AN ASSESSMENT OF THE 

NATIONAL INSTITUTE OF STANDARDS 

AND TECHNOLOGY 

MATERIALS SCIENCE AND 

ENGINEERING LABORATORY 

FISCAL YEAR 2008 

AN ASSESSMENT OF THE 

NATIONAL INSTITUTE OF STANDARDS 

AND TECHNOLOGY 

MATERIALS SCIENCE AND 

ENGINEERING LABORATORY 

FISCAL YEAR 2008 

Panel on Materials Science and Engineering 

Laboratory Assessments Board 

Division on Engineering and Physical Sciences 

THE NATIONAL ACADEMIES PRESS 

Washington, D.C. 

www.nap.edu 
THE NATIONAL ACADEMIES PRESS 500 Fifth Street, N.W. Washington, DC 20001 

NOTICE: The project that is the subject of this report was approved by the Governing Board of 

the National Research Council, whose members are drawn from the councils of the National 

Academy of Sciences, the National Academy of Engineering, and the Institute of Medicine. The 

members of the panel responsible for the report were chosen for their special competences and 

with regard for appropriate balance. 

This study was supported by Contract No. SB134106Z0011 between the National Academy of 

Sciences and the National Institute of Standards and Technology, an agency of the U.S. 

Department of Commerce. Any opinions, findings, conclusions, or recommendations expressed 

in this publication are those of the authors and do not necessarily reflect the views of the agency 

that provided support for the project. 

International Standard Book Number-13: 978-0-309-12728-8 

International Standard Book Number-10: 0-309-12728-9 

Copies of this report are available from 

Laboratory Assessments Board 

Division on Engineering and Physical Sciences 

National Research Council 

500 Fifth Street, N.W. 

Washington, DC 20001 

Additional copies of this report are available from the National Academies Press, 500 Fifth 

Street, N.W., Lockbox 285, Washington, DC 20055; (800) 624-6242 or (202) 334-3313 (in the 

Washington metropolitan area); Internet, http://www.nap.edu. 

Copyright 2008 by the National Academy of Sciences. All rights reserved. 

Printed in the United States of America
The National Academy of Sciences is a private, nonprofit, self-perpetuating society of distinguished scholars engaged 

in scientific and engineering research, dedicated to the furtherance of science and technology and to their use for the 

general welfare. Upon the authority of the charter granted to it by the Congress in 1863, the Academy has a mandate 

that requires it to advise the federal government on scientific and technical matters. Dr. Ralph J. Cicerone is president 

of the National Academy of Sciences. 

The National Academy of Engineering was established in 1964, under the charter of the National Academy of 

Sciences, as a parallel organization of outstanding engineers. It is autonomous in its administration and in the selection 

of its members, sharing with the National Academy of Sciences the responsibility for advising the federal government. 

The National Academy of Engineering also sponsors engineering programs aimed at meeting national needs, 

encourages education and research, and recognizes the superior achievements of engineers. Dr. Charles M. Vest is 

president of the National Academy of Engineering. 

The Institute of Medicine was established in 1970 by the National Academy of Sciences to secure the services of 

eminent members of appropriate professions in the examination of policy matters pertaining to the health of the public. 

The Institute acts under the responsibility given to the National Academy of Sciences by its congressional charter to be 

an adviser to the federal government and, upon its own initiative, to identify issues of medical care, research, and 

education. Dr. Harvey V. Fineberg is president of the Institute of Medicine. 

The National Research Council was organized by the National Academy of Sciences in 1916 to associate the broad 

community of science and technology with the Academy’s purposes of furthering knowledge and advising the federal 

government. Functioning in accordance with general policies determined by the Academy, the Council has become the 

principal operating agency of both the National Academy of Sciences and the National Academy of Engineering in 

providing services to the government, the public, and the scientific and engineering communities. The Council is 

administered jointly by both Academies and the Institute of Medicine. Dr. Ralph J. Cicerone and Dr. Charles M. Vest 

are chair and vice chair, respectively, of the National Research Council. 

www.national-academies.org 
PANEL ON MATERIALS SCIENCE AND ENGINEERING 

ROBERT J. EAGAN, Sandia National Laboratories (emeritus), Chair

JOHN ALLISON, Ford Motor Company 

EDMUND W. CHU, Alcoa Technical Center 

DAVID R. CLARKE, University of California, Santa Barbara 

KENNETH DAVIS, Arizona State University and Consultant 

DELBERT E. DAY, Missouri University of Science and Technology 

LISA DHAR, InPhase Technologies, Inc. 

MARK EBERHART, Colorado School of Mines 

RICHARD GAMBINO, State University of New York at Stony Brook 

WILLIAM A. GODDARD III, California Institute of Technology 

BRIDGETTE L. GOMILLION-WILLIAMS, The Dow Chemical Company 

ELIZABETH G. JACOBS, Texas Instruments, Inc. 

EDMUND H. MOORE, Air Force Research Laboratory 

OMKARAM NALAMASU, Rensselaer Polytechnic Institute 

THOMAS X. NEENAN, Warwick Effect Polymers 

THOMAS P. RUSSELL, University of Massachusetts, Amherst 

ISAAC C. SANCHEZ, The University of Texas, Austin 

MARK L. WEAVER, University of Alabama 

SHEREE WEN, WEN Technology and WENLAB USA 

ROBERT M. WHITE, Carnegie Mellon University (emeritus) 

Staff 

JAMES P. McGEE, Director 

ARUL MOZHI, Senior Program Officer 

CY BUTNER, Senior Program Officer 

LIZA HAMILTON, Administrative Coordinator 

JONATHAN ELLSAESSER, Senior Project Assistant 

iv 
Acknowledgment of Reviewers 

This report has been reviewed in draft form by individuals chosen for their 

diverse perspectives and technical expertise, in accordance with procedures approved by 

the National Research Council’s Report Review Committee. The purpose of this 

independent review is to provide candid and critical comments that will assist the 

institution in making its published report as sound as possible and to ensure that the 

report meets institutional standards for objectivity, evidence, and responsiveness to the 

study charge. The review comments and draft manuscript remain confidential to protect 

the integrity of the deliberative process. We wish to thank the following individuals for 

their review of this report: 

Katherine Faber, Northwestern University, 

Katharine Frase, IBM Corporation, 

Frank E. Karasz, University of Massachusetts, and 

David C. Larbalestier, Florida State University. 

Although the reviewers listed above have provided many constructive comments 

and suggestions, they were not asked to endorse the conclusions or recommendations, nor 

did they see the final draft of the report before its release. The review of this report was 

overseen by Alton Slay, Warrenton, Virginia. Appointed by the National Research 

Council, he was responsible for making certain that an independent examination of this 

report was carried out in accordance with institutional procedures and that all review 

comments were carefully considered. Responsibility for the final content of this report 

rests entirely with the authoring panel and the institution. 

v 

Contents 

SUMMARY 1 

THE CHARGE TO THE PANEL AND THE ASSESSMENT PROCESS 3 

CERAMICS DIVISION 5 

MATERIALS RELIABILITY DIVISION 10 

METALLURGY DIVISION 15 

POLYMERS DIVISION 19 

PROGRAMS FUNDED UNDER THE AMERICA COMPETES ACT 23 

OVERALL CONCLUSIONS 27

vii 

Summary 

The Materials Science and Engineering Laboratory (MSEL) of the National Institute of 

Standards and Technology (NIST) works with industry, standards bodies, universities, and other 

government laboratories to improve the nation’s measurements and standards infrastructure for 

materials. Its work is aligned with the mission of NIST, which is to promote U.S. innovation and 

industrial competitiveness by advancing measurement science, standards, and technology in 

ways that enhance economic security and improve our quality of life. 

The MSEL consists of 149 technical staff, including 5 NIST Fellows, and 184 guest 

researchers, with total funding of $44.8 million at the time of this review. The MSEL is 

organized in four divisions: Ceramics, Materials Reliability, Metallurgy, and Polymers. A panel 

of experts appointed by the National Research Council (NRC) assessed the four divisions. Panel 

members visited these divisions and reviewed their activities. 

As requested by the Director of NIST, the scope of the assessment included the following 

criteria: (1) the technical merit of the current laboratory programs relative to the current state of 

the art worldwide; (2) the adequacy of the laboratory facilities, equipment, and human resources, 

as they affect the quality of the laboratory technical programs; and (3) the degree to which the 

laboratory programs in measurement science and standards achieve their stated objectives and 

desired impact. In addition to these three criteria, the panel was asked by the Director of NIST to 

assess the projects within the laboratory conducted under the America COMPETES Act of 2007, 

which supports the President’s American Competitiveness Initiative (ACI).1

On the basis of its assessment of the MSEL conducted in March 2008, the NRC’s Panel 

on Materials Science and Engineering concluded that, for the selected portion of the MSEL 

programs reviewed, the staff, the projects, and many facilities are outstanding. The projects are 

clearly focused on the mission of MSEL. The facilities and equipment are rationally upgraded 

within budget constraints, with several facilities being unique; the funding provided through the 

America COMPETES Act of 2007 is being used effectively. Division chiefs and staff evinced 

high morale, attributable to several factors: clear definitions of expectations and of the processes 

for realizing them, strong support of the MSEL from NIST leadership and of NIST generally 

from the President and from the Congress (through the American Competitiveness Initiative and 

the America COMPETES Act), and positive feedback from customers. 

Since the previous NRC assessment of the laboratory,2

 the MSEL has won internal NIST 

competitions to fund promising projects, terminated projects of relatively low impact, hired a 

few new staff and some postdoctoral temporary staff through the highly competitive NRCadministered National Academies Research Associateship Program, and upgraded experimental 

capabilities. The result is an organization that is strong in staff, facilities, and focus. 

The relatively new MSEL program planning and evaluation process provides a 

framework for the MSEL to assess ongoing and new projects with regard to risk and impact. 

The inclusion of an assessment of risk and steps to mitigate it, along with a process to 

“authenticate” the need—that is, to identify and verify the need of customers—is noteworthy. 

 1

 See Domestic Policy Council, Office of Science and Technology Policy, 2006, American Competitiveness 

Initiative, Washington, D.C. “America COMPETES Act” is the short title for the America Creating Opportunities to 

Meaningfully Promote Excellence in Technology, Education, and Science Act of 2007 (Public Law 110-69). 2

 National Research Council, 2005, An Assessment of the National Institute of Standards and Technology 

Measurement and Standards Laboratories: Fiscal Years 2004-2005, Washington, D.C.: The National Academies 

Press. 

1 
The MSEL technical staff is strong and productive as measured by publication in refereed 

journals, output of products (such as standard reference materials [SRMs] and standard reference 

databases [SRDs]), awards, and strong demand by customers (U.S. industry) for advanced 

measurement services and standards. Staff and managers participate in and are elected by their 

peers to lead major technical societies, which validates the quality of the staff and enhances the 

reputation and stature of NIST. 

Funding for various programs under the America COMPETES Act started in fiscal year 

(FY) 2007, so it is early to assess its impact. The projects receiving this funding are well 

conceived, and the first results are positive. The Ceramics Division, which is responsible for 

enhancing the NIST capability in the National Synchrotron Light Source (NSLS) at the 

Brookhaven National Laboratory, is effectively applying the funding to perform unique 

measurements that have already resulted in new discoveries. The enhanced research capability is 

significant enough that it should be managed in a way that brings broader participation from 

NIST in establishing priorities for the portion of beam time that NIST controls. The Metallurgy 

and the Materials Reliability Divisions share in executing a program to develop standards and 

test protocols related to the hydrogen economy—specifically, to the safety of pipelines to 

transport hydrogen under high pressure. A flexible research and test facility is under 

construction at the NIST facility in Boulder, Colorado, that holds promise of greatly enhancing 

the capability of NIST to study this complex problem. A related project to measure hydrogen 

content rapidly in order to assess materials compatibility is solid but small. The project to build 

the first broadband coherent anti-Stokes Raman scattering microscope is off to a good start in the 

Polymers Division. 

Issues and opportunities for improvement are cited in the division chapters. Issues that 

are common to varying degrees among the divisions include the following: a large fraction of the 

staff is retirement-eligible, and limited hiring resulting from constrained budgets may threaten 

capabilities; some equipment is antiquated and some facilities are in need of upgrade, notably in 

Boulder. Several projects beneficially incorporated modeling and simulation, but more is 

needed. 

In future NRC panel assessments, project presentations should briefly include the size, 

start date, and expected duration of a project as well as indicating linkages to other projects, if 

applicable, as an adjunct to the statement of partnerships and other evidence of authentication 

that was frequently provided. Providing data that compare MSEL capabilities with those of 

other laboratories would be helpful as well. Trend data for 5 years would help the panel in 

evaluating progress in projects and assessing the strength of programs. 

2 
The Charge to the Panel and the Assessment Process 

At the request of the National Institute of Standards and Technology, the National 

Academies, through its National Research Council, has since 1959 annually assembled panels of 

experts from academia, industry, medicine, and other scientific and engineering environments to 

assess the quality and effectiveness of the NIST measurements and standards laboratories, of 

which there are now nine,3 as well as the adequacy of the laboratories’ resources. In 2008, NIST 

requested that five of its laboratories be assessed: the Building and Fire Research Laboratory, the 

Manufacturing Engineering Laboratory, the Materials Science and Engineering Laboratory, the 

NIST Center for Neutron Research, and the Physics Laboratory. Each of these was assessed by a 

separate panel of experts; the findings of the respective panels are summarized in separate 

reports. This report summarizes the findings of the Panel on Materials Science and Engineering. 

For the FY 2008 assessment, NIST requested that the panel consider the following 

criteria as part of its assessment: 

1. The technical merit of the current laboratory programs relative to the current state of 

 the art worldwide; 

2. The adequacy of the laboratory facilities, equipment, and human resources, as they 

 affect the quality of the laboratory technical programs; and 

3. The degree to which the laboratory programs in measurement science and standards 

 achieve their stated objectives and desired impact. 

In addition, because NIST has begun to receive increases in funding through the 

President’s ACI and the America COMPETES Act of 2007, the Director of NIST also requested 

that the assessment panels specifically examine and review the progress of all of the FY 2007-

funded initiatives relevant to their respective laboratories and comment on these program growth 

areas explicitly in their reports. 

The context of this technical assessment is the mission of NIST, which is to promote U.S. 

innovation and industrial competitiveness by advancing measurement science, standards, and 

technology in ways that enhance economic security and improve the quality of life. The NIST 

laboratories conduct research to anticipate future metrology and standards needs, to enable new 

scientific and technological advances, and to improve and refine existing measurement methods 

and services. 

To accomplish the assessment, the NRC appointed a panel of 20 volunteers whose 

expertise matched that of the work performed by the MSEL staff. Each panel member was also 

assigned to one of four review teams whose members’ expertise matched that of the work 

performed by the staff in the four MSEL divisions being assessed: Ceramics, Materials 

Reliability, Metallurgy, and Polymers.4 

The Materials Reliability Division review team held a 1-day meeting at the Materials 

Reliability Division facility in Boulder, Colorado, on March 13, 2008. The other three review 

teams individually visited their respective MSEL divisions at the NIST facilities in Gaithersburg, 

 3

The nine NIST laboratories are the Building and Fire Research Laboratory, the Center for Nanoscale 

Science and Technology, the Chemical Science and Technology Laboratory, the Electronics and Electrical 

Engineering Laboratory, the Information Technology Laboratory, the Manufacturing Engineering Laboratory, the 

Materials Science and Engineering Laboratory, the NIST Center for Neutron Research, and the Physics Laboratory. 4

 See http://www.msel.nist.gov/ for more information on MSEL programs. Accessed August 12, 2008. 

3 
Maryland, on March 19, 2008. During their 1-day meetings they attended presentations, tours, 

demonstrations, and interactive sessions with the MSEL staff. Immediately following the 

division review team meetings, the entire panel assembled for a day-and-a-half meeting at the 

NIST facilities in Gaithersburg on March 20-21, 2008. During that time the panel attended 

interactive sessions with the laboratory managers, and also met in a closed session to deliberate 

its findings and to define the contents of this assessment report. 

The panel’s approach to the assessment relied on the experience, technical knowledge, 

and expertise of its members, whose backgrounds were carefully matched to the technical areas 

within which the MSEL activities are conducted. The panel reviewed selected examples of the 

standards and measurements activities and the technological research presented by the MSEL. It 

was not possible to review the MSEL programs and projects exhaustively. The examples 

reviewed by the panel were selected by the MSEL. The panel’s goal was to identify and report 

salient examples of accomplishments and opportunities for further improvement with respect to 

the following: the technical merit of the MSEL work, its impact with respect to achieving its own 

definition of its objectives, and specific elements of the MSEL’s resource infrastructure that are 

intended to support the technical work. These highlighted examples for each MSEL division are 

intended collectively to portray an overall impression of the laboratory, while preserving useful 

suggestions specific to projects and programs that the panel considered to be of special note 

within the set of those examined. The assessment is currently scheduled to be repeated 

biennially. While the panel applied a largely qualitative rather than a quantitative approach to 

the assessment, it is possible that future assessments will be informed by further consideration of 

various analytical methods that can be applied. 

The comments in this report are not intended to address each program within the MSEL 

exhaustively. Instead, this report identifies key issues and focuses on representative programs 

and projects relevant to those issues. Given the necessarily nonexhaustive nature of the review 

process, the omission of any particular MSEL program or project should not be interpreted as a 

negative reflection on the omitted program or project. 

The report’s Summary first highlighted issues that apply broadly to several or all of the 

divisions or to the laboratory as a whole. Then, after this chapter on the charge to and approach 

taken by the panel, individual chapters present observations specific to the respective laboratory 

divisions. Comments on the progress of the programs funded under the America COMPETES 

Act are followed by overall conclusions. 

4 
Ceramics Division 

SUMMARY 

The Ceramics Division has programs that are well defined and focused on its mission; it 

has developed several state-of-the-art facilities, some of which are unique; it has a fine, 

productive staff; and it has an enthusiastic and effective leadership team that vigorously 

evaluates the technical performance of the staff. The MSEL-wide project evaluation process, 

while burdensome in its early implementation, has been effectively employed by the Ceramics 

Division to redefine its project portfolio. The division’s aggregated research capabilities support 

materials characterization, particularly in x-ray metrology and synchrotron-based methods, and 

those located in the state-of-the-art Advanced Measurements Laboratory (AML) that are among 

the best. Proactive performance evaluation has addressed personnel issues to enhance the 

capability of the Ceramics Division. The staff is very productive, as measured by publications in 

refereed journals and the delivery of many standard reference materials and phase-equilibrium 

diagrams. The programs integrate theory and modeling with experimental studies, where 

feasible, to create a balanced portfolio. 

The funds appropriated under the America COMPETES Act of 2007 have been 

effectively used to enhance the capability of the three NIST beam lines in the National 

Synchrotron Light Source, a U.S. Department of Energy (DOE) national user facility, at the 

Brookhaven National Laboratory in New York. Noteworthy accomplishments include fielding 

the most advanced synchrotron detectors and performing, for the first time, interfacial structure 

measurements on commercially important high-dielectric-constant gate oxides. Several 

industrial partners are involved in the research. 

The division has made good use of the exceptional capabilities in the AML, where it has 

11 modules comprising two laboratories focused on nanomechanics (using atomic force 

microscopy [AFM], scanning tunneling microscopy [STM], and nanoindentation) and x-ray 

metrology, using a custom-built parallel beam diffractometer. Both require exceptional stability 

of the measurement environment. 

Other noteworthy accomplishments include the first combinatorial measurements of 

metal high-dielectric-constant oxide structures and the release of the first nanoparticle reference 

materials. There are also important, ongoing projects to provide a spectrum of standard 

reference materials, standard test methods, and standard reference databases. These projects may 

not appear in refereed publications, but they do appear in thousands of laboratories worldwide as 

essential elements of research and production activities. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

The staff of the Ceramics Division are experienced, knowledgeable, and recognized as 

leading authorities in their respective fields. Evidence of the quality of the research being 

designed, organized, and conducted by the staff in the division includes the large number (185) 

of peer-reviewed publications in the past 18 months; collaborative relationships, both long and 

short term, with outside organizations such as the American Ceramic Society, other government 

agencies, and the National Cancer Institute (NCI); and national and international awards (e.g., 

election as fellows in technical societies and members of the National Academy of Engineering) 

received by staff members for their outstanding research accomplishments. 

5 
The division is engaged in a wide range of important research topics, including the 

analysis, compilation, and dissemination of crystallographic and phase-equilibrium databases 

that serve thousands of materials engineers and scientists throughout the world. These topics 

also include modern and timely research fields such as nanodevices for measurement and 

standards, nanoparticles for medical applications, and synchrotrons for measuring the nanoscale 

structure of solids. The fact that all three NIST synchrotron beam lines are being used to 

capacity is strong evidence of the usefulness, capability, and demand for these state-of-the-art 

facilities. 

No major weaknesses were detected in the overall research program. The division staff is 

effectively evaluating the research projects on a timely basis and eliminating struggling projects 

in favor of projects in areas where future growth is more likely to occur. 

ADEQUACY OF INFRASTRUCTURE 

The FY 2008 technical portfolio of the Ceramics Division totals $13,030,000, with 

$830,000 supporting NIST Fellows’ projects. Technical work is grouped in four topical areas: 

nanomechanical properties, structure determination methods, functional properties, and 

synchrotron methods. 

The capabilities of the Ceramics Division to characterize materials by x-ray and 

synchrotron radiation, scanning probe microscopy, and other analytical techniques are, in 

aggregate, state of the art, and in several cases they are unique. Eleven laboratory modules in the 

AML—a state-of-the-art facility with Class 10,000 to Class 100 air quality, temperature control 

ranging from 0.25 o

C down to 0.01 oC, and exceptional vibration control—provide x-ray 

metrology and nanomechanics laboratories and facilities needed to prepare standards required by 

U.S. industry to develop materials and devices based on nanotechnology. The capabilities on the 

beam lines in the NSLS at the Brookhaven National Laboratory incorporate unique equipment 

designed by NIST to provide measurement capabilities used by NIST scientists as well as many 

industrial and university-based collaborators. These noteworthy measurement capabilities have 

been directly applied to fulfilling the mission of the Ceramics Division to develop analytical 

techniques and SRMs. 

The division has worked effectively within its budget to develop its experimental 

capabilities, but some of the equipment (e.g., furnaces and x-ray diffraction equipment used in 

phase-diagram studies) has exceeded what would generally be considered its useful life. 

The division has an effective approach to assessing its staff and taking appropriate 

actions to address performance issues. The staff who presented their work to the panel were 

enthusiastic and articulate in describing their generally outstanding work. The Ceramics 

Division should increase efforts to compete more effectively for NRC postdoctoral students, both 

for the immediate capability that they bring and for their potential as future permanent staff. 

The productivity of the staff is outstanding, as measured by publications in refereed 

journals with high Institute for Scientific Information impact factor ratings. Moreover, the 

demand for the SRMs supplied by the division, including new reference materials developed for 

the emerging nanotechnology field—such as for gold nanoparticles—is evidence of the impact of 

the staff’s productivity. Recognition in the form of an invited paper in Science5

 and the 2006 

 5

 S.J.L. Billinge and I. Levin, 2007, “The Problem with Determining Atomic Structure at the Nanoscale,” 

Science, Vol. 316 (April 27): pp. 561-565. 

6 
Outstanding Paper Award in Measurement Science and Technology6

 is noteworthy. The 

refereed publications were appropriately supplemented by practice guides, such as Fractography 

of Ceramics and Glasses.

7

ACHIEVEMENT OF OBJECTIVES AND IMPACT 

The Ceramics Division is meeting the NIST mission, vision, core competencies, and 

many of its core values. The division has suffered from limited hiring. It needs to compete more 

effectively for postdoctoral students in the NRC-administered National Academies Research 

Associateship Program. Measurement science, rigorous traceability, and the development and 

use of standards are, taken together, a core competence of the Ceramics Division. The division 

demonstrates customer focus to promote U.S. innovation and industrial competitiveness. 

Nanomechanical Properties Group 

The Nanomechanical Properties Group conducts five projects, all initiated between 2006 

and 2008. Two of these make effective use of NIST’s comprehensive collection of state-of-theart atomic-resolution testing capabilities in the AML: two scanning probe microscopes with 

capabilities including STM and AFM, two instrumented indenters with unprecedentedly small 

noise and thermal drift, and an optical interferometer with 1-nanometer-depth resolution. 

One of the AML-related projects has resulted in a highly precise prototype 

microfabricated cantilever beam array for calibrating commercial atomic force microscopes. 

This array has been employed by five vendors of atomic force microscopes and by users of these 

microscopes in industry, academia, and government. The other AML-related project has focused 

on nanoindentation for measurements of fracture and viscoelastic properties of materials and 

structures—including fracture toughness measurement in thin, amorphous films. 

A large component of one exciting project, focused on nanoscale-particle property 

measurements and standards, was initiated at the request of the National Cancer Institute in 2006. 

The NCI is engaged in an initiative to make use of the special properties of nanoscale particles to 

radically change the way that cancer is diagnosed, treated, and prevented. The NIST 

contribution, which makes very effective use of NIST core measurement competence, involves 

the development of measurements and standards for the physical characterization (with respect to 

size, surface area, charge, agglomeration, stability, and purity) of nanoscale particles of interest 

to the NCI program. The Ceramics Division-led NIST team has so far completed the first 

reference materials for biomedical applications, released in January 2008. These reference 

materials are for particles of 10, 30, and 60 nanometer diameter. Computational approaches are 

also under development in the Ceramics Division for specific particle properties. 

Two very recently initiated projects—Mechanical Reliability Measurements for 

Microelectromechanical Systems (MEMS) and Piezospectroscopy Measurements and 

Standards—appear to be well planned and oriented toward important applications. The former 

employs the design of a macroscale test structure in a novel manner for microscale structures, 

and the latter addresses nanoscale stress mapping with a NIST-built Raman optical probe. 

 6

 R.S. Gates and J.R. Pratt, 2007, “Prototype Cantilevers for SI-Traceable Nanonewton Force Calibration,” 

Measurement Science and Technology, Vol. 17, no. 10, pp. 2852-2860. 7

 National Institute of Standards and Technology, 2007, NIST Recommended Practice Guide: Fractography 

of Ceramics and Glasses, Gaithersburg, Maryland.

7 
Structure Determination Methods Group 

The portfolio of the Structure Determination Methods Group contains a balanced set of 

projects that were initiated during three separate decades. The database work is among the best, 

and the diffraction metrology work and standards work are excellent. 

The group’s mission is focused on SRMs, SRDs, computational tools, and x-ray, 

electron, and neutron diffraction. Core competencies lie in x-ray metrology; x-ray, electron, and 

neutron-based structure measurements; structure determination computational tools; and phaseequilibrium and crystallography determination. Customer engagement is strong, as demonstrated 

by SRM distribution through vendors with instrumentation packages, SRD licensing and 

distribution agreements, workshops, and the collaborative partnership with the American 

Ceramic Society on phase-equilibrium diagrams. 

The community demands that NIST continually improve SRMs; some 700 are sold each 

year. NIST certified the amorphous fraction of a 50:50 mixture of silicon and SRM 676a 

(alumina powder) to an accuracy that is considered to be the best; this is a noteworthy 

accomplishment. X-ray reflectometry can be used to measure the thickness and interfacial 

roughness of thin films repeatably. Many semiconductor industry partners demand this degree of 

measurement. The new work on measuring local structure is an excellent new start, and that 

work has been published in Science.

8

 The long-term work on ceramic phase-equilibrium data 

and crystallographic databases is among the best. 

Functional Properties Group 

The focus of the Functional Properties Group is measurement science, standards, and 

technology pertaining to the functional properties of advanced materials and devices, including 

ceramics and nanomaterials. The Functional Properties Group is a leader in three areas: 

combinatorial measurement methods, nanocalorimetry measurements, and thermoelectric 

measurements and standards. Of the three projects in these areas, one is almost mature—

Combinatorial Measurement Methods for Advanced Complementary Metal Oxide 

Semiconductor (CMOS) Devices, a project that started in 2004. 

There are only two or three combinatorial thin-film synthesis laboratory facilities in the 

United States and a similar number in Japan. The NIST facilities are among the best of these and 

will be further enhanced by an atomic-layer deposition tool destined for the Nanofabrication 

Facility (located in the AML). For example, the material currently used for the CMOS is 

reaching its fundamental materials limit, and thus new materials are required by the $750 billion 

semiconductor industry. Semiconductor customers (Semiconductor Manufacturing Technology 

Consortium [SEMATECH], Intel Corporation, Micron Technology, Qualcomm, NIMS Japan, 

and IMEC, Belgium) are partnering with NIST to address this matter. 

Beyond the qualification of partners, the impact of the projects is measured by public 

recognition (Science Watch), invited NIST presentations, awards, effective partnership with 

users, SRM sales, database royalties, customer surveys, technology transfer to users, and patents 

(to a lesser degree). Regularly scheduled internal and external assessments of the Ceramics 

Division project portfolio by independent evaluators and customers or potential customers 

identified in the MSEL project management process are critical to authenticating projects’ 

 8

 S.J.L. Billinge and I. Levin, 2007, “The Problem with Determining Atomic Structure at the Nanoscale,” 

Science, Vol. 316 (April 27): pp. 561-565.

8 
impact. An excellent opportunity exists for the Functional Properties Group to develop novel, 

combinatorial-compatible measurement methods. This quality work should be continued in 

order to help address these types of materials issues within the semiconductor industry. 

Synchrotron Methods Group 

Three mature projects that began in 1993 are found in the Synchrotron Methods Group, 

and the impact from this effort is expected to continue to increase when new facilities are 

constructed within the next several years. Support for synchrotron-related work was enhanced 

by funding through the America COMPETES Act, as discussed in the chapter on this funding. 

CONCLUSIONS 

The Ceramics Division is conducting high-quality research on a broad range of topics 

that strongly support the mission and core interests of the MSEL and NIST. The staff is using 

the financial resources and equipment at its disposal in an efficient manner. The research is 

widely recognized as being of high quality and in many instances is judged to be among the best. 

9 
Materials Reliability Division 

SUMMARY 

The theme of the Materials Reliability Division, located in Boulder, Colorado, is the 

reliability of structures—from bridges to single cells. The organization of the division lines up 

well with its work and helps focus on the emerging areas of nanoscale reliability and cell and 

tissue mechanics. The division has effectively built on its core competency of mechanical 

property measurements and extended the applications to small sizes (nano) and biological areas. 

The projects are clearly focused on the mission of the MSEL, and the division has engaged its 

NIST colleagues in Gaithersburg, Maryland, in several projects. 

The quality of the technical staff is generally excellent, and the division’s laboratories are 

well equipped, with a few exceptions. The division programs should add enhanced modeling 

and theory expertise. The recent transfer of staff to augment the theoretical and modeling 

capability is good. Reliability testing is only part, albeit an essential part, of the science and 

application of reliability engineering needed by U.S. industry. The division has made excellent 

progress in recruiting staff by transferring two individuals from Gaithersburg, but there remains 

an imbalance between experimental expertise and the modeling commonly used in industry. A 

more visible program of three-dimensional finite-element modeling of thermal and electrical 

stresses is desirable. The division should increase its efforts to access expertise in other divisions 

at NIST and/or to add staff. 

In general, the physical infrastructure facilities of the Materials Reliability Division are 

dated, but overall the laboratories are well equipped. The ratio of technician support to 

professional support seems to be very low for laboratories of this caliber and size (a situation not 

unique at NIST to this division). 

The productivity, as measured by publications and products, for example, Charpy test 

specimens, is very good. Staff members have won awards, and an appropriate number of 

meetings were hosted. The division is a good example of executing the MSEL project evaluation 

process to focus its effort on projects that fulfill the mission of the MSEL. 

The division has done a good job of developing new and important areas of research 

beyond its traditional focus. It has reached out to establish a customer base in areas such as 

biomaterials and has worked to reinvigorate its traditional core competency in large-structure 

reliability programs. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

The technical merit of the work in the Materials Reliability Division is high, whether in 

the historic role of supplying Charpy test specimens or at the new frontier of exploring the 

application of stress measurements to biological systems. The ability to address a diversity of 

projects attests to the quality of the staff and the management of the division. Generally, the 

staff has augmented its capability by forming partnerships in the areas in which it needs help. 

The area of medical device reliability would benefit from added expertise in reliability analysis. 

In general, the technical work reviewed was excellent and in some cases unique. Theory and 

modeling could enrich the experimental program. Steps have been taken to augment the staff; 

continued additions are warranted. 

10 
ADEQUACY OF INFRASTRUCTURE 

The equipment associated with the structural materials projects of the division is often 

old, but it has been updated with modern electronics. The basic test equipment has some unique 

capabilities that were designed and constructed by NIST staff—for example, very low 

temperature test cells. A hydrogen test facility under construction, while not reviewed in detail, 

appears to be very versatile and will be a significant contribution to the work relating to the 

technologies targeted by the ACI and the America COMPETES Act (see the chapter below on 

this funding). The Nanoscale Reliability Group has constructed a unique atomic force 

microscope for the measurement of mechanical properties at the nanoscale and has established 

good teaming with industry and universities. 

ACHIEVEMENT OF OBJECTIVES AND IMPACT 

The technical work of the division is grouped in three topical areas: structural materials, 

cell and tissue mechanics, and nanoscale reliability, as discussed below. 

Structural Materials Group 

The Structural Materials Group has core competencies in mechanical testing on a 

macroscale and in developing standard measurement techniques for materials and properties that 

are critical to the nation’s infrastructure. This group manages the Charpy Standard Reference 

Material and Verification Program, which sells several thousand units a year. All of the 

structural materials work is clearly focused, and the payoffs from success are clear. Good 

customer ties were shown—for example, in joint planning with DOE and the U.S. Department of 

Transportation (DOT) on hydrogen and on pipeline safety. The mature (historic) Charpy Test 

Sample Program has an element of science in computational models and crack tip measurements. 

The impact of the work is high and clear for the specific projects and more generally as it relates 

to understanding the failure of large, complex structures. It is a vital role for NIST to play.

This group maintains equipment capable of tensile, fatigue, and fracture impact analysis 

and crack tip opening analysis (CTOA) in the range of 1 N to 4.4 MN over a temperature range 

of liquid helium to 1000 o

C. The equipment has been installed in the laboratory for an extended 

period of time, in some cases having been in service since the 1960s, although periodic 

electronic and other upgrades have kept most of the equipment in state-of-the-art condition. 

Some areas, such as nondestructive evaluation, have been diminished through attrition of staff. 

However, this laboratory and its personnel remain fully capable as a valuable, unbiased resource 

for responding to critical national infrastructure testing needs, such as the investigation of the 

collapse of the World Trade Center’s Twin Towers and now the hydrogen pipeline safety effort 

as one of the ACI-related programs. 

The Pipeline Safety project is a basic data-gathering and measurement activity that has as 

a clear customer the pipeline industry. It is an indispensable standards activity. A strength of the 

activity is the continued development of the fracture toughness test, based on the optical 

measurement of the crack tip angle, as a measurement tool for evaluating pipeline safety. This 

laboratory operates with a relatively small permanent staff, but it has done a good job of using 

postdoctoral, cooperative, and other guest researchers to supplement labor needs. In addition, 

the laboratory is highly collaborative in much of its work, leveraging its mechanical testing 

11 
expertise with others laboratories in the MSEL and other agencies, such as DOT, for funding. 

There is a need for extending the strain-rate capabilities for the high-speed fracture mechanics 

testing of pipelines to remain competitive. Data from these tests are essential for those who 

accurately model pipeline rupture under burst conditions. 

Supplying Charpy test SRM samples is a large and important component of the work of 

the Structural Materials Group. This group has established itself as providing SRMs for Charpy 

testing to meet the ASTM (formerly known as the American Society for Testing and Materials) 

standards. This is the most successful SRM program at the MSEL. The Structural Materials 

Group supported the revision of two International Organization for Standardization (ISO) 

standards in FY 2007. 

Cell and Tissue Mechanics Group 

One of the reasons why NIST has a history of success is that it has maintained a research 

program at the leading edge of developing fields where measurement methods and, eventually, 

standards will be central. In the rapidly developing field of tissue and cell engineering, NIST has 

a vital role in indentifying the crucial parameters that will need to be measured. 

The Bioreactors project has established a strong and promising collaboration with a 

University of Colorado research group for investigating the effect of different types of forces on 

the histology, growth morphologies, and various tissue expressions under realistic in vitro tissue 

growth environments. The research being performed is elegant, conceptually simple, and likely 

to provide important insights into tissue growth under conditions pertinent to actual body strains. 

This is excellent basic research, although it is premature to judge whether it will also lead to a set 

of instruments that can measure tissue response characteristics that will be of essential value to 

the burgeoning field of tissue culture for biomedical replacements. Bringing in a biomedical 

industry partner could add value. 

The Single Cell Mechanics BioMEMS project is one among the worldwide activities 

working to establish methods for the in vitro measurement of cell deformation and mechanics. 

Many of these activities are focused on using the mechanical response of cells as a tool for 

assessing disease progression and the viability of cells. The more sophisticated projects are 

those that combine the two- and three-dimensional response of cells to deformation with 

complementary mechanics-based models of the deformation to elucidate the deformation 

mechanisms. The current force-displacement measurements at the Materials Reliability Division 

using a uniaxial straining MEMS device designed and fabricated at NIST facilities is a promising 

approach. The reliability is limited by the lack of strain measurements in other directions as well 

as by any mechanics modeling to relate the measurements to the underlying histological structure 

of the cells. Complementary efforts and tools reside in the Ceramics Division. The Materials 

Reliability Division should expand interdivisional collaborations. 

The single-cell tester used in this research was conceived by NIST and was fabricated by 

the NIST in-house MEMS facilities. The first of its kind, this tester has the potential to play a 

key role in increasing the understanding of tissue formation, disease progression, and disease 

treatment and may impact drug discovery. 

Medical Device Reliability is one of the projects in the biomaterials area. Medical 

applications represent a significant sector of the U.S. health industry. Current unacceptably high 

failure rates of implantable medical devices such as pacemakers, cardiac defibrillators, and 

neural transmitters point to the urgent need to establish standards and to develop measurement 

12 
methods to ensure quality, reliability, and consistency and so to minimize the need for repetitive 

procedures to remove recalled devices from the human body. 

NIST is working with the International Electronics Manufacturing Initiative Medical 

Electronics team to address short- and long-term reliability issues with medical devices. The 

division has established programs to develop new measuring tools, explore methods to improve 

reliabilities, and develop accelerated testing standards. Teamed with companies and with the 

National Institutes of Health (NIH), the Cell and Tissue Mechanics Group has gathered critical 

data on the next generation of devices and identified key exposures of failure mechanisms. The 

target of this work is to reduce the failure rate to less than 0.1 percent (current levels are an 

order-of-magnitude higher). Although the group has organized workshops with important 

industry players, the division researchers would benefit from collaborating more directly with 

experts who can help establish more direct links between the current technical characteristics of 

devices and their reliability and performance. The division should apply a more focused and 

specific plan to address reliability issues and to include experts well versed in reliability. 

The Cell and Tissue Mechanics Group has noted that parylene (coatings used in 

implanted probes) degrades in the presence of electrical fields and has communicated this 

important observation to the Food and Drug Administration. 

Overall the Cell and Tissue Mechanics Group has excellent staff who are employing 

innovative approaches. 

Nanoscale Reliability Group 

Strain engineering is an important new area of semiconductor technology. As devices 

have scaled down from micrometers (1,000 nm) to 45 nm today and 20 nm in the next few years, 

perfectly induced localized strains in device structures can enhance electron and hole mobility by 

more than 30 percent, leading to faster devices. Strain metrology, therefore, is indispensable for 

the U.S. semiconductor industry.9

The metrology of strains at the nanoscale is extraordinarily difficult, and no group has yet 

measured strains in microprocessors. The Nanoscale Reliability Group has developed its 

techniques using geometrically simpler structures (doped nanowires) where measurement of the 

stress state is less complex. 

The group used transmission electron microscopy (TEM) and scanning electron 

microscopy (SEM) together with commercially available software tools to acquire diffraction 

data and lattice images with high spatial resolution (10 nm for diffraction, 0.2 nm for imaging), 

and then measured the changes in lattice parameters across nanowires. These data were used to 

produce two-dimensional strain maps in gallium nitride/indium gallium nitride (GaN/InGaN) 

nanowires. A goal of the work is to develop three-dimensional strain mapping, which would be 

a significant advance. A challenge using this approach is to interpolate the results of these 

measurements to actual devices. 

One of the successes of the Nanoscale Reliability Group has been the use of atomic force 

microscopy to study localized strain on the nanoscale. The quality of the research is comparable 

with that of leading groups in this area, and the contributions in the area of contact resonance 

AFM imaging are at the forefront of such work. Complementary work using tip enhanced 

Raman spectroscopy provides a suite of capabilities for developing metrology at the nanoscale. 

 9

 A. Diebold et al., 2008, “Update Presentation on Metrology Roadmap,” International Technology 

Roadmap for Semiconductors, Spring 2008, U.S. Metrology Technical Working Group. 

13 
There is considerable overlap with research on nanomechanics at the NIST Gaithersburg site. 

The establishment of Communication Working Groups within the MSEL is a good step toward 

strengthening the collaborations between the different AFM groups. 

Another of the strengths of the Nanoscale Reliability Group has been the evaluation of 

material properties at small length scales. This is a crucial technical and intellectual endeavor 

because many of the mechanical properties of metals and polymers are different at small lengths. 

For example, there is the well-known indentation size effect, wherein the hardness of many 

metals and polymers increases as the indentation load, and hence the size of the hardness 

impression, is decreased. The question arises as to whether other related mechanical properties 

of concern to the microelectronics industry, such as fatigue strength, are also different at small 

length scales and, if so, why. Few groups other than the NIST group at Boulder are tackling 

these important questions. One of the difficulties is that it is necessary to do both the testing and 

the evaluation at the same dimensions. One approach, taken both at NIST and at the Max Planck 

Institute in Germany (by a NIST researcher working there), is to use cyclic Joule heating to 

differentially strain and hence fatigue the interconnect lines while monitoring their 

microstructural changes with complementary electrical measurements. This work has quantified 

the combined effect of mechanical constraint and dimensional scaling, which were shown to 

dramatically alter the fatigue failure resistance of aluminum lines. Although aluminum lines are 

increasingly being replaced in microelectronics by copper, it is expected that this measurement 

approach can be readily transferred to the investigation of the fatigue of copper interconnects in 

devices. 

The focus on nanoscale strain metrology is understandable, given the huge importance of 

the microelectronics industry. The group may also wish to consider the strain metrology 

associated with polymer electronics devices and displays. There are two distinct challenges. On 

the one hand, polymer-based electronics will be much larger than current silicon-based 

electronics, and so the strain metrology has to be performed over much larger dimensions 

without loss of precision. On the other hand, even though polymers generally exhibit larger 

compliances than those of metals and semiconductors, the strain incompatibilities with 

nonpolymeric components, such as interconnects and chips, are larger, and so the local strains 

that have to be quantified will be larger. In addition, the recent use of Green’s function 

calculations to perform lattice displacement mapping around a germanium (Ge) quantum dot in 

silicon (Si) provides an opportunity for the group to develop capability in finite-element 

modeling, plasticity theory, and mechanics analysis. An active recruiting program to add staff 

and backfill for anticipated retirements is desirable. 

CONCLUSIONS 

The projects reviewed are focused on the mission of the MSEL and build effectively on 

the historic strength of the Materials Reliability Division in mechanical testing for reliability. 

Augmenting the experimental capability with modeling and simulation expertise by the transfer 

of staff and hiring will greatly enhance the strength of the program. 

The division has developed several unique measurement tools and devices that have 

potential to strengthen the competitive position of U.S. industry. The recently enhanced focus at 

NIST on obtaining patents may be beneficial and should be used to explore the best approach for 

commercializing these developments. 

14 
Metallurgy Division

SUMMARY 

The panel reviewed 20 of the Metallurgy Division’s projects and engaged the division 

staff in discussions of the MSEL project evaluation process. Overall, the programs reviewed are 

well conceived and executed, responsive to NIST’s mission, and of high scientific and technical 

quality. The morale of the division is generally high, which may be the result of the division’s 

recently improved infrastructure and facilities, increased capital spending, stable core 

competencies, and positive outlook toward future opportunities. 

The division’s staff level has been steady from FY 2006 to FY 2008, a plateau after the 

preceding 10 years of decline. The division uses postdoctoral fellowships to recruit new hires. It 

should also consider initiatives that would attract more senior people. A related area of concern 

is a decline in knowledge and a rise in technology gaps resulting from the retirement of some 

senior staff. The division should develop a plan for knowledge capture and/or a succession plan 

either to mentor junior researchers or to hire senior researchers in critical technical areas. 

Many of the Metallurgy Division’s staff members are recognized both internally and 

externally, as is evident by the awards that they have received. The division has continued to 

maintain exemplary visibility through the organization of workshops at NIST, publications, and 

conference presentations. Overall, the staff has evinced a high level of commitment and 

dedication. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

The Metallurgy Division maintains a capable and engaged workforce devoted to 

achieving the goals of NIST. It is part of the NIST mission to increase innovation and industrial 

competitiveness by advancing measurement science, standards, and technologies in order to 

enhance economic security and improve the quality of life. The division maintains a diversity of 

activities including both fundamental sciences and applied studies in support of these goals. 

The technical merit of the Metallurgy Division is high relative to the state of the art. In 

general, the quality of the research is excellent. Some examples of outstanding research are 

provided below. 

Particularly noteworthy are efforts to standardize and improve hardness measurement, to 

develop atomistic modeling in support of the development of nN-level force standard for very 

small loads, to develop fundamentals-based quantitative models of microstructural evolution in 

materials for the extraction of kinetic data from experiments, and to develop a fundamental 

science-based understanding of the mechanisms leading to tin (Sn) whisker formation in 

electronic devices. Major accomplishments include the development of SRMs for hardness 

testing and a complete revision of the ASTM standards for hardness testing, which accomplish 

the goal of improving hardness as a measure of materials properties and quality control. The nNlevel force standard based on gold nanowires is cutting edge. NIST continues to lead the 

development of thermodynamic and kinetic databases, which will have broad applicability in all 

areas of materials engineering. Modeling efforts directed toward sustainable energy sources and 

hydrogen storage are timely and necessary. The formation of tin whiskers on lead-free surface 

finishes has evolved into a major reliability issue in microelectronics. Research at NIST has 

15 
revealed the mechanisms for whisker formation, which could lead to inhibiting it, thereby 

extending the service lifetimes of future components. 

The in situ, x-ray stress measurement capability for sheet metals undergoing deformation 

was exceptional. This type of measurement, which has never been done before in sheet metals, 

represents a breakthrough in deformation materials metrology. NIST should continue to develop 

this exciting technology so that it can be applied more broadly to solve practical engineering 

problems. 

ADEQUACY OF INFRASTRUCTURE 

The Materials Science and Engineering Laboratory’s commendable capital investment is 

welcomed by the division staff and will enhance the laboratory’s capabilities. The new tunneling 

characterization probe instrument adds to an already impressive magnetic thin-film fabrication 

and characterization capability. The strain measurement enhancement of the Kolsky bar 

technology will provide novel high-speed direct strain measurements, which are important and 

will be of interest to a broad range of researchers. The Lorenz microscope will provide state-ofthe-art imaging capability for the Magnetics Group. 

The division should assess its computing needs and develop a strategy for the future. The 

division’s staff appears innovative and willing to deal with difficult problems. One of these, as 

mentioned, is the decline in staff associated with staff members’ not being replaced upon 

retirement. An effort should be made to hire experienced individuals and not to rely entirely on 

NRC postdoctoral fellowships. 

The staff expressed some concerns that traditional measurement expertise may disappear 

with future retirements. Such expertise gaps should be identified and a strategy developed to 

maintain important core competencies. An effort should be made to capture this experience 

through mentoring. 

ACHIEVEMENT OF OBJECTIVES AND IMPACT 

The Metallurgy Division is doing well in terms of meeting its objectives of establishing 

standards and providing technology for supporting mainline U.S. industry (e.g., automotive, 

aerospace, and magnetics industries). However, it appears to have a gap in its ability to develop 

technologies that may be disruptive. The division should consider incentives for initiating 

projects that have high risk but also could have high payoff. There may be opportunities for it to 

accomplish this by working more closely with small and medium-sized businesses. An example 

would be in magnetics, where spin torque devices are a potential opportunity that should be 

explored, as well as magnetic sensors for biomedical applications. Small Business Innovation 

Research (SBIR) programs may be an important way to facilitate such efforts and should be fully 

explored. The current project selection process is a positive development, but it probably needs 

to be fine-tuned to ensure that high-risk, disruptive technologies are not filtered out. 

In general, the materials profession lags other fields (e.g., biology, astronomy, and others) 

in effective use of Web technology for knowledge dissemination and collaboration. The 

Metallurgy Division is highly proficient at disseminating knowledge through publications, 

presentations, and in particular at workshops such as the diffusion workshops. It has an excellent 

opportunity to leverage the division’s existing activities and to be a leader in the effective use of 

Web and information technology (cyber infrastructures) to disseminate information (databases 

16 
and models). The current Web-accessible databases for thermodynamics and diffusion are 

excellent leading-edge examples that could be expanded. There are currently only limited sets of 

thermodynamic data available; however, these could be easily expanded and serve as best 

practices by other groups within the MSEL and within other government-supported research 

laboratories. 

The Metallurgy Division has played an important technical role in a number of highvisibility failure analyses (e.g., analysis of the World Trade Center collapse, the sinking of the 

Titanic, and the failure of naval structures). The work on the Titanic has led to related studies of 

the Ellis Island Ferry and USS Arizona wrecks in efforts to establish the practicality of salvage 

and a timetable for preservation activities. Considering the vast number of aging wrecks 

populating the nation’s waterways, the technical merit of these activities relative to the state of 

the art is quite high. These examples could showcase for laypersons and national leaders the 

Metallurgy Division’s expertise and the national need for experts in metallurgy. However, the 

efforts referred to here largely involved full-scale structural analysis coupled with metallurgical 

insights and are not tied in with other computational efforts; this appears to be a missed 

opportunity. The impact of these efforts could be increased by identifying underlying themes of 

research and how they tie in with other division research areas. This would allow the Metallurgy 

Division to capitalize on the high visibility that such projects provide. 

The use of computational materials science tools to incorporate and disseminate 

information and knowledge is a growing trend within the materials profession. Strengthening 

this activity within the MSEL and making these models available to the broader research 

community offer important means of increasing the impact of the MSEL. 

There are good examples of cross-group and cross-division collaboration in the MSEL, 

and there is an excellent collegial atmosphere of cooperation. However, many of the division’s 

major research projects are disconnected. The Metallurgy Division could increase the impact of 

its research through better integration of its existing expertise into some cross-group projects that 

would demonstrate the impact of this combined expertise. An example might be an integration 

of efforts in thermodynamics, kinetics, and evolution of microstructure in Pb-free 

electrodeposits, with (currently nonexistent) efforts at using this information to predict the key 

properties of solders and, in turn, structural analysis of electrical interconnects. This would 

make use of all of the impressive expertise in thermodynamics, phase transformations, property 

development, and full-scale structural analysis. Other examples might be in the use of thermal 

barrier coatings for improving the performance of turbine blades for power generation or in the 

development of magnetic sensors. 

A high level of innovation was evinced within the Metallurgy Division. In particular: 

• The development of high-resolution three-dimensional chemical imaging 

(demonstrated in multilayer stacks) is highly innovative and the first known use of 

this technique on crystalline structure compensating for diffraction effects. This 

research has significant potential for development as a high-throughput evaluation 

tool for crystalline nanostructures. 

• The measurement of stress by means of multidirectional x-ray diffraction during 

sheet metal forming is a highly innovative first use of this technique. It provides a 

new approach for characterizing of the evolution of yield surfaces required for the 

simulation of sheet metal forming. 

17 
• The use of depth-resolved x-ray microbeam stress measurements to measure stresses 

within dislocation cells is a highly creative and unique research. 

CONCLUSIONS 

The Metallurgy Division represents a unique, high-quality research effort in the 

development of measurement science and materials standards in selected areas of critical 

importance for American competitiveness. The division could enhance its effectiveness by 

identifying common themes to better coordinate its activities and by increasing its focus on the 

entrepreneurial, highly innovative sectors of the U.S. economy. 

18 
Polymers Division 

SUMMARY 

The Polymers Division has done outstanding work with an energetic and highly 

motivated group focused on customers and collaborations to achieve its objective of providing 

critical measurement solutions with a high impact. In addition, the division has done 

exceptionally well in executing several projects in areas of critical importance to industry 

(electronic materials, biomaterials, and industrial polymers), homeland security (passport 

security with the U.S. Department of State and the U.S. Government Printing Office), the U.S. 

Department of Justice (body armor), consortia (SEMATECH, the Semiconductor Research 

Consortium, and others), and academia. The division has been very proactive in engaging 

faculty and graduate students in its research portfolio and in attracting them in large numbers 

through the NRC-NIST postdoctoral fellowships. This has proven to be a very effective 

recruiting mechanism. 

Energy is a significant contemporary problem; NIST in general and the Polymers 

Division in particular can make important contributions to the measurement science and 

technology related to organic photovoltaics (OPVs) and energy storage devices. Efforts in this 

area are slightly below an effective critical mass and should be increased if the Polymers 

Division is to have significant impact in this area. 

The presentations to the panel did not indicate how the recommendations of previous 

NRC panels have been addressed, and for many of the programs presented, a plan for the future 

was not clearly laid out. For example, it is not clear how the Matrix-Assisted Laser Desorption 

Ionization (MALDI) program has been reoriented to address the previous panel’s comment that 

“the work in the laboratory on mass spectrometry . . . (MALDI-mass spectrometry) of polymers 

has been very relevant. It is now time to consider whether the ‘low-hanging fruit has been 

picked.’ The laboratory may wish to consider whether the most effective use of resources is to 

continue these programs at their current levels.”10 Even presentations showing breakthrough 

results did not clearly articulate a vision for the future. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

The polymer projects in all six of the Polymers Division’s groups demonstrate 

outstanding technical performance in most areas, with examples of state-of-the-art 

accomplishments, and strike a good balance between exploring the frontiers of measurement 

science and technology and in transferring the know-how to U.S. industry for economic impact, 

strengthening U.S. competitiveness. The researchers have been publishing papers in journals, 

presenting at workshops, and giving invited presentations to conferences, industry, and 

academia. They also have received several noteworthy awards, including the Presidential Early 

Career Award for Scientists and Engineers, American Chemical Society fellow, and NIMS 

young scientist awards. 

The division’s programs are highly leveraged with cooperative research and development 

agreements, or CRADAs (e.g., the Electronics Materials CRADA with Intel Corporation), 

 10 National Research Council, 2005, An Assessment of the National Institute of Standards and Technology 

Measurement and Standards Laboratories: Fiscal Years 2004-2005, Washington, D.C.: The National Academies 

Press, p. 75. 

19 
interagency agreements (e.g., Biomaterials NIH Research Project Grants [R01s], 

Exploratory/Developmental Grants [R21s], National Institute of Dental and Craniofacial 

Research/NIH grants), visitors, sabbaticals (e.g., Intel, IBM, Seoul National University), and 

synergistic collaborations (e.g., SEMATECH in electronics materials). 

NIST-developed measurement methods can have far-reaching consequences in 

transforming U.S. industries and competitiveness. The Polymers Division should more 

aggressively cultivate relationships with analytical equipment companies, both as customers and 

collaborators, in order to define an easy path for technology to reach the marketplace. 

ADEQUACY OF INFRASTRUCTURE 

This division of 106 people with a budget of $14 million is pursuing 22 projects with a 

great deal of success. However, given the resources available, the division should either obtain 

additional resources or consider deemphasizing programs that require substantially more 

resources in order to offer a reasonable probability of success. A return on investment and/or 

impact assessment should be done, investment should be made, and resources should be placed 

in those areas where a significant impact can be made realistically. The fuel cell effort is an 

example. While this problem is important, it is a complex problem that requires a significant 

investment of personnel and other resources. The level of effort currently underway is 

insufficient to have substantial impact. This is not a criticism of the technical level of the current 

effort, but rather a realistic assessment of the potential outcomes. Either more investment needs 

to be made or the efforts of the program should be redirected elsewhere. 

The depth and breadth of the staff are impressive, as is the division’s continuing ability to 

attract high-quality staff, associates, and postdoctoral fellows. The objectives and the vision for 

building a diverse workforce will be challenging in the absence of significant hiring. 

Several group leaders are serving also as principal investigators for projects. While these 

leaders seem to be doing an effective job of carrying out both leadership and technical functions, 

this may not prove to be an effective long-term strategy. 

There was not apparent within the division a sufficient computational materials science 

effort to complement the outstanding experimental accomplishments. In several areas, theory 

and simulations to interpret the experimental measurements could likely provide additional 

predictive power. Hiring a knowledgeable senior computational scientist or NRC postdoctoral 

fellows with theoretical expertise may be an effective way to initiate an effort in this direction. 

ACHIEVEMENT OF OBJECTIVES AND IMPACT 

Electronic Materials Group 

The Electronic Materials Group has done an outstanding job of developing measurement 

methods for the use of polymeric materials for the electronics industry. The group has 

extensively collaborated with major industrial customers (Intel, IBM, and Advanced Micro 

Devices), consortia (e.g., SEMATECH), and academia. The effort is currently targeting 

opportunities to develop similar methods for emerging electronics areas (flexible electronics, 

OPVs, and energy). Its efforts in dimensional metrology with Intel and other collaborators using 

critical-dimension small-angle x-ray scattering (CD-SAXS) can complement, validate, and 

augment existing destructive and nondestructive pattern shape measurement technologies. 

20 
The high-quality, important, fundamental studies on understanding the materials sources 

of line-edge roughness are of significance in driving the electronics industry down Moore’s 

curve. An example is the development of measurement methods delineating the rheological 

basis for residual stress in patterns printed by nanoimprint lithography. It is important to apply 

this technology for sub-25 nm CMOS and non-CMOS patterning applications. 

The integrated suite of measurement capabilities, including x-ray techniques coupled 

with spectroscopy, serves as an example of how this group has been able to illustrate the 

importance of conjugated plane tilt and side chain interdigitation in explaining the serendipitous 

observation of high conductivity in pBTTT (poly(2.5-bis(3-quaterdecylthiophene-2-yl)-

thieno[3.2-b]thiophene), a thiophene-based copolymer. 

Nanostructured Materials Group 

The Nanostructured Materials Group has 14 people working on a large number of 

projects that do not seem to be related. For example, the templated assembly of block 

copolymers, fate of nanoparticles in biological systems, and fuel cell membrane efforts have 

little in common. Nevertheless the projects, such as the block copolymers work, appear to be 

well thought out and tightly coupled with industry and likely to have a broad impact. The 

measurement methods developed for gold and titanium dioxide nanoparticles and their 

aggregation and characteristics in biological systems are rigorous. 

Processing Characterization Group 

The 19 people in the Processing Characterization Group focus on nanotube metrology, 

directed assembly, and microrheometry. In the area of microrheometry, significant resources are 

to be deployed in the future in addressing measurement needs of complex fluids with rheology, 

spectroscopy, microscopy, and microfluidics. The Nanotube Metrology Program is outstanding 

and has made noteworthy progress since 3 years ago when demonstrated concepts during the 

previous NRC assessment were only at the idea stage. The integrated approach employing key 

techniques in dispersion, separation, and standards development with nanotubes is an example of 

the depth and breadth that this group brings to bear on addressing important measurement 

problems. 

Biomaterials Group 

The Biomaterials Group has made impressive progress in the past 3 years. The project 

on dental materials has been well refocused and reorganized to be of high impact by 

concentrating on improving the understanding of the fundamentals of composite shrinkage, stress 

development, tooth and composite interphase, and interphase stability under bacterial challenge 

in order to develop clinically relevant information related to shrinkage and microleakage. There 

is an opportunity for this group to find a pathway for biomarker materials to become available to 

U.S. industry and academia, as they can have a high impact on biomedical research. The 

Quantum Dot Program is exemplary in this regard in terms of quality of work. 

The Protein Preservation project systematically examined the relationship between 

material properties and protein stability using a model system and found that there is a 

correlation between local glass dynamics and protein stability in glass. This group has 

21 
developed a benchtop surrogate for neutron backscattering using steady-state fluorescence 

techniques. 

The major emerging industry in regenerative medicine will continue to raise 

multifactorial problems in materials science. There will be a growing and continuing need for 

standards and metrology that address the needs of this industry, with NIST uniquely positioned 

to play a large role. Progress is being made in this regard and, in particular, there has been close 

cooperation with ASTM to provide leadership in the development of reference scaffolds for 

tissue engineering. 

Characterization and Measurement Group 

The Characterization and Measurement Group has enjoyed great success in its MachineReadable Travel Documents project, in which it tackled an important problem for the U.S. 

Department of State and carried it out remarkably well. This group has the capabilities needed to 

address challenging technical problems quickly and well. 

The group is performing a study of the ballistic resistance of polymeric materials by 

examining compromised body armor. The results obtained using a folding test apparatus 

designed by the group motivated the U.S. Department of Justice’s National Institute of Justice to 

include folding protocols in the draft of its current ballistic armor standard. The group should 

pursue opportunities for beneficial follow-on projects. 

The project on Thermal Properties at the Nanoscale has developed new measurement 

techniques for nanothermomechanometry. One application to carbon fullerenes (C60) was 

mentioned to the panel. It has promising potential for other applications. 

Combinatorial Methods Group 

The Combinatorial Methods Group has done an outstanding job of retaining the best of 

an open-source consortium model while expanding the underlying core strengths of the group to 

probe complex interfaces and thin films. The group has accomplished impressive developments 

of a library of microfluidic surface-initiated grafted copolymers with systematic gradients in 

chemistry, architecture, and molecular weight. It has also developed an impressive microfluidic 

technique to determine copolymer reactivity ratios. 

CONCLUSIONS 

The Polymers Division is doing an effective job in building an outstanding research team. 

The team is talented, energetic, and motivated to have an impact on polymer measurement 

science and technology. The division should review its programs to ensure a critical mass per 

program by either providing more resources or trimming the number of programs. Building 

some computational work is important to complement the outstanding experimental 

accomplishments. In several areas, theory and simulations to interpret the experimental 

measurements could likely provide additional predictive power. Energy is a significant 

contemporary problem, and NIST in general and the Polymers Division specifically can make 

important contributions to the measurement science and technology related to OPVs and energy 

storage devices. 

22 
Programs Funded Under the America COMPETES Act 

SUMMARY 

The funding under the America COMPETES Act started in FY 2007, so it is early to 

assess its impact. The projects benefiting from the funding are well conceived, and the first 

results are positive. The Ceramics Division is responsible for enhancing the NIST capability in 

the National Synchrotron Light Source at the Brookhaven National Laboratory. It is effectively 

applying the funding to attain new capability such as interfacial structure measurements on highdielectric-constant gate oxides. The enhanced research capability is significant enough that it 

should be managed in a way that brings broader participation from NIST in establishing 

priorities for the portion of beam time that NIST controls. The Metallurgy and the Materials 

Reliability Divisions share in executing a program to develop standards and test protocols related 

to the hydrogen economy—specifically, to the safety of pipelines to transport hydrogen under 

high pressure. A flexible research and test facility is under construction at the NIST facility in 

Boulder that promises to greatly enhance the capability of NIST to study this complex problem. 

A related project to measure hydrogen content rapidly in order to assess materials compatibility 

is solid but small. The project to build the first broadband coherent anti-Stokes Raman scattering 

microscope is off to a good start in the Polymers Division. 

CERAMICS DIVISION 

A strong core competence of the Ceramics Division is in the area of x-ray measurements 

on materials, in which the use of a synchrotron as the x-ray source represents a very important 

class of measurement technique. Synchrotrons provide a source of x-ray radiation that is intense, 

bright, collimated, tunable, and polarized—all characteristics not available from laboratory x-ray 

sources. This technique offers uniquely accurate subnanometer-resolution measurements of the 

electronic, chemical, and spatial structure of advanced materials, including semiconductor 

electronic materials, polymeric materials, nanotubes, catalysts, and biomaterials. 

The Synchrotron Methods Group within the Ceramics Division focuses on three 

important technical areas: the development of synchrotron measurement methods, material 

structural determination using synchrotron measurements, and synchrotron beam-line operations 

at the National Synchrotron Light Source, a DOE national user facility at the Brookhaven 

National Laboratory in New York. NIST’s Synchrotron Methods Group operates three beam 

lines (experiment stations) that have x-ray wavelengths appropriate for measurements on 

materials spanning the entire Periodic Table of the Elements. The NIST group is widely 

recognized as a pioneer and leader in the development and application of synchrotron-based 

techniques, and opportunities to use the NIST beam lines are in high demand. Although the 

facility operates full 24-hour days, industry and academia applicants seeking facility 

measurement opportunities exceed capacity by nearly 2 to 1. 

The expertise of the NIST team lies principally in the area of specialized detectors. The 

funding under the America COMPETES Act has been directed toward several specific capability 

upgrades: 

• A state-of-the-art analyzer and multi-element detector for near-edge x-ray absorption 

spectroscopy (NEXAFS) capability was installed in 2007 on beam line U7A. In 

23 
addition, funding has been committed to the NIST Electronics and Electrical 

Engineering Laboratory in Boulder, Colorado, for the development of a detector to 

provide unprecedented NEXAFS sensitivity and selectivity. This work is in progress 

and slated for completion in December 2009. The application of this capability is in 

the surface chemistry and molecular structure of materials, including self-assembled 

monolayers, deoxyribonucleic acid (DNA), proteins, other biological materials, 

organic and molecular electronics, polymer surfaces and interfaces, catalysts, and 

nanotubes. 

• A new detector for extended x-ray absorption fine structure capability was installed 

in 2007 on beam line X23A2. The application of this capability is in measuring 

local atomic and electronic structures from nanolayer thin films to bulk materials and 

from crystalline to highly disordered materials of higher molecular weight 

(beginning with titanium on the Periodic Table). 

• A new, high-throughput endstation for x-ray standing wave spectroscopy capability 

was installed in 2007 on beam line X24A. This line is used for the lower- and 

middle-molecular-weight materials. 

• A major project, in excess of $1 million capital, was begun in partnership with 

Sandia National Laboratories to implement a new variable kinetic energy x-ray 

photoelectron spectroscopy (VKE-XPS) capability on beam line X24A for highspatial-resolution measurements. The new surface measurement capability will be 

completed in 2008, and enhanced depth measurements, to less than 1 nanometer, 

will be completed in 2009. A scientific program using the high-throughput VKEXPS was initiated with SEMATECH to study next-generation transistor gate layer 

structures. 

• A novel three-dimensional VKE-XPS chemical microscope is under development, 

also for beam line X24A. This capability will provide strategic chemical and 

structural insights in nanotechnology applications such as transistor gate-stacks, 

organic electronics, MEMS lubrication, self-assembled-monolayer templates, and 

catalysts. The project is a Phase II SBIR collaboration slated for delivery in the 

summer of 2009. 

• Owing to the unexpected flat funding under the America COMPETES Act in 2008, 

two projects were put on hold: the Synchrotron Enhanced Scanning Tunneling 

Microscopy project and the Modernized High-Resolution Diffraction Beamline 

project. 

An exciting and very timely development is the DOE announcement that a new, billiondollar beam line—NSLS II—will be built on the Brookhaven site, with groundbreaking in 2009 

and occupancy starting in 2012. The x-ray radiation source will be 10,000 times brighter than 

the current NSLS, with the potential for major enhancements in measurement capabilities. The 

existence of the NIST ACI Synchrotron project enables NIST to plan construction of two new 

state-of-the-art beam lines in the new facility. The NIST team has already begun responding to 

this exciting and unique opportunity to maintain leadership in synchrotron-based materials 

measurements. 

The capability emerging from the enhanced funding is broadly applicable to NIST 

programs; therefore, it may be desirable to establish a formal process for prioritizing the projects 

that are performed during the time that the facility is under NIST control. (The DOE user24 
facility process that competitively selects projects determines who uses the beam lines the 

remainder of the time.) 

MATERIALS RELIABILITY DIVISION

The hydrogen pipeline safety project is part of a coordinated NIST program to develop 

the infrastructure for a hydrogen economy. The Metallurgy Division is focusing on research and 

development test methods to look at issues such as developing hydrogen-resistant alloys and 

looking at supersaturation effects on alloys. The Materials Reliability Division has taken 

responsibility for measuring the mechanical properties, in the presence of hydrogen, of existing 

and new high-strength pipeline steels. The purpose is to ascertain whether, and at what 

pressures, existing gas or petroleum pipelines in the United States could be used for shipping 

hydrogen around the country in preparation for a possible hydrogen fuel economy. This is an 

essential material property measurement activity for which the Materials Reliability Division is 

well equipped based on its past and present experience in bulk material property mechanical 

testing and pipeline testing. The facility that the division needs for extending its capabilities to 

testing in hydrogen is under construction and will give NIST at Boulder an unrivaled facility for 

testing pipeline steels under realistic hydrogen transportation conditions. 

METALLURGY DIVISION 

One project in the Metallurgy Division modestly funded through the America 

COMPETES Act is focused on competitiveness relative to the hydrogen economy. Since the 

project is at an early stage, an assessment of it may be premature; however, in general it is off to 

a good start. It is the Hydrogen Distribution (hydrogen embrittlement of steels) project, which 

has a sound technical approach and is a worthwhile activity. NIST has the required expertise to 

meet the project’s objectives. The level of coordination between MSEL divisions on this project 

is excellent. The tie between this project and increasing American competitiveness is somewhat 

tenuous, but the transportation of gaseous hydrogen is clearly important to the success of the 

hydrogen economy. 

A second project receiving funding through the America COMPETES Act is an effort to 

develop a rapid high-throughput measurement of hydrogen content for assessing novel materials 

for hydrogen storage. This Hydrogen Storage project is technically sound and has demonstrated 

the feasibility of a new measurement approach (infrared emissivity) for attacking this problem. 

The magnitude of the effort may be too small to make a major impact. If successful, when the 

hydrogen economy becomes a reality, this project could assist in spawning new industries, thus 

improving U.S. competitiveness. 

POLYMERS DIVISION 

The Bioimaging Program and efforts in optical coherence microscopy, broadband 

coherent anti-Stokes Raman scattering (CARS) microcopy, and the associated technology efforts 

fit the mission of ACI. The Optical Coherence Microscopy Program is on its pathway to 

commercialization with an SBIR Phase III program. CARS technology is unique because of its 

ability to image cells with three-dimensional spatial resolution, non-invasively and without using 

labels. Using contrast in vibrational spectra, CARS microscopy can provide physical and 

25 
chemical information from the cells to characterize their response to different materials as well 

as determine differences in spatial heterogeneities between normal and diseased cells. 

The Bioimaging Program built the first broadband CARS instrument in 2004, has more 

recently developed time-resolved detection methods to reduce nonresonant background, and has 

developed algorithms for faster and flexible spectral recovery. 

26 
Overall Conclusions 

The Materials Science and Engineering Laboratory is meeting its stated objectives of 

providing state-of-the-art metrology services to both traditional industry and emerging industries. 

The partnerships with other federal agencies, industry, and universities to extend the MSEL’s 

expertise into the biology and medical fields are noteworthy. The laboratory’s facilities are very 

good, given the budget constraints, and a number of unique and state-of-the-art experimental 

capabilities exist in the MSEL. The MSEL programs could benefit from a modest increase in 

theory and modeling to complement the strong experimental studies. The laboratory’s project 

evaluation process to ensure focus on the needs of NIST’s customers has had a beneficial effect. 

Progress on the recently initiated ACI-related programs is excellent. 

27