staff.

CONTACT: H.S. Lew

Bl68 Building Research

(301) 975-6061

LARGE

ENVIRONMENTAL

CHAMBER

The large environmental chamber

is 14.9 m X 12.8 m x 9.5 m high.

It has an earth floor and may be

excavated as needed for building

construction. The chamber is one

of the largest of its kind, capable

of accommodating two-story

houses under simulated environmental conditions. This chamber

has been used for thermal performance, heating and cooling load

measurements, and energy con- sumption studies of buildings of

different kinds.

CAPABILITIES: The chamber is capable of automatically maintaining steady and/or dynamic

temperature profiles from -45 °C

to 65 °C and humidity from

50 percent relative humidity (rh)

at 1.7 °C up to 35 °C dewpoint at

49 °C. A wider range of rh (15 percent to 80 percent) may be obtained manually. Air circulation

maintains the temperature variation within the chamber to within

Technician IVlax Peltz ex- amines cracks on a precast

concrete beam-column connection being tested for

strength and ductility in the

NIST tri-directional test

facility.

±1 °C. Damper-control return

ducts in all four corners of the chamber permit good air distribution. Supply air is furnished by

ceiling diffusers.

APPLICATIONS: The chamber is used to measure indoor temperature fluctuation, heat loss and

heat gain through building envelopes, energy conservation and

moisture condensation studies,

and air infiltration under simulated and dynamically fluctuating

outdoor temperature cycles. The

chamber has been used to test a wide variety of conventional and

special structures and equipment,

including military hardware (such

as inflatable life rafts, relocatable

air-inflatable hospital units, and

portable walk-in coolers) under ex- treme climatic condiUons.

AVAILABILITY: This facility, along

with several smaller chambers

(including one designed for

vehicles), has substantial potential for use by researchers in

industry and universities. Collaborative programs and individual research can be arranged.

CONTACT: David A. Didion

B114 Building Research

(301) 975-5881

CALIBRATED

HOT BOX

The calibrated hot box measures

the heat transfer coefficient of fullscale building wall sections. Designed in accordance witli ASTM Standard C976, it consists of two large, heavily insulated cham77 BUILDING AND FIRE RESEARCH
RESEARCH FACILITIES

bers—an environmental chamber

and a climatic chamber—each

with one open side. Indoor and

outdoor conditions are simulated

in the chambers. The open test section measures 3 m x 4.6 m. A wellinsulated frame supports the wall specimen that is clamped between

the open sides of the two chambers.

CAPABILITIES: This facility is the

only one of its kind designed to perform simultaneous dynamic

transfer measurements of air,

moisture, and heat during simulated winter and summer conditions under steady-state and

dynamic climatic conditions.

While the environmental chamber

temperature and humidity are maintained to simulate a relatively steady and narrow range of indoor conditions, the climatic

chamber can attain temperatures

ranging from -40 °C to 65 °C. The apparatus measures the perfor- mance of homogeneous or composite walls having a range of thermal resistance from 0.35 m^

to 8.8 m^ • C/W. It accommodates

wall specimens up to 0.6 m thick

and up to 700 kg/m in weight per

unit area.

APPLICATIONS: NIST researchers

use the facility to develop standard

test methods to evaluate dynamic

thermal performance of full-scale

walls under cyclic temperature

conditions. The building industry

and government agencies are seek- ing reliable evaluation techniques

for wall thermal mass, especially

to predict energy consumption of

buildings with heavy mass effects

in comparison to standard woodframe buildings.

NIST has participated in roundrobin test activities with domestic

and overseas thermal insulation

laboratories.

AVAILABILITY: The facility

provides a unique opportunity to measure simultaneous transfer of

air, moisture, and heat through

wall and roof specimens with openings for windows and doors. While

available for use by those outside

NIST, this apparatus must be

operated by NIST staff.

CONTACT: A. Hunter Fanney

B320 Building Research

(301) 975-5864

LINE HEAT-SOURCE

GUARDED HOT PLATE

The 1-m guarded hot-plate apparatus measures thermal conductivity of building insulation. NIST

researchers use the hot plate to

provide calibration specimens for guarded hot plates in other

laboratories. The hot plate also is

used to investigate edge heat loss from thick thermal insulation materials. This facility is the only one

of its kind in the world that will permit low-density thick insulation to be measured with an uncertainty of less than 0.5 percent.

CAPABILITIES: This apparatus has

a test temperature range of 80 °C for the hot plates and

-20 °C for the cold plates. The apparatus permits measurement of

vertical and horizontal heat flow

to simulate heat transfer through

ceilings and walls, respectively.

This apparatus operates within

its own carefully controlled temperature and humidity en- vironment shielded by an insulated aluminum enclosure. This

facility provides for absolute meas- urement of thermal resistance of

thick and low-density test specimens used as transfer standards. These standards are used to

calibrate or verify heat flow meter (ASTM C508) or guarded hot-plate

(ASTM CI 77) equipment.

AVAILABILITY: This apparatus is

available for use by those outside

NIST, but it must be operated by

NIST staff. Collaborative programs

may be arranged.

CONTACT: A. Hunter Fanney

B320 Building Research

(301) 975-5864

FIRE RESEARCH

FACILITIES

As the federal government's principal fire research laboratory,

NIST maintains some of the

country's best and most extensive

fire testing facilities. A substantial

portion of NIST's fire tests are per- formed in a specially equipped fire

research building, which measures

27 m X 57 m and is designed for

large-scale fire experiments.

Smoke abatement equipment permits large fire tests to be conducted safely without polluting

the environment.

In addition to several individual burn rooms, which are modified from time-to-time to ac- commodate special NIST testing

requirements, the facility also houses several specially designed

calorimeters for measuring the

rate of heat release from materials

and large samples, a room/

corridor facility for studying

smoke and toxic gas transport,

pilot furnaces, and reduced-scale

model enclosures. Also, a two-story

"townhouse" is used to study fire

spread from a burning room, smoke transport between levels, and sprinkler performance. The

townhouse features a living room

that is continuously weighed, al- lowing the burning rate of finish

materials to be measured.

A new computer-based data acquisition system provides state-ofthe-art data collection capabilities

for all large-scale fire testing. Up

to 300 instruments with scanning

rates over 100 channels per second can be dedicated to a single test. During an experiment, real-time,

full-color graphics present the data as collected, with automatic

conversion to engineering units

for gas analysis, rate of heat

release, temperature, and other measurements. A fire simulation laboratory,

containing personal computers,

state-of-the-art graphics, video

and reference materials, and associated databases, is used to

develop, demonstrate, and apply

fire modeling computer programs.

CAPABILITIES:

Heat-Release Rate Calorimeters.

NIST pioneered and developed the oxygen consumption methodology

for measuring the rate of heat

release and has used it longer and

in more devices than any other

laboratory. The major benefit of

this technique is the independence

of the apparatus in measuring enthalpy responses to changes in

heat release rate. NIST has two calorimeters

available for measuring the rate of

heat release of freestanding items,

such as pieces of furniture. The

smaller one has a capacity of

\i MW; the larger, 7 MW.

Provisions for measuring smoke

production and gas species yield

are available with both instruments.

78
Fire protection engineer

Vytenis Babrauskas helped

develop the NIST cone

calorimeter, it provides

data critical to predicting

the fire hazard of a product

using a small sample of material—replacing timeconsuming and expensive

full-scale tests.

Room/Corridor Facility. NIST

researchers have constructed and

used a room/corridor faciUty to

evaluate an analytical model that

predicts the transport of smoke

and toxic gases from the room of

fire origin into the corridor and

secondary target rooms. The

design of this facility makes it possible to measure the hazards associated with the burning of wall

linings or room furnishings by

evaluating the rate of heat release,

smoke production, and toxic gas

generation. The facility is available in its present form or with

design modifications for evaluating a variety of building contents and furnishings.

Burn Rooms. A standard burn room built to ASTM specifications,

2.4 m X 3.7 m X 2.4 m high, adjoins a large overhead hood that

collects the exhaust products from

the room fires. The exhaust collection system is calibrated to measure the rate of heat release and the generation rates of smoke

and other combustion products

from the fire. The burn room is

available for developmental and

validation studies of mathematical models and for studies of fire performance of furnishings and interior finish materials.

The room fire environment can be characterized in terms of

temperature and pressure

gradients and the spatial distribution of thermal flux, gaseous combustion products, and smoke.

Other measurements permit the

calculation of thermal losses to

the room boundaries and mass

and energy flows from the room.

Smaller burn rooms also are

available.

Pilot Furnaces. A pilot furnace

for evaluating the fire endurance

of wall assemblies or floor/ceiling

assemblies is available. This furnace, capable of handling

specimens 1 m x 1 m, may be

used for research purposes only

and cannot be used for code acceptance testing. Typically, fire exposure similar to that specified by

ASTM E119, under carefully controlled conditions of furnace pressure and oxygen concentration, can be carried out. Depending on

the parameters required, a variety

of other exposure conditions can

be applied.

Reduced-Scale Models. NIST

facilities are available for reducedscale modeling of full-scale fire

configurations. Physical models

offer an economical means of

achieving sufficient variation of

physical parameters for a generalized understanding of fire behavior. Based on the results of

reduced-scale experiments,

limited full-scale verification then can be performed.

Fire Simulation Laboratory. The

laboratory contains four personal

computer workstations, a highresolution graphics workstation, a

digitizing table for entering building design data, a plotter, and a

printer. The workstations are connected to NIST's mainframe computers, a minicomputer, and the computerized database in the Fire Research Information Service. Computer programs available

for use and development in the

laboratory address room fire

growth, fire and smoke transport

through buildings, building structural fire protection, escape and

rescue, and sprinkler response.

Special graphic display programs

also are available. A database for

use with some of the programs has

been assembled.

AVAILABILITY: Industry, university, and government representatives are encouraged to use

these fire testing facilities on a collaborative or independent basis,

with certain restrictions. For safety

reasons, NIST staff must closely

supervise all use of the facilities.

CONTACT: Jack E. Snell B2I8 Building Research

(301) 975-6850

79 BUILDING AND FIRE RESEARCH
COMPUTER

SYSTEMS

LABORATORY

Both users and manufacturers of computer and telecommunications teclinology benefit from tlie work of the

NISI Computer Systems Laboratory (CSL). Its research

and testing programs foster the orderly development of an "open systems" environment intended to make all forms

of information technology compatible and interoperable.

For manufacturers of hardware and software, industrywide adoption of standards expands marketing opportunities, and users are freed of the constraints and

frustrations of incompatible proprietary systems.

IVIuch of the laboratory's work is devoted to advising and

assisting industry in developing standards that satisfy user needs and yet accommodate innovations that differentiate

the products of competing vendors.

Emerging Integrated Services Digital Network (ISDN)

technology will permit simultaneous transmission of

digitized voice, data, text, and images over telephone

lines. A CSL-created forum for North American manufacturers and users of ISDN is helping define both potential

ISDN applications and their underlying technical specifications. Similar efforts are intended to refine and further the

adoption of communication protocols supporting the Open

Systems Interconnection model and the evolving Portable

Operating System Interface for Computer Environments. In addition, laboratory personnel perform conformance tests

to evaluate the compatibility of new products with these

and other standards.

To help protect information in federal computer systems,

laboratory personnel advise and assist federal agencies in

planning computer security programs, increasing awareness of the need for computer security, and carrying out

computer security training.

The laboratory also has research programs on computer

security, parallel processing, automated speech recognition, database and network management, software

engineering, and other topics related to the effective use

of information technology.

Contact: James H. Burrows

B154 Technology

(301) 975-2822

COOPERATIVE

RESEARCH

OPPORTUNITIES

INFORMATION

SYSTEMS

ENGINEERING

DATABASE TESTING

To aid the management of information resources, NIST researchers are developing test methods and techniques for

evaluating implementations of the database language SQL and Infor- mation Resource Dictionaiy System (IRDS) for conformance to

federal, national, and international standards. The researchers are attempting to derive a general

methodology for designing confor- mance tests, to use this methodology to generate test suites, and to

evaluate the test suites for effectiveness. A prototype implementation

of the IRDS specifications, which

may be suitable for such tasks as modeling the structure of a stan- dard and for recording the parts of

a standard specifically tested, will

be used in this project.

CONTACT: Alan H. Goldfine

A266 Technology

(301) 975-3252

GEOGRAPHIC

INFORMATION SYSTEMS

Geographic information systems

(CIS) technology allows users to

collect, manage, and analyze

large volumes of spatially refer- enced and associated data. New

research directions are emerging

from the interdisciplinary uses of

GIS. NIST researchers are exploring future GIS technology through

studies into integrating computer

graphics standards, database

management standards, expert sys- tems technology, and optical disk

technology to support GIS applications. Their research is focused on

providing GIS compatibility

through standards and confor- mance testing for future GIS standards, such as the Digital

Cartographic Data Standard. Because the activities of many

governmental and private organizations are land and/or locationally related, GIS technology

will be important in integrating

existing spatial data for these

organizations.

CONTACT: Henry Tom

A266 Technology

(301) 975-3271

COMPUTER

GRAPHICS TESTING

The development of several

graphics standards and work on

related conformance testing and

measurement techniques for

graphics software are under way

at NIST. Specifically, NIST researchers are testing implementations of the graphical kernel

system (GKS), the computer

graphics metafile (CGM), and the programmer's hierarchical interactive graphics system (PHIGS)

for conformance to existing and

emerging federal, national, and international standards.

Researchers are attempting to

derive a general methodology for

designing conformance tests, to

use this methodology to generate

test suites, and to evaluate the test

suites for effectiveness. The computer graphics laboratory, which

contains various computer

graphics hardware and software

systems designed to support stan- dard specifications, is used in

80
these efforts. An existing test suite

for GKS is available with a FORTRAN interface. Priority is being given to testing methodologies and test suites for PHIGS,

COM, and the conversion of FORTRAN tests for all computer

graphics standards to other lan- guages (C, Pascal, and Ada).

CONTACT: Mark W. Skall A266 Technology

(301) 975-3265

SYSTEMS AND

SOFTWARE

TECHNOLOGY

INTERFACES FOR

COMPUTER

ENVIRONMENTS

For the past several years, NIST

has collaborated with vendors,

users, and voluntary standards

organizations to advance the implementation and use of the stan- dard on Portable Operating

System Interface for Computer

Environments (POSIX). POSIX

promotes the portability of computer applications at the source

code level. NIST researchers continue to work with voluntary standards committees to develop

additional standards needed for

interfaces to operating systems, including commands and utilities, system administration, and operating system security. Research

efforts focus on the operating sys- tems functional areas of NIST's

Application Portability Profile for Open System Environments, which

integrates federal, national, and

international standards to provide

functionality needed for a broad

range of government information

technology applications.

CONTACT: Allen L. Hankinson

B266 Technology

(301) 975-3290

INTERACTIVE

MEDIA

Portable multimedia courseware (computer-based interactive training software) provides a viable

alternative to the current practice

of distributing courseware with

proprietary interfaces to system services. NIST and other federal agencies are working together to

develop a strategy for multimedia

courseware that would create an

environment in which highquality portable courseware is

available as commercial, off-theshelf products competitively supplied by vendors. Researchers are

developing a computer-based interactive training applications profile

that would identify needed standards in response to user needs.

CONTACT: Allen L. Hankinson

B266 Technology

(301) 975-3290

SOFTWARE

QUALITY

Growing dependence on computers requires assurance that

critical systems will operate reliably and exactly as intended

without adverse effects, even when

outside circumstances cause other

systems to fail. NIST researchers

are studying problems and potential solutions in building and

operating high-integrity systems

and are looking at life-cycle

methodology, risk management.

formal methods, object-oriented

design, software reliability, clean- room techniques, and formal

verification.

CONTACT: Allen L. Hankinson

B266 Technology

(301) 975-3290

COMPUTER

SECURITY

COMPUTER

SYSTEMS SECURITY

Computer systems are vital ele- ments of today's business and

scientific environments. However,

as sensitive and critical information is processed and stored on

computer systems often interconnected by local area networks,

there is an increasing need for methods to protect that information from unauthorized access or

modification. But selection of in- formation security measures

should be based on cost analysis of such measures and the resulting

reduction in losses. NIST researchers are investigating various technologies that can be used to

achieve additional control and

security of information on computer systems. Their research involves the identification, analysis,

development, and application of

these technologies.

Although it is desirable to have security mechanisms as an

integral part of computer systems

and networks, this is not always

possible or economical because

such mechanisms often are not

part of the original system design.

NIST researchers also are examining the technology available to enhance the security of existing

systems. This research involves

identifying, analyzing, and comparing security mechanisms used

in isolation or combination.

CONTACT: Stuart W. Katzke

A2l6 Technology

(301) 975-2934

SECURITY IN ISDN AND

OSI NETWORKS

NIST has initiated a laboratorybased program to bring together

government organizations and

contractors interested in interoperability and security in the Open Systems Interconnection

(OSI) computer network architecture and the Integrated Services

Digital Network (ISDN) communications architecture. Researchers develop prototype

systems to demonstrate the interoperability of proposed standards

for OSI and ISDN using a selected

set of security services. These standards are expected to be implemented in commercial

applications with a broad market.

Researchers plan to develop

demonstration prototypes of applications and equipment, including hardware and sof^vare, that

provide one or more levels of

security in an OSI and/or ISDN en- vironment. Specifications will be

developed for data formats,

protocols, interfaces, and support

systems for security in an OSI/ISDN environment that can

be used as a basis for Federal Infor- mation Processing Standards.

Users, developers, and vendors

jointly can define, develop, and

test systems that will provide a

rjinge of telecommunications, net- work management, and security

services in a distributed information processing environment.

CONTACT: Stuart W. Katzke

A2l6 Technology

(301) 975-2934

81
COOPERATIVE RESEARCH OPPORTUNITIES

MALSOSQUS CODE AND

RELATED THREATS

Operators and users of computer

systems and networks are experiencing an increased number of incidents of malicious code (such as computer viruses and "worms"),

unauthorized access ("hackers,"

for example), and similar threats.

Protection from such threats

requires a combination of management awareness, user involvement, and technical protection.

NIST researchers are actively involved in improving each of these

areas. Their research involves an

understanding of both the potential technical vulnerabilities of sys- tems and of how systems are used

and administered. Advanced

methods of system protection,

anomaly detection, system selfaudit, and related techniques are being developed. In addition,

methods of rapid reaction and

response to computer security incidents are being developed and

coordinated throughout the

federal government.

CONTACT: Stuart W. Katzke

A2l6 Technology

(301) 975-2934

NETWORK SECURITY

ARCHITECTURE

To protect computer systems and

networks, NIST is developing a comprehensive security architecture consistent with the Open Sys- tems Interconnection (OSI)

Reference Model.

Cryptographic functions are being implemented in certain OSI

layers to provide data secrecy, data

integrity, and peer entity authentication. The research will combine the security standards for

individual OSI layers into a

unified security framework. As

The cryptographic adapter

held here by computer

specialist Shu Jen Chang is one of several being

evaluated for various applications by NIST computer

security researchers.

part of this project, NIST researchers will define a common

interface for cryptographic algorithms and develop a key management methodology capable of providing keys to the cryptographic functions of any layer.

CONTACT: Stuart W. Katzke

A2 16 Technology

(301) 975-2934

SYSTEMS AND

NETWORK

ARCHITECTURE

NETWORK

MANAGEMENT

NIST researchers are working with

industry to establish a set of standards for exchanging network

management information between

heterogeneous management systems. Their goal is to establish a

standard enabling integrated,

interoperable, automated management of multivendor computer systems, routers, bridges, switches,

multiplexors, modems, and

provider services. The researchers are defining

protocols for exchanging management information; identifying, collecting, and specifying the format

of managed objects; defining

protocols to support management

functions in the areas of fault, configuration, performance, security,

and accounting; and implementing prototype management sys- tems reflecting the protocols and

specifications. Other research

areas include network management user displays, network

management applications

software development, and application of expert systems to network

management.

CONTACT: Kevin L. Mills B2 17 Technology

(301) 975-36I8

DIRECTORY SERVICES

AND DYNAMIC ROUTING

In cooperation with industry, NIST

is pursuing development of commercial off-the-shelf products implementing standard distributed

directory services and dynamic

routing. The distributed directory

services require research work in

several areas, including access

control, replication of information, extension of directory

schemas, and distributed update.

Proposed solutions to these directory problems are implemented

and tested in a NIST prototype

directory implementation con- forming to the international directory standard (X.500).

The aim of NIST dynamic rout- ing research is development of an

international standard for the ex- change of routing information

between autonomous domains.

NIST researchers propose and

analyze a variety of mechanisms

to accommodate such exchanges,

and they investigate proposed

algorithms through simulation

models.

CONTACT: Kevin L. Mills B2 17 Technology

(301) 975-36I8

AUTOMATED PROTOCOL

METHODS

NIST researchers are designing

tools for editing, compiling, and

interpreting computer communications protocol specifications. The goal of the research is

to advance the state of the art in

using such tools to realize automatically executable implementation of the protocols. As part of

this project, NIST researchers are

developing a syntax-directed

82
editor for Estelle and, using the same grammar, devising a portable compiler for Estelle and the supporting runtime libraries.

CONTACT: Kevin L. Mills B2 17 Technology

(301) 975-3618

ADVANCED

SYSTEMS

INTEGRATED SERVICES

DIGITAL NETWORKS

In cooperation vi^ith industrial and

other users, NIST advances the development of standards for Integrated Services Digital Networks

(ISDN), which combine voice,

data, text, and image communications over a single network connection. Research in this area focuses on the measurement capabilities

and testbed facilities required to

develop conformance tests and per- formance metrics for emerging

ISDN standards. Activities include

support for standards writing,

development of the technical foundation for implementation agree- ments on protocol options, and

testing ISDN implementations for

interoperability. NIST researchers

also are involved in the research

and standardization of B-ISDNbased protocols as well as FDDI

conformance tests.

CONTACT: David Su

B364 Materials

(301) 975-6194

PERFORMANCE OF

MODERN-ARCHITECTURE

COMPUTERS

NIST researchers in the area of computer-systems performance

are promoting the effective evaluation and efficient use of advanced

computers by the federal govern- ment. Their areas of interest include: characterization of new

computer architectures to identify

improved ADP technology for applications; exploration of economical programming methods that standardize across classes of architecture; and design of coherent

evaluations that economically

and reliably characterize the machines. Two dedicated, instru- mented multiprocessors serve as

special project resources. One has

16 nodes loosely coupled as a

hyper-cube; the other has

16 processors in a shared-memory

configuration.

These NIST researchers also

are involved in the development of instrumentation and related management techniques for

gigabit networks used for

visualization-based applications.

CONTACT: Robert]. Carpenter

B364 Materials

(301) 975-5677

As industrial standards for optical

disk media evolve, test methods

will be needed for conformance

testing of the media. NIST researchers are setting up a

laboratory to develop and

demonstrate data/media inter- change tests and to verify confor- mance to established or planned

national and international standards for rewritable and write

once, read many (WORM) type

optical disks. The program will be

coordinated with voluntary standards committees and interested

federal agencies.

CONTACT: Dana S. Grubb

A61 Technology

(301) 975-2915

DISTRIBUTED

SYSTEMS

NIST researchers are developing

application profiles that will promote integrated platforms for

video, imagery, computer data,

and voice, thus defining multimedia applications in a distributed processing environment.

This research focuses on

prototype development and

demonstration using ISDN

technology.

CONTACT: Wayne H. McCoy

A2 16 Technology

(301) 975-2984

AUTOMATIC SPEECH

RECOGNITION

Recent advances in automatic

speech recognition technology

have resulted in computers able to

recognize correctly continuous

speech with lexicon sizes of at

least 1,000 words. Speech

databases are typically large in

size (gigabytes) and too costly for any one organization to develop.

To improve the technology, the research community relies heavily on shared use of the databases and

standard test methodologies.

With support from the Defense

Advanced Research Projects

Agency and other agencies, NIST

has collected speech database material and, using CD-ROM technology, distributed this material to more than 100 research organizations. Researchers at NIST also have developed CD-ROM format

speech databases that are used for

speech recognition research in

large vocabulaiy speech (5,000-

word office correspondence), word

spotting, speaker identification/

verification, and goal-directed

spontaneous speech. Among the research facilities used are a VAX

1 1/780, a Sun workstation, and

speech-processing peripherals and

software tools. Areas of interest include characterization of the

speech database materials (such

as acoustic-phonetic locators and

classifiers), artificial neural nets, performance measurement, and

natural languages.

CONTACT: David S. Pallett A2 16 Technology

(301) 975-2935

IMAGE

RECOGNITION

Image-recognition research at NIST focuses on developing

methods for evaluating image

quality, compression efficiency,

and image systems used in opticalcharacter recognition. These

evaluation methods are designed

to include highly parallel computers and special-purpose chips

as well as conventional computer

architectures. The methods being

developed are used for automated

fingerprint recognition, automation of data entry from images of

forms, and measurement of recognition systems on realistic applications. A general model of the

recognition process in parallel

computers is being implemented

to provide better methods to

analyze the performance of SIMD (single-instruction,

multiple-data) computers for image compression, image qualit)'

evaluation, and recognition

accuracy. CONTACT: Charles L. Wilson

A2l6 Technology

(301) 975-2080

83 COMPUTER SYSTEMS LABORATORY
RESEARCH

FACILITIES

INFORMATION

SYSTEMS ENGINEERING

FACILITY

The information systems engineering facility consists of laboratories

with the computer hardware and

software needed for research and

development of standards,

guidance to federal agencies, and

validation tests. The following

areas are included: graphics;

programming languages; database

management systems; distributed

database management systems; object database management systems; data dictionary systems; data

administration, especially

database design; data interchange;

knowledge-based and expert systems; and geographic information

systems (GIS).

CAPABILITIES: The facility contains a variety of computers.

Among them are a VAX 1 1/785,

Symbolics 3650 LISP machine,

386 and 486 microcomputers,

Macintosh II, Silicon Graphics

IRIS workstation, and a SUN

SPARC II workstation. Other computer systems, such as the NIST

Cray Y-MP supercomputer, are accessible. Also available are a

variety of hard-copy output devices, such as laser printers, camera output systems, and color thermal transfer printers.

Software used in the facility

includes:

graphical kernel system (GKS)

and programmer's hierarchical interactive graphics system (PHIGS)

implementations, which allow

graphics programmers to design a wide variety of graphics programs,

ranging from simple passive

graphics to complex real-time

systems;

computer graphics metafile

(CGM) implementations that per- mit transfer of graphical pictures

among heterogeneous graphic

devices;

a variety of programming lan- guage processors and system

software; database management systems

for the VAX, workstations, and

microcomputers supporting SQL

and object technologies;

a prototype implementation of

the Information Resource Dictionary System (IRDS) standard; LISP and Prolog;

microcomputer expert system

shells; and

GIS systems.

Validation suites are available

for testing conformance to Federal Information Processing Standards

(FIPS) for COBOL, FORTRAN,

Pascal, Ada, GKS, CGM, and

database language SQL. Testing

services are provided for COBOL,

FORTRAN, Pascal, Ada, GKS, CGM,

and SQL.

APPLICATIONS: An active area of

cooperative work is the development and evaluation of tests to

validate the conformance of lan- guage processors and other system

software to FIPS. Major programs

under way are: validation of the programming language processors COBOL, FORTRAN, Pascal, and

Ada; validation of the GKS, PHIGS,

and CGM graphics systems; validation of database language SQL;

and validation of IRDS.

Possible future work includes

the development of tests and procedures for validating additional

programming language systems,

such as VHSIC Hardware Description Language, MUMPS, C, LISP,

and Prolog; for validating the computer graphics interface; and for

validating the following data

management and data inter- change software: SQL2, SQL3,

84

data description file for information interchange, and abstract syntax notation one (ASN.l).

AVAILABILITY: The facility, which

must be used under the guidance

of NIST staff, is available for collaborative projects in test development and application research.

CONTACT: David K.Jefferson A266 Technology

(301) 975-3262

COMPUTER AND

NETWORK SECURITY

FACILITY

The NIST computer and network

security facility is used to improve

the current security posture of

federal computer and telecommunication systems and to provide security for these systems as

they migrate toward open system

environments. Research done in

the facility is aimed at applying

methods to protect the secrecy and

integrity of information in computer systems and data networks;

evaluating personal identification and authentication techniques to

control access to information

resources; and developing computer and network security architectures to determine proper

implementation of controls for integrity and confidentiality of infor- mation and authentication of

users.

CAPABILITIES: The facility is equipped with mini- and

microcomputers, security devices,

terminals, personal identification

systems, and access to large

mainframes and supercomputers

through local area, national, and

global networks. A variety of communications technologies and applications environments are

available for research efforts, in- cluding Open Systems Interconnection and Integrated Services

Digital Network for developing

and testing security protocol

standards.

Operational capabilities include a computer emergency

response team to facilitate identification and response to acute

Using an Integrated Services Digital Network

software pacl(age, computer scientists Douglas

White and Camie Roberts

demonstrate how this technology will allow remotely

located computer users to participate in voice and

video conferencing.
computer and telecommunications security incidents involving

self-repiicating computer viruses.

Test and evaluation capabilities

range from specific functionality

tests of cryptographic modules to

test methodologies for network

security protocols to the specific

criteria used to evaluate the

trustworthiness of systems that handle unclassified, but sensitive,

data.A risk management laboratory,

utilizing a Dell System 325 (AT

clone), is available for research in

risk management techniques and

methodologies and evaluation of

risk management software to deter- mine applicability to different agency environments. Three Sun

computers support the development of advanced computer access

control systems based on smart

token technology. The virus

laboratory uses two IBM PS/2

Model 60s, a Sun workstation for

research in multiuser environments; and a Macintosh SE for research in the MacOS environment.

A small systems security laboratory

completes the computer and net- work security facility.

APPLICATIONS: The facility is used primarily to develop and test

federal standards for computer

and network security. Support is

provided to other federal agencies

and industry where the protection

of unclassified data is required.

AVAILABILITY: Collaborative research programs can be arranged.

CONTACT: Stuart W. Katzke

A2 16 Technology

(301) 975-2934

ISDN AND DISTRIBUTED

SYSTEMS FACILITY

The NIST Integrated Services

Digital Network (ISDN) and distributed systems facility provides

laboratories for research and

development, standards, and con- formance testing in distributed computer systems and advanced

computer communications,

including ISDN and the fiber distributed data interface (FDDI). Significant research and development

programs include open distributed

systems, transaction processing,

distributed multimedia, ISDN applications, ISDN conformance testing, and broadband ISDN.

CAPABILITIES: The facility is equipped with microcomputers,

workstations, minicomputers,

multimedia display units, ISDN

and Ethernet communications,

and laser printers. Access to mainframes and supercomputers

is provided via local, national, and

global networks. The laboratories

have eight basic rate interface

(BRI) ISDN lines, three Sequent

computers (S27, S81), five Sun

workstations, four 386-class microcomputers, four ISDN ter- minal adapters, four ISDN

telephones, two ISDN protocol

analyzer/emulators, and two Macintosh microcomputers. In the

near future, researchers anticipate

access to primary rate interface ISDN as well as the BRI. The

laboratories also feature software

for compiling formal descriptions

of distributed systems into implementations, tool kits for programming distributed systems,

and user interfaces as well as advanced operating systems such as MACH.

APPLICATIONS: Facilities are used

primarily for developing and test- ing federal, national, and international standards for advanced

communications and distributed multimedia systems.

Research activities support the North American ISDN Users' Forum, chaired by NIST. The

forum was established by NIST

with industry in 1988 to create a

strong user voice in the implementation of ISDN applications.

Through the forum, users and

manufacturers concur on ISDN applications, the selection of options

from standards, and conformance

tests. NIST works with the forum

to develop tests that determine

whether the agreed-to specifications will result in compatible

products and services. A principal focus is standards

conformance test design for ISDN

implementations based on CCITT

recommendations. NIST has

developed reference implementations for the Q.92I andQ.931

recommendations, conformance

test suites for both recommendations, and a conformance test sys- tem based on these items. In

addition, conformance research on broadband ISDN is conducted.

Also under development are application profiles for ISDN, research in distributed computing

environments, and prototype distributed multimedia information

systems based on ISDN and other

communications media. Researchers have produced a distributed reference implementation

for the International Standard

Transaction Processing Protocol

directly from a formal specification and are investigating how

transactions support multimedia

information access and cooperative processing.

AVAILABILITY: Collaborative research programs with government,

industry, and academia can be ar- ranged and are encouraged.

CONTACT: Shukri A. Wakid

A224 Technology

(301) 975-2904

85 COMPUTER SYSTEMS LABORATORY
COMPUTING AND

APPLIED MATHEMATICS

LADORATORY

The NIST Computing and Applied Matliematics Laboratory

develops mathematical, statistical, and state-of-the-art

scientific computing tools that help other NIST researchers

and collaborators accomplish their research objectives.

In new initiatives focusing specifically on the needs of

U.S. industry, the laboratory is developing algorithms,

databases, and software for computer-aided modeling of

complex phenomena, such as charge distribution in semiconductors, protein folding, and phase changes in structural materials. In the ongoing Design for Quality

program, laboratory scientists and collaborators from

industry and academia are developing and refining new

statistical, mathematical, and computer-based models for

improving and integrating the design, engineering, and

manufacturing of new materials and products. NIST materials scientists and engineers are using these methods to improve the fabrication of advanced ceramics.

Other research programs focus on advanced computer

graphics programs that produce two- and threedimensional visualizations of complex problems or create

images integrating data from scientific experiments.

NIST-pioneered methods for displaying, manipulating,

analyzing, and transmitting large volumes of data are

providing researchers with new perspectives and new ex- perimental capabilities. The laboratory also is developing

software applications for harnessing the problem-solving

power of parallel processors, an effort carried out in

conjunction with the federal government's muitiagency

program on high-performance computing and

communications.

Contact: Francis E. Sullivan

B11 2 Technology

(301) 975-2732

COOPERATIVE

RESEARCH

OPPORTUNITIES

APPLIED AND

COMPUTATIONAL

MATHEMATICS

SCALABLE PARALLEL

ALGORITHMS

A major problem for users of massively parallel computers is the

lack of libraries of commonly used

subroutines. Algorithms and computer codes developed for singleprocessor machines rarely give

massive speedups when transferred

to massively parallel computers.

NIST researchers concentrating on algorithm research for massively parallel computations are making substantial progress in al- gorithms for important problems

in computational geometry, such

as triangulation in two and three dimensions. Additional research

focuses on random processes, in- cluding Monte Carlo simulations,

and randomizing algorithms.

CONTACT: Francis E. Sullivan B 112 Technology

(301) 975-2732

NON-LINEAR

MECHANICS

Mathematical analysis, used with

symbolic computation, leads to efficient analytical approximations

by computers. Perturbation algorithms applied to non-linear differential equations, especially in

celestial mechanics, result in

analytical developments where the complexity grows exponentially

with the order of the approximation. Several avenues are being explored at NIST to simplify literal developments generated by perturbation algorithms applied to nonlinear systems. These include

identifying algebraic structures on

the domain of the normalization.

smoothing transformations to eliminate perturbation terms outside the kernel of the Lie derivative, preparatory transformations

of a geometric nature, and creat- ing natural intermediaries.

Problems being examined in- clude resonances at an equilibrium, perturbed pendulums,

and the major theories of celestial mechanics. NIST researchers,

using a LISP computer, are focus- ing their studies on algorithms

amenable to computer automation through symbolic processors.

CONTACT: Andre Deprit

A302 Administration

(301) 975-2709

MATHEMATICAL

MODELING AND SOFTWARE

Mathematical and computational

problems are becoming more

elaborate as measurement techniques, physical understanding,

and computational capability improve. Solving these problems requires innovative combinations of

the methods of modern applied

and computational mathematics.

With scientists and engineers,

NIST mathematicians develop and

analyze mathematical models of phenomena; design and analyze

computational methods and experiments; transform these methods into efficient numerical

algorithms for modern, highperformance computers; and implement them in high-quality

mathematical software. Active

areas of interest include crystal

growth, fluid flow, electromagnetic waves, magnetic materials,

molecular dynamics simulations,

partial differential equations, and

several kinds of inverse problems.

CONTACT: James L. Blue

A238 Administration

(301) 975-3809

86
OPTIMIZATION AND

COMPUTATIONAL

GEOMETRY

In many aspects of NIST's research, the need arises for computational procedures, such as

curve fitting, parameter estimation, and maximum entropy calculations. These activities require

solving various types of optimization problems. NIST researchers

investigate many aspects of numerical optimization, including large-scale linear and quadratic programming problems by

interior-point methods, and the extension of these procedures to

general large-scale non-linear

programming problems via sequential quadratic programming

methods. Researchers also have

developed procedures for nonlinear least squares and orthogonal distance regression

problems, and they produce

software for these methods as needed.

Computational geometry is a

rapidly emerging field with applications in robotics, statistical mechanics, cartography, computer

graphics, materials science, and

molecular dynamics. Researchers

at NIST have developed robust and

efficient computational schemes

to compute tri angulations and

shellings of point sets, Voronoi

diagrams, and other geometrical

calculations. Algorithms for two- and three-dimensional triangulation have been implemented for

sequential and parallel machines

and are used at NIST and other

scientific centers.

CONTACT: Paul T. Boggs

A238 Administration

(301) 975-3816

STATISTICAL

ENGINEERING

DESIGN FOR QUALITY

Through its Design for Quality

(DFQ) program, NIST supports collaborative research within NIST

and with industry, academia, and

technical societies to develop tech- nology for quality improvement.

Such collaborations are aimed at meeting critical industrial product

and process design needs. A typical

collaboration involves industrial

partners, NIST and academic subject matter experts, and NIST

statisticians, mathematicians, and

computer scientists. The technology developed is disseminated

through industrial collaborations,

tutorials, workshops, conferences,

and publications. Current DFQ

projects include technology

development for advanced materials characterization, formulation and processing, and

computer-integrated flexible piece

parts manufacturing.

Materials being investigated include: silicon nitride, reinforced

structural ceramics, superconducting ceramics, atomized metals,

polymer composites, dental and

medical materials, and artificial diamond films. The techniques of

statistically planned experiments

are used to understand the cause and effect relations among measurement, testing, and processing

parameters; microstructural features; mechanical, electrical, and

chemical properties; and perfor- mance attributes.

In the area of computercontrolled high-precision machining, statistical methods and other

quality techniques are used to

characterize and model those factors affecting dynamic friction.

derive correction factors to compensate for backlash and temperature bias, and determine adaptive

servo-control process parameters

for optimal operation.

CONTACT: Raghu N. Kacker

A337 Administration

(301) 975-2109

MEASUREMENT

ASSURANCE

Quality assurance for physical and

chemical measurements requires assessment of uncertainties for highly precise measurement sys- tems and development of on-line

quality control strategies. NIST

statisticians, confronted with difficult uncertainty problems,

develop and refine methods, such

as the bootstrap, for application to experiments like the recent redeter- mination of the atomic weight of

nickel or determining confidence

intervals for polarized beam measurements. Methods for developing

and validating models are explored for dealing with complex

error structures.

In the process control area, change-point algorithms and computer-intensive software have been

applied to a materials reliability

problem where a noisy sequence of welding voltages contains peaks indicating points of metal detachment. The programs were

originally developed by NIST researchers to detect changes in chemical processes. Research is

still needed for electronic systems

where autocorrelative structure and limited knowledge of the underlying distribution of in-control

measurements are at issue.

Calibrations, where instrument

response depends on stimuli over a

regime, is of ongoing interest. Research is focused on optimal procedures for real-life models and on

improving uncertainty estimation

for Scheffe-type bounds.

CONTACT: M. Carroll Croarkin

A337 Administration

(301) 975-2849

SCIENTIFIC

COMPUTING

ENVIRONMENTS

SCIENTIFIC

VISUALIZATION

Researchers at NIST are developing and applying advanced

methods for using state-of-the-art,

computer-based scientific graphics

for rendering complex experimental, computational, and analytical

results in physics and chemistry.

Researchers use a collection of

vector and raster workstations,

photographic and video hardware,

high-speed networking for trans- mitting large graphics data sets between computers and graphics

devices, and computational

geometry algorithms and software

for the analysis of two- and three- dimensional data sets. Techniques

also have been developed to manipulate dynamic objects in automated design and manufacturing systems; to display

quasicrystal structures with

icosahedral symmetries and scan- ning electron tunneling microscopy data with polarization

analysis; and to study models of

turbulent combustion showing the dependence of solutions on time

and fuel-oxidizer mixture

parameters.

CONTACT: Sally E. Howe

B146 Technology

301/975-3807

87
FACILITIES

INDEX

Acoustic Anechoic Chamber 31

Automated Manufacturing Research FaciHty 31

Calibrated Hot Box Facility 77

Cold Neutron Research Facility 66

Computer and Network Security Facility 84

Electromagnetic Anechoic Chamber 23

Electron Paramagnetic Resonance Facility 53

Fire Research Facilities 78

Fluid Metering Research Facility 45

Ground Screen Antenna Range 22

High-Voltage Measurement Facility 21 Information Systems Engineering Facility 84

ISDN and Distributed Systems Facility 85

Large Environmental Chamber 77

Large-Scale Structures Testing Facility 76

Line Heat-Source Guarded Hot Plate 78

Low-Background Infrared Radiation Facility 52

Magnetic Microstructure Measurement Facility 54

Materials Science X-Ray Beamlines 71 Mechanical Behavior Laboratories 70

Metals Processing Laboratoiy 68

Mode-Stirred Chambers 22

Near-Field Scanning Facility for Antenna Measurements 22

Neutron Depth Profiling Facility 46

NIST Research Reactor 64

Nitrogen Flow Measurement Facility 45

Polymer Composite Fabrication Facility 68

Powder Characterization and Processing Laboratoiy 69

Radiopharmaceutical Standardization Laboratory 54

Semiconductor Processing Research Laboratory 20

Small-Angle X-Ray Scattering Facility 70

Synchrotron Ultraviolet Radiation Facility-II 52

Transverse Electromagnetic Cells 23

Tri-Directional Test Facility 76

Water Flow Measurement Facility 45

SUBJECT

INDEX

Advanced systems 83

Advanced Technology Program 7 Applied and computational mathematics 86

Atomic physics 47

Automated production technology 26

Biotechnology 32

Building environment 73

Building materials 73

Calibration and related measurement services 1

1

Ceramics 56

Chemical engineering 35

Chemical kinetics and thermodynamics 35

Computer security 81

Electricity 12 Electromagnetic fields 17 Electromagnetic technology 18

Electron and optical physics 47

Energy-related inventions 1

1

Factory automation systems 29

Fire measurement and research 75

Fire science and engineering 75

Information services 1

1

Information systems engineering 80

Inorganic analytical research 36

Intelligent processing of materials 55

Ionizing radiation 50

Malcolm Baldrige National Quality Award 6

Manufacturing Technology Centers 8

Materials reliability 57

Metallurgy 6l Organic analytical research 37

Polymers 59

Precision engineering 24

Process measurements 40

Quantum metrology 49

Quantum physics 51 Radiometric physics 48

Reactor radiation 62

Research and technology applications 9 Robot systems 27

Scientific computing environments 87

Semiconductor electronics 15 Standard Reference Data 10

Standard Reference Materials 10 Standards and certification information 8

Standards management 9

State technology outreach 9

Statistical engineering 87

Structures 72

Surface and microanalysis science 42

Systems and software technology 81

Systems and network architecture 82

Technology development and small business innovation

Thermophysics 43

Time and frequency 51 Voluntary laboratory accreditation 1

1

Weights and measures 9

88
U.S. DEPARTMENT OF COMMERCE

Robert A. Mosbacher, Secretary

Robert M. White, Under Secretary for Technology

National Institute of Standards and Technology

John W. Lyons, Director

National Institute of Standards and Technology

Gaithersburg, Md. 20899

(301)975-2000

Boulder, Colo. 80303

(303)497-3000

August 1991

NIST Special Publication 817

Prepared by the Public Affairs Division

SP 817 Staff:

Writers: Mark A. Bello, Gail Porter

Editor: Sharon A. Shaffer

Production: Virgina M. Covahey,

Sheila D. St. Clair

Graphic Design and Art Direction:

William N. Welsh, Marilyn B. Ugiansky

Principal Photographers: H. Mark Heifer,

Geoffrey Wheeler, Bessmarie Young

Illustrator: Don Price

Printing Coordination: Warren Overman

Public Affairs Division

A903 Administration Building

National Institute of Standards and Technology

Gaithersburg, Md. 20899

(301)975-2762

Any mention of commercial products is for information only;

it does not imply recommendation or endorsement by the

National Institute of Standards and Technology nor does it imply that the products mentioned are necessarily the best

available for the purpose.