TABLE OF CONTENTS

                                                                       Page
OVERVIEW . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1

TECHNICAL ACTIVITIES . . . . . . . . . . . . . . . . . . . . . . . . . . .4

     Ceramic Coatings. . . . . . . . . . . . . . . . . . . . . . . . . . .5

     Ceramic Machining . . . . . . . . . . . . . . . . . . . . . . . . . 18

     Ceramic Processing. . . . . . . . . . . . . . . . . . . . . . . . . 26

     Electronic and Photonic Ceramics. . . . . . . . . . . . . . . . . . 33

     Evaluated Materials Data. . . . . . . . . . . . . . . . . . . . . . 50

     Intelligent Processing of Materials . . . . . . . . . . . . . . . . 60

     Mechanical Properties of Brittle Materials. . . . . . . . . . . . . 70

     Nanostructured Materials. . . . . . . . . . . . . . . . . . . . . . 87

     Standard Reference Materials. . . . . . . . . . . . . . . . . . . . 91

     Superconductivity . . . . . . . . . . . . . . . . . . . . . . . . .103

     Synchrotron Radiation . . . . . . . . . . . . . . . . . . . . . . .113

     Theory and Modeling . . . . . . . . . . . . . . . . . . . . . . . .125

     Other Projects. . . . . . . . . . . . . . . . . . . . . . . . . . .131

RESEARCH STAFF AND FIELDS OF INTEREST. . . . . . . . . . . . . . . . . .136

SUMMARY:  OUTPUTS AND INTERACTIONS . . . . . . . . . . . . . . . . . .  148

     Patents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .149

     Conferences and Workshops Sponsored . . . . . . . . . . . . . . . .151

     Standard Reference Materials. . . . . . . . . . . . . . . . . . . .153

     Technical/Professional Committee Leadership . . . . . . . . . . . .155

     Industrial and Academic Interactions. . . . . . . . . . . . . . . .161

FACILITIES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .183

APPENDIX . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .192

     Organizational Chart
      National Institute of Standards and Technology

     Organizational Chart
      Materials Science and Engineering Laboratory

     Organizational Chart
      Ceramics Division

DISCLAIMER

Certain trade names and company products are mentioned in the text or identified in illustrations
in order to adequately specify the experimental procedure and equipment used.

In no case does such identification imply recommendation or endorsement by the National
Institute of Standards and Technology, nor does it imply that the products are necessarily the best
available for that purpose.                                 OVERVIEW

The format of the 1995 NIST Ceramics Division Report is similar to that begun last year,
emphasizing the programmatic nature of our activities rather than those of individual groups. 
Scientific and technical descriptions of research are organized by programs which are comprised
of individual projects.  Additional sections describe staff and skills, and important outputs of our
research.  This format reflects increasing intergroup activities and the desire to focus resources
on the most critical technical issues.  The participation of U.S. industry in all phases of the
research has been strongly encouraged, e.g., the consortia on Machining of Ceramics, and Powder
Processing from Slurries.  The output of the Ceramics Division program is made available to U.S.
industry and the ceramics community through a number of avenues including presentations,
publications, and direct collaborations with companies and universities.  During this past year the
research program produced 147 publications, about 80 presentations, and 3 invention disclosures. 
Four new Cooperative Research and Development Agreements (CRADAs) were signed with
companies and universities.

We are proud of the fact that a number of individuals in the Ceramics Division were the
recipients of special awards during the year:  Craig Carter was the first recipient of the Coble
Award from the American Ceramic Society based upon his work on the modeling of the sintering
process; Debra Kaiser received the Sigma Xi Outstanding Young Scientist Award for her work
on the magnetooptical imaging of flux pinning in high Tc superconductors; Ron Munro, Ed
Begley, and Joyce Harris were given Measurement Service Awards by the Standards Reference
Data Office for their development of the first comprehensive database of the properties of high
Tc superconductors; Tze-jer Chuang was made a Fellow of ASME, and Said Jahanmir was the
recipient of an ASME Service Award.

One new employee, Patricia McGuiggan, was hired into the Division in 1995.  Her expertise in
measurements of surface phenomena at the atomic level is expected to contribute significantly
to a new effort on microtribology.

Sandy Dapkunas completed a six-month term as an "NIST Industry Fellow."  The general
purpose of the Industry Fellow Program is to allow NIST personnel to spend time in U.S.
Industry to obtain first-hand knowledge of how NIST can best serve industrial needs.  Sandy
worked at the Pratt and Whitney Division of United Technologies Corp. in West Palm Beach
Florida with a group heavily involved in the development of coatings for aircraft engines.  His
goal during his stay there was to learn how materials transition from the laboratory to a product,
and how NIST can impact this process.  His experience there has already  enhanced the NIST
coatings program.

In 1995, the Ceramics Division continued a significant involvement with the Advanced
Technology Program (ATP), through funding by ATP to work directly with several ATP
awardees, through review and program monitoring, and through the efforts of Division personnel
who served on ATP Source Evaluation Boards and in the development of ATP focused programs. 
In addition Subhas Malghan has served in the NIST Program Office for much of 1995.

The Ceramics Division research program has had the following significant acccomplishments in 
1995:

    A microstructural model of strain effects in superconducting tapes has been developed. 
     This model is based on synchrotron radiation microradiography, optical microscopy, and
     electrical resistance measurements.

    The utility of magneto-optical imaging for routine nondestructive analysis of high Tc
     superconductors, even when the specimen surfaces are not polished, has been
     demonstrated.  

    NIST Standard Reference Database 62: High Temperature Superconductors, Version 1,
     has been completed.  This database provides evaluated thermal, mechanical, and
     superconducting property data for these materials commonly called high temperature
     superconductors. 

    An international workshop, jointly sponsored by NIST and the Institute for Mechanics and
     Materials, was held on April 22-23, 1995, in San Diego to discuss the scientific and
     standardization issues associated with instrumented indentation.  Over ninety
     representatives from industry, academia and national labs around the world met to discuss
     the indentation process, from both an experimental and a theoretical point of view, and
     to address the problems underlying the lack of standardization in the field.

    Small angle neutron scattering studies indicate that the prevailing orientation of the cracks
     in plasma spray deposited coatings depends directly on the spray angle.  Interlamellar
     pores, however, which are mostly parallel to the substrate surface, are unlike the cracks
     in that their orientation is not a strong function of spray angle.  The results offer the first
     proof that the quantity and the character of the porosity in these materials can each be
     controlled by selecting the appropriate processing protocols.

    Thirteen new procedures for characterization of powders for secondary properties were
     developed as part of the International Energy Agency program on powder characteriztion. 
     The procedures and 2000 powder samples were sent to the thirty-three participants from
     six countries. 

    Two procedures for primary characterization of ceramic powders have already passed the
     ASTM C-28 (American Society of Testing and Materials) main committee ballot and
     adopted as standards.  Three more procedures are in various committee levels.  Six
     additional procedures will be drafted for ASTM adoption.  Two standard reference
     materials (SRMs) have been produced using the procedures developed in this project.

    The results of studies conducted as part of the Ceramic Machining Consortium clearly
     show the effects on fracture strength of material batch-to-batch variations, repeatability,
     interlaboratory reproducibility, and machining conditions for three different silicon nitrides
     being considered for commercial applications.

    A thermal MOCVD system, designed and built at NIST for ferroelectric oxide film
     deposition, has been modified to include metalorganic bubblers with an oxygen preheater
     and improved temperature control.  These modifications have improved the reproducibility
     of the deposition experiments.  A set of processing conditions has been established for
     the deposition of epitaxial BaTiO3 films on single crystal MgO and KTaO3 substrates in
     the modified system.

    A non-parametric bootstrap statistical method has been applied to lifetime prediction of
     InP components exposed to water and to argon gas at 50% relative humidity. Use of
     nonparametric bootstrap method permitted lifetime predictions to be made and resulted
     in a proof-test level prediction which  would provide a desired lifetime of 27 years at a
     95% confidence level.

    The strain and bond distortions in epitaxial InAs, InGaAs and thicker InAs films have
     been studied via x-ray standing-wave and x-ray-absorption fine structure measurements. 
     The results indicate that, for both InAs and InGaAs monolayers, strain and bond
     distortions are accurately described by macroscopic elastic theory.  Thicker InAs films
     are found to collapse beyond a critical thickness of about 2 monolayers, accompanied by
     a large degree of structural disorder and bond-length relaxation.

    Standard Reference Materials (SRM's) were developed for ceramic Knoop and Vickers
     hardness which are compatible with ASTM and ISO standard test methods.  SRM #2830,
     the Knoop SRM became available in January, 1996.  SRM #2831, the Vickers standard,
     will be available in the summer of 1996.  Two standard test methods that rely in part on
     the SRM's have been adopted by ASTM.

    CRADAs were signed with Digital Equipment Corp. (now Quantum) and Censtor to
     jointly study the tribochemistry of the head-disk interface and to develop new
     instrumentation required  to measure head-disk durability.  Several testers were donated
     by our industrial partners to NIST to help to accelerate the research effort.

Stephen W. Freiman
Chief, Ceramics Division
                           TECHNICAL ACTIVITIES                             CERAMIC COATINGS

The Coatings program is a measurement and characterization effort which addresses the
processing reproducibility and performance prediction issues associated with, primarily, thermal-
spray deposited ceramic coatings.  The program focuses on plasma-spray-deposited ceramic
thermal barrier coatings used in aircraft gas turbines and expected to be used in land-based
turbines and diesel engines.  Sales in the thermal-spray industry are currently valued at over one
billion dollars annually, a significant portion of which is ceramic thermal-barrier coatings. 
Collaborations have been established with industrial organizations including Pratt and Whitney,
General Electric, Caterpillar, METCO, MetTech and Zircoa as well as the Thermal Spray
Laboratory at the State University of New York at Stoney Brook and the Thermal Spray
Laboratory at Sandia National Laboratory.  The program includes collaboration with the National
Aerospace Laboratory and the National Mechanical Engineering Laboratory, both in Japan, to
examine functionally gradient materials.  Research is also conducted on the processing and
properties of chemical-vapor-deposited (CVD) diamond films in collaboration with Westinghouse,
an Advanced Technology Program (ATP) awardee, and on Physical Vapor Deposited (PVD)
ceramic coatings in collaboration with Praxair, another ATP awardee.

Participants in the NIST program are located in the Ceramics, Materials Reliability and Reactor
Radiation Divisions of the Materials Science and Engineering Laboratory as well as the Chemical
Science and Technology Laboratory.

The approach taken in the plasma-spray (PS) research has been to build on the analytical
capabilities at NIST and the material processing capabilities of collaborators.  The program has
the following elements:

    development of techniques for characterization of physical and chemical properties of
     stabilized zirconia feedstock to provide data for increased processing reproducibility as
     well as data required for production of a Standard Reference Material suitable for
     calibration of light-scattering size distribution instruments used in industry for analysis
     of PS powder;

    development of scattering techniques to determine the quantity, size and orientation of
     porosity and microcracks in PS ceramic coatings suitable for use in modeling the
     thermomechanical behavior of these materials;

    development of methods to measure chemical, elastic modulus, and thermal properties on
     a scale suitable for use in microstructural models of behavior;

    development of techniques to model thermomechanical behavior of thermal-barrier
     coatings to enable more reliable performance prediction; and

    development of techniques for accurate measurement of the thermal conductivity of PS
     coatings by use of the guarded hot-plate technique suitable for incorporation in ASTM
     standards and to provide a method for comparison with routine industrial techniques.

Research on chemical mapping of powders and microstructures is conducted in the Microanalysis
Division of the Chemical Science and Technology Laboratory.  Thermal property research is
conducted in the Materials Reliability Division and the Reactor Division participates in both the
powder analysis and scattering projects.  A strong attribute of the PS coatings research is the use
of common materials for which complementary data can provide a more complete understanding
of processing-microstructure-property relationships.

Research is also conducted on the formation of chemically-vapor-deposited (CVD) diamond
films.  This research is focused on the hot-filament method utilizing graphite as a carbon source. 
This research has allowed the determination of basic system parameters which control nucleation
and growth of the diamond film in a relatively easily controlled, inexpensive process.

For additional information about the Coatings Program, please contact S. J. Dapkunas at
301-975-6119 or e-mail to Dapkunas@micf.nist.gov.

PROJECT TITLE:  Micro-Mechanical Modeling and Computer Simulations

PROGRAM TITLE:  Ceramic Coatings

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Fuller, Edwin R. Jr.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-5795
Fax number:           (301) 990-8729
E-mail address:            Edwin.Fuller@nist.gov

Other NIST Principal investigator(s):  Carter, W. Craig
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-3971
Fax number:                    (301) 990-8729
E-mail address:                     wcraig@pruffle.nist.gov

                               Langer, Stephen A.
Mailing Address:                    NIST
                               NIST North (820), 365
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5423
Fax number:              
E-mail address:                     stephen.langer@nist.gov

                               Roosen, Andrew R.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-6166
Fax number:                    (301) 990-8729
E-mail address:                     roosen@borax.nist.gov

Technical Description:

This project is designed to elucidate the mechanics and physics of heterogeneous materials at the
mesoscopic level and to develop computationally efficient algorithms and computational codes
for simulating the micro-mechanical behavior of advanced ceramic microstructures.
Technical Objectives:

This research is designed to assist industry in developing new paradigms for elucidating micro-
mechanical behavior, fracture, deformation, damage, and other nonlinear phenomena, in real and
simulated microstructures.  A technique for obtaining average linear response from a particular
microstructure is envisioned.  Predictions of response for simulated and digital representations
of actual microstructures are a primary goal.  Efficient storage and microstructural representation
techniques are to be developed.  The goal is the development of a set of tools which all materials
scientists can and will want to use.

Outcomes:

A new paradigm for materials calculations is foreseen through the development of the
computational tools which will forge this paradigm shift.  The tools could be further developed
by third parties and potentially lead to new commercial ventures associated with software
repackaging.  Finally, inexpensive means by which industry may test and design new
microstructures may be produced.

Accomplishments:

Averaged elastic behavior of thermal barrier coatings was calculated on a microstructural basis
from digitized images and compared with experimental measurements.  The computational
simulations were performed on random regions from a micrograph of polished sections of a
plasma sprayed zirconia coating.  Both plan and section views were considered.  Elastic
properties were treated as orthotopic in the plane.  Experimental measurements were performed
via Hertzian indentation with a spherical indenter on micro-hardness machine.  The specimen area
sampled for both the simulations and the experiments was approximately 0.01 mm2.

Localized microstructural strains in an heterogeneous microstructure were calculated from a
digitized micrograph of a polycrystalline alumina.  Texture information, which was input into
these calculations, was determined experimentally from backscattered Kikuchi patterns, electron
backscattered patterns (EBSP), in a scanning electron microscope (SEM).  Correlation of the
microstructural simulations with a micro-Raman techniques for measuring localized strains in an
heterogeneous microstructure was performed.

Initial studies of the elastic, thermal shock, and fracture behavior of silicon nitride have produced
exciting results.

Outputs:

Several important outputs were derived from this project.  A letter of appreciation was received
from the Ford Research Division signifying their appreciation for our initial efforts.  A computer
code, called OOF (Object-Oriented Finite Elements), is currently available for alpha-testing.

Technical papers:

J. Xu, B.N. Cox, M.A. McGlockton, W.C. Carter, "A Binary Model of Textile Composites II:
Elastic Regime," Acta Met and Metall.. 43 9 3511-3524 (1995)

Impact:

Many industrial researchers have asked that we model their particular problems and have asked
for use of our developed codes.

PROJECT TITLE: Instrumented Indentation

PROGRAM TITLE:  Ceramic Coatings

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Smith, Douglas T.
Mailing Address:           NIST         
                      Materials (223), A329
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5768
Fax Number:           (301) 990-8729
E-Mail Address:            dougs@mailserver.nist.gov

Other NIST Principal investigator(s):  Wallace, Jay S.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5984
Fax Number:                    (301) 990-8729
E-Mail Address:                     jwallace@mailserver.nist.gov

Technical Description:

In this program, the ability of instrumented (or continuously recording) indentation to determine
various mechanical properties of ceramic coatings and bulk materials is studied.  Work focuses
primarily on standardization issues and on methods for determining such material properties as
hardness, elastic modulus, yield strength, and resistance to microfracture.

Technical Objectives:

The program has four primary objectives:

1.   To organize workshops and symposia that will bring the indentation community towards
     consensus on recommended test and analysis procedures, and to participate in indentation
     round robins.

2.   To collect experimental data (load-displacement curves) and correlate them with analytical
     and numerical modeling of the indentation process, in order to better understand
     deformation processes beneath indenters, particularly in film-substrate and multilayer
     systems.

3.   To use instrumented indentation to quantify hardness, Young's modulus, porosity and
     microcrack density in ceramic coatings, both to characterize as-prepared coatings and to
     quantify damage evolution.

4.   To study the microstructural damage done in the indentation of brittle coatings and bulk
     material, and correlate with other material properties such as machinability and wear
     resistance that depend on microfracture processes.

Outcomes:

Recommended guidelines for test and calibration procedures will help users with different
machines and at different labs compare results effectively.

Reliable mechanical property data at small length scales will aid designers of thin film and
multilayer structures.

The use of indentation to introduce and quantify microcrack damage may lead to use of the
technique to predict wear resistance and fracture toughness easily.

Accomplishments:

An international workshop on instrumented indentation, sponsored jointly by NIST and the
Institute for Mechanics and Materials, was held in San Diego in April, 1995.  The workshop is
described under "Highlights," below.  Follow-up symposia are planned for 1996.

A higher-load instrumented indenter system was designed and constructed to extend
measurements to loads of 4 kg.  The previous maximum load had been 0.1 kg.

Instrumented indentation was used to study the machinability of dental ceramics.  Correlations
were observed between the energy absorbed in an indentation loading-unloading cycle and the
energy required to grind away a unit volume of material.

The technique was also used to quantify a) microcrack density in damaged silicon nitride and b)
porosity in thermal spray coatings, both through shifts in the Young's moduli of the materials. 

Output:

A detailed report on the Indentation Workshop is being prepared.  In addition, several technical
papers have published: 

Technical papers:

"Quantifying Local Microcrack Density in Ceramics: A Comparison of Instrumented Indentation
and Thermal Wave Techniques," D.T.  Smith and L. Wei, J. Amer. Ceram. Soc. 78, 1301 (1995).

K.G. Kreider, M.J. Tarlov, G.J. Gillen, G.E. Poirier, L.H. Robins, L.K. Ives, W.D. Bowers, R.B.
Marinenko and D.T. Smith, "Sputtered Amorphous Carbon Nitride Films."  Journal of Materials
Research, in press.

L.M. Hsiung, R.L. Lankey, H.N.G. Wadley, D.T. Smith, J.Z. Zhang, J.W. Golz, B.L. Halpern and
J.J. Schmitt, "Jet Vapor Deposited Aluminum-Aluminum Oxide Nanolaminates."  For "Novel
Techniques in Synthesis and Processing of Advanced Materials," TMS/ASM Materials Week 
1994, in press.

Impact:

The instrumented indentation program in the Ceramics Division is still relatively new, and as yet
has had only modest demonstrated impact in the industrial sector.  One clear benefit, however,
came from the workshop that is described below.  At that workshop, many attendees from
industry (25 from U.S. companies, 6 from foreign companies) had the opportunity to listen to,
and talk to, many of the leading researchers in the field.  (Some of the leading researchers are,
in fact in the industrial sector, and several gave presentations at the workshop.)  The interaction
gave the industry participants an up-to-date look at how the technique can help them characterize
the mechanical properties of the materials with which they work.

PROJECT TITLE:  Characterization of Thermal Spray Zirconia Powders

PROGRAM TITLE:  Ceramic Coatings

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Malghan, Subhas
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6101
Fax Number:           (301) 990-8729
E-Mail Address:            malghn@enh.nist.gov

Other NIST Principal investigator(s):  Pei, P.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-3681
Fax Number:                    (301) 990-8729 
E-Mail Address:                     ppei@enh,nist.gov

                               Dapkunas, S.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6130
Fax Number:                    (301) 990-8729
E-Mail Address:                     dapkunas@micf.nist.gov

Principal Investigator(s) Outside NIST:  Zajchowski, P.
Mailing Address:                      United Technologies, Pratt & Whitney
                                 400 Main Street M/S 165-34
                                 East Hartford, CT 06108
Telephone:                            (203) 565-8463
Fax Number:                      (203) 565-4108
E-Mail Address:           
                                 Harter, D.
Mailing Address:                      400 Main Street
                                 East Hartford, CT 06108
Telephone:                            (203) 565-8787
Fax Mumber:                      (203) 565-4108
E-Mail Address:      
Technical Objectives:

The objective of this project, conducted in collaboration with Pratt and Whitney (P&W) under
the auspices of the National Center for Manufacturing Science (NCMS), was to characterize mass
fraction (7 to 8%) yttria containing zirconia powders by physical and surface chemical techniques
to identify differences between powders manufactured by different methods and producers and
to develop correlations among powder properties and deposition efficiency.

Outcomes:

Two major outcomes are expected:  (1) development of correlations among powder properties
and deposition efficiency, (2) development of experimental procedures to characterize powders.

Accomplishments:

Through extensive interactions with thermal spray industry, thirteen powders produced by
different types of manufacturing processes were selected for this study. These powders were
manufactured according to the current P&W powder specifications but no correlations could be
developed among the powder properties, coating quality and deposition efficiency (DE). This lack
of correlation and powder variability was the motivation for conducting the present study.

The powder properties studied were: chemical composition, density (true, apparent and tap),
particle size distribution, powder morphology, agglomerate integrity, interface chemistry, relative
heat uptake by differential thermal analyses, phase composition, and specific surface area. The
above characterization procedures were developed and tested. The powder properties that affected
DE were tap density, relative heat uptake and selective PSD data. Data from characterization
methods such as density, agglomerate integrity and optical and SEM micrographs were able to
differentiate the powders by various manufacturing processes.

Impact:

Both the NIST developed characterization methods and the correlation established between the
powder properties and the performance of the thermal barrier coatings have enabled P&W and
other engine manufacturers to tighten powder specifications. This in turn would improve the
quality of the thermal barrier coated parts.

Outputs:

A SRM zirconia powder is in preparation to help the thermal spray industry to standardize their
experimental procedures such as PSD. 

Technical Paper:

"Characterization and Processing of Spray Dried Zirconia Powders for Plasma Spray Application"
P.Pei, S.G.Malghan, S.J. Dapkunas and  P.H.Zajchowski, Journal of Thermal Spray Technology,
In print

PROJECT TITLE:  Processing / Microstructure Relationships in Plasma-Sprayed Coatings

PROGRAM TITLE:  Ceramic Coatings   

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Long, Gabrielle G.
Mailing Address:           NIST
                      Materials (223), A163
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5975
FAX number:           (301) 990-8729
E-mail Address:            gabrielle.long@.nist.gov

Other NIST Principal investigator(s):  Allen, Andrew J.
Mailing Address:                    NIST
                               Materials (223), A163
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5982
FAX number:                    (301) 990-8729
E-mail Address:                     andrew.allen@.nist.gov

Principal Investigator(s) outside NIST:  Ilavsky, Jan
Mailing Address:                     Thermal Spray Laboratory
                                State University of New York
                                Stony Brook, NY 11793
Telephone:                           (301) 975-4435
Fax number:                     (301) 990-8729
E-mail Address:                      jan.ilavsky@.nist.gov

Technical Description:

This project is designed to characterize the pore and crack microstructure of plasma-sprayed
ceramic coatings as a function of processing parameters, and relate these to the properties of the
deposit product. 

Technical Objectives:

The technical objective of this project is a systematic investigation of
processing-microstructure-property relationships leading to improved process models that can
ultimately offer quantitative predictability of product plasma-sprayed ceramic microstructures. 

Outcomes:

These investigations are expected to result in a better understanding of the
processing-microstructure-property relationships in plasma-spray deposition of ceramics. 
Improved processing models will enable the prediction and control of the deposit properties as
a function of the spray system and the spray parameters, optimization and reduction of
development costs of deposits in engineering practice, and broadening of the field of applications
due to increased reliability and predictability of the deposits.

Accomplishments:

Plasma-sprayed deposits are composed of splats created by the rapid solidification of molten or
semi-molten feedstock particles.  Rapid cooling of the particles results in the formation of
metastable phases and complex microstructures.  The main features in the microstructure of
plasma-sprayed coatings are the splats, separated by interlamellar pores, voids around unmelted
particles, and cracks that are most likely formed upon cooling.
Small-angle scattering was applied to the quantitative characterization of the crack and pore
microstructure of plasma-sprayed deposits.  The anisotropic character  of the microstructure has
been observed and the methods and techniques for separating the intralamellar crack population
from the interlamellar pore population have been  developed, in which the surface areas and
volume of each are derived.  

Outputs:

J. Ilavsky, H. Herman, C. C. Berndt, A. N. Goland, G. G. Long, S. Krueger, and A. J.
Allen,"Porosity in Plasma-Sprayed Alumina Deposits" in Thermal Spray _ Industrial
Applications, C. C. Berndt and S. Sampath, Eds. (ASM International, 1994) 709-714.

J. Ilavsky, A. J. Allen, G. G. Long, S. Krueger, H. Herman, C. C. Berndt, and A. N. Goland,
"Anisotropy of the Surfaces of Pores in Plasma Sprayed Alumina Deposits"  in Thermal Spraying
_ Current Status and Future Trends, A. Ohmori, Ed. (High Temperature Society of Japan, 1995)
483-488.

J. Ilavsky, A. J. Allen, G. G. Long, S. Krueger, C. C. Berndt, and H. Herman, "Influence of
Spray Angle on the Pore and Crack Microstructure of Plasma-Sprayed Deposits" J. Amer. Ceram.
Soc., in press (1996).

A. J. Allen, N. F. Berk, S. Krueger, G. G. Long, H. Kerch, and J. Ilavsky, "New Developments
in Multiple Small-Angle Scattering Studies of Advanced Ceramics," in Neutron Scattering in
Materials Science _II, D. Neumann, T. Russell and B. Wuensch, Eds. (Materials Research
Society, Pittsburgh, 1995)  347-352.

                             CERAMIC MACHINING

Recent studies have estimated that of the total production cost, machining can account for (30
to 60)% and sometimes even up to 90% for high-precision ceramic components.  The high cost
and sometimes uncertain reliability at times associated with machining damage in ceramic
components in comparison with their metallic counterparts are often cited as impediments to the
wide spread use of these materials.  The goal of the NIST Ceramic Machining Program is to
assist the U. S. industry, through a joint research program, in the development of precision
machining technology for the manufacture of reliable and cost-effective products made from
advanced ceramics.  In addition to research within MSEL, joint research is conducted with the
Precision Engineering Division, Automated Production Research Division, and Statistical
Research Division.  The specific projects address Grinding Optimization, Machinability Database,
Nano-Precision Grinding, Mechanisms of Material Removal, Characterization of Machining,
Damage, and Chemically Assisted Machining.

The research in this program is conducted in cooperation with ceramic producers and users as
well as the academic research community and government laboratories.  Much of this research
is conducted as part of the NIST Ceramic Machining Consortium, consisting of 20 members from
industry and academia, and which provides guidance on manufacturing issues and near term
implementation of program results.

Current research materials include those intended for structural applications, such as silicon
nitride, and dental materials, such as machinable glass.

For additional information about the Machining Program, contact Said Jahanmir at 301-975-3671
or e-mail requests to Said@enh.nist.gov

PROJECT TITLE: Ceramic Machining Consortium

PROGRAM TITLE: Ceramic Machining

Principal investigator(s):  

NIST Staff:
Designated Project Leader:  Jahanmir, Said
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-3671
Fax number:           (301) 990-8729
E-mail address:            Said@enh.nist.gov

Other NIST Principal investigator(s):  Ives, Lewis K.
Mailing Address:                    NIST
                               Materials (223), A265
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6013
Fax number:                    (301) 990-8729
E-mail address:                     lkives@enh.nist.gov

                               Cellarosi, Mario
Mailing Address:                    NIST
                               Materials (223), A265
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6123
Fax number:                    (301) 990-8729
E-mail address:                     cellarosi@enh.nist.gov

Principal investigator(s) outside NIST:  Allor, Richard
Mailing Address:                     Ford Motor Company
                                Scientific Research Laboratory
                                P.O. Box 2053, Mail Drop 2313
                                Dearborn, MI 48121
Telephone:                           (313) 322-4338
Fax number:                     (313) 323-1129

                                Ikeda, Jeri A. S.
Mailing Address:                     Norton Company
                                P.O. Box 15008, MS 420-301
                                Worcester, MA 01615-0008
Telephone:                           (508) 795-2459
Fax number:                     (508) 795-4283
E-mail address:                      ikeda@world.std.com

Technical Description:

This project provides measurement methods, data, and mechanistic information needed by
industry for their effort in developing  innovative, cost-effective methods for machining of
advanced ceramics.  The specific projects during the reporting period were as follows: (1)
Grinding Optimization, (2) Machinability Database, (3) Nano-Precision Grinding, (4) Mechanisms
of Material Removal, and (5) Characterization of Machining Damage.  Industrial and academic
organizations participate in this program by either joining the Ceramic Machining Consortium
or by signing a CRADA for joint research on specific research tasks.  The following is a list of
organizations who were members of the Consortium during the last year: Ceradyne, Inc.;
Cercome, Inc.; Cincinnati Milacron, Inc.; Corning, Inc.; Dow Chemical Company; Eaton
Corporation; Eonic, Inc.; Ferro Corporation; Ford Motor Company; General Electric Company;
General Motors Corporation; Georgia Institute of Technology; Norton Company; Stevens Institute
of Technology; Texas A&M University; Torrington Company; Tower Oil and Technology
Company; University of Connecticut; University of Maryland; University of Massachusetts;
University of Rochester; and West Advanced Ceramics, Inc.  In addition, the Norton Company
contributed to the machining efforts through an individual CRADA.

Technical Objectives: 

The objective of this program is to assist the U. S. industry, through a joint research program,
in the development of precision machining technology for the manufacture of reliable and cost-
effective products made from advanced ceramics.

Outcomes:

Five major outcomes are expected from this program: (1) recommendations for optimum sets of
grinding parameters to be used on specific silicon nitride ceramics, (2) a PC-based database
containing data and information on machinability of advanced ceramics, (3) guidelines for
obtaining damage-free nano-precision surfaces made from bearing grade silicon nitride ceramics,
(4) descriptive models for the process of material removal in grinding including the role of
microstructure and the effect of mechanical properties on grinding, and (5) characterization of
grinding-induced damage in different ceramics and evaluation of several non-destructive
techniques for damage detection.

Accomplishments:

The effect of grinding parameters on strength and surface finish of three commercial silicon
nitrides were evaluated in an industrial setting.  The results showed no distinguishable change
in fracture strength that could be associated with the different grinding conditions for the samples
ground in the longitudinal direction of the flexure test bars.  These tests also provided
information on the repeatability and reproducibility of results obtained in grinding as reflected
in surface roughness and strength of machined test samples.

The database structure and the search strategy for the Ceramic Machinability Database were
completed.  A prototype version was developed and evaluated internally.

Research on the microstructural aspects of the material removal process in grinding showed that
intergranular fracture leading to grain dislodgement is the primary material removal process in
materials with weak grain boundaries and interfaces.  Analysis of ground surfaces showed that
the debris generated by grinding contain extremely fine particles that are much smaller than the
grain size of the material being ground.  Suggesting that the grains are shattered just prior to
separation from the surface.

The results of bi-axial strength tests on ceramics with a rising R-curve behavior showed that such
materials have a greater tolerance toward machining-induced damage in comparison with
ceramics possessing a flat R-curve.  The results of this study suggest that in addition to the
enhanced damage tolerance, these materials also posses an improved machinability through easy
intergranular microfracture.

The feasibility of a thermal wave measurement method and an ultrasonic method were evaluated
for the detection of machining-induced damage in ceramics.  Both methods were found to be
capable of detecting microcracks (on the order of 20 micrometers) that could reduce the strength
of ceramic components.

Outputs:

The results of this research program were discussed with the industrial and academic partners on
a semi-annual basis.  In addition to these interactions, the NIST staff were invited to participate
in more than a dozen conferences and technical workshops devoted to ceramic machining.  

Technical Papers:

Ahn, H. S., Wei, L. and Jahanmir, S., "Non-destructive Detection of Damage Produced by A
Sharp Indenter in Ceramics," Manufacturing Science and Engineering, PED-Vol. 68, ASME
Press, New York, NY, (1994) 923-933.

Xu, H. H. K. and Jahanmir, S., "Microfracture and Material Removal in Scratching of Alumina,"
J. Materials Sci., 30 (1995) 2235-2247.

Xu, H. H. K., Jahanmir, S. and Wang, Y., "Effect of Grain Size on Scratch Interactions and
Material Removal in Alumina," J. Am. Ceram. Soc., 78 (1995) 881-891.

Xu, H. H. K. and Jahanmir, S., "Effect of Grain Size on Scratch Damage and Hardness of
Alumina," J. Mat. Sci. Lett., 14 (1995) 736-739.

Xu, H. H. K. and Jahanmir, S., "Scratching and Grinding of a Machinable Glass-Ceramic with
Weak Interfaces and Rising T-Curve," J. Am. Ceram. Soc.,  78 (1995) 497-500.

Xu, H. H. K. and Jahanmir, S., "Effect of Microstructure on Abrasive Machining of Advanced
Ceramics," Ceramic Eng. and Sci. Proc., 16 (1995) 295-314.

Liang, H. and Jahanmir, S., "Boric Acid as an Additive for Core-Drilling of Alumina," J. of
Tribology, 117 (1995) 65-73. 

Jahanmir, S., Hwang, T., Whitenton, E., Job, L. and Evans, C., "Measurement and Analysis of
Forces in Grinding of Silicon Nitride," Proc. of ASME Tribology Symposium, H. Masudi (ed.),
PD-Vol. 72, ASME Press, New York, NY, (1995) 15-24.

Strakna, T. J., Jahanmir, S., Allor, R. and Kumar, K., "Effect of Grinding Direction on Fracture
Strength of Silicon Nitride," Machining of Advanced Materials, S. Jain and D. Yang (eds.),
AMD-Vol. 208, ASME Press, New York, NY, (1995) 53-64.

Wei, H. H. H. Xu, and S. Jahanmir, "Evaluation of Thermal Wave Imaging Technique for
Detection of Machining Damage in Ceramics," NIST IR 5645, March 1995.

Hsu, C. J., Wang, J. C., and Hsu, S. M., "Chemically Assisted Machining of Si3N4," Advances
in Science and Technology 9, High Performance Materials in Engine Technology, P. Vincenzini,
Editor, Techna, 1995.

Patents:

1.  "Method of Fabricating Articles," U.S. Patent Application Serial No. 08/062,534.

Impact:

The seventeen companies that have signed CRADA's to either join the Ceramic Machining
Consortium or to participate in a specific joint research project, have a direct access to the
information generated in this program.  The results of the NIST research program on ceramic
machining is being used by these companies to develop new ceramic materials and grinding
fluids, and to optimize their manufacturing operations to develop cost-effective methods.  In
addition, participation of the six academic institutions provides a unique opportunity both for the
industry members and for the university faculty and their students.   This program provides a
unique educational opportunity for the students to participate in an industry-lead research
program. 
PROJECT TITLE:  Chemically Assisted Machining of Ceramics

PROGRAM TITLE:  Ceramic Machining

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Hsu, Stephen M.
Mailing Address:           NIST
                      Materials (223), A265
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6120
Fax Number:           (301) 990-8729
E-Mail Address:            hsu@micf.nist.gov

Principal Investigator(s) outside NIST:  Uphoster, Russ
Mailing Address:                     Kennametal Inc.
                                P. O. Box 231
                                Latrobe, PA 15650
Telephone:                           (412) 539-5441
Fax Number:                     (412) 539-5255

Technical Description:

The US ceramic industry has identified the current machining technology with its low material
removal rate as a major cost barrier to the introduction of advanced ceramics into mass markets.

Rapid machining of tough ceramics such as Si3N4 often is not feasible because of the rapid heat
build up at the interface due to high friction, and the possible introduction of residual surface
cracks which often render the component unusable.  Machining research in Germany and Japan
have emphasized ultra-stiff machine design, heat control, and continuous electrochemical wheel-
dressing.  Both countries have had national programs on machining of ceramics for the past five
years.  Many of the advanced machining tools are now designed and built in these countries.  
The machining industry in the U.S. is mostly small machine shops where expensive machinery
often poses an unacceptable economic burden.  Within these constraints, chemically assisted
machining technology represents an attractive technological option, as well as a major
competitive edge for the U.S. machining industry.  Chemically assisted machining (CAM)
technology, if it is brought into fruition will be low cost, will not require expensive machining
tools, and will significantly lower the ceramic components manufacturing cost.

This project is to survey various chemical environments and to assess their effects on the rate of
materials removal, surface finish, amount of diamond wear during ceramic machining processes;
develop basic measurement methodology and standards to assess the effects of coolants on
machining; conduct basic mechanism studies on promising chemical compositions, and based on
the results, develop new chemistries to increase the machining rate, improve the surface quality
at lower cost.

Technical Objectives:

The project objective is to increase the rate of ceramic machining while controlling the surface
finish through modification of contact stresses and material properties by controlled surface
chemical reactions.  The technology should be capable of providing cost-effective machining
techniques using existing machining tools.  

Accomplishments:

A simple bench-top cutting device with a diamond wheel was used for screening chemistries. 
Tests were performed at various speeds and loads, and material removal rates and cutting forces
were measured.  Results have shown that coolant chemistry can influence the material removal
rate by several order of magnitudes without changing the surface quality.  There is no current
coolant that is specifically designed for ceramic machining.

Toxicity and waste disposal are important criteria in the selection of chemistries as the machining
industry is under constant pressure to avoid the use of halogens and other traditional chemistries
used in the industry.  Several chemistries have been identified and they significantly increase the
machining rate.

We are working closely with Kennemetal Corp. who has an existing production line producing
silicon nitride and Sialon wear inserts.  Their input and guidance have proved to be invaluable. 
Samples of coolant and materials were supplied to us.  These are materials currently being used
in their production facility.  This provides a sound baseline of current technology and practice. 
They have also provided test procedures for corrosion so that we can screen the chemistries more
effectively.

A surface grinder was set up and instrumented.  Precise grinding test procedures (constant feed
rate and constant pressure procedures) were developed to assess chemical effects on machining. 
Results confirmed findings from the cutting tests.  The G ratio, the ratio of diamond wheel wear
to the amount of material removed, was measured using a wheel print method.  A four fold
increase in the G ratio was achieved using an experimental chemistry.  Analysis of the results
suggested that the wear of the diamond was crucial in controlling the materials removal rate.  For
grinding silicon nitride, a minimum grinding (tangential) force was necessary to start the material
removal process and this minimum force was different for different fluids.  A maximum grinding
force beyond which further increase in grinding force would not increase the material removal
rate but would increase the surface damage also existed.  The maximum force is also different
for different fluids.  This suggested optimum grinding conditions existed for a particular wheel-
fluid-workpiece combination that would have the fastest grinding rate and minimum surface
damage.  These findings have also been validated on a vertical grinder which was donated by
Kennemetal.

Outputs:

Technical Publications:

Wang, J. And Hsu, S. M., "Chemically Assisted Machining of Ceramics," J. of Tribology, 116,
423-429, 1994.

Hsu, C. J., Wang, J. C., and Hsu, S. M., "Chemically Assisted Machining of Si3N4, "Advances
in Science and Technology 9, High Performance Materials in Engine Technology, P. Vincenzini,
Editor, Techna, 1995.

Patents:

A process to chemically assisted machining of ceramics, filed in 1994 with the US Patent Office.

A process to assist machining of ceramics using chemicals, patent disclosure filed in NIST in
April 1995.

Impact:

The feasibility of chemically assisted machining of ceramics has been demonstrated.  This opens
up a new way to lower the cost of components made from advanced materials without the heavy
investment requirement of expensive machinery to machine advanced materials.  This technology
allows the US industries to regain some competitive edge in the fabrication and manufacturing
sector while providing a major advantage for the U.S. ceramic producers.
                            CERAMIC PROCESSING

Processing of ceramic powders to the green and sintered states is a major component in the
production of ceramics with high degrees of reproducibility and cost-effectiveness.  Several
programs have been initiated in a number of countries involved in advanced ceramics to address
these issues.  Technical elements affecting the cost-effective manufacturing are synthesis of novel
powders that have tailored properties, repeatability and reproducibility in the measurement of
powder properties, procedures for characterization of secondary properties of powders, powder-
aqueous environment interactions, and sintering behavior of green ceramics.

The program on ceramic processing is designed to address some of these issues with a focus on
improvement of measurement quality in ceramic powders processing.  This is accomplished by
providing the U.S. ceramics community the ability to control ceramic powder properties so that
cost-effective manufacturing can be achieved.  The current program continues to emphasize
structural ceramics with application of silicon nitride to automotive engines.  The specific
elements of the program are as follows:

    ceramic powder characterization techniques, measurement science, sensors and models for
     intelligent processing, standard methods and standard reference materials;

    powder processing science to understand interrelationships between powder characteristics
     and their processing environment; and

    novel processing and synthesis methods as applied to nanosize and ultra-pure powders.

Ceramic processing projects address the development of standard procedures, standard reference
materials, improving the scientific basis of powder dispersion measurements in slurries, overall
improvement in measurement accuracy, and leadership in national and international
standardization activities including the ISO and ASTM.  The powder characteristics of interest
include physical and surface chemical properties, and phase composition.  In addition, grain-
boundary characterization, and crystallographic texture investigations are carried out using
advanced characterization tools.  In powder processing, our efforts have been focused around
high-energy agitation milling of powders, textured Al2O3 microstructure, and hot-isostatic-pressing
of silicon nitride.

For further information on the Ceramic Processing Program, contact S. J. Dapkunas at 
301-975-6119 or e-mail to Dapkunas@micf.nist.gov.

PROJECT TITLE:  Powder Characterization

PROGRAM TITLE:  Ceramic Processing

Principal investigator(s):  

NIST Staff:
Designated Project Leader:  Malghan, Subhas
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6101
Fax number:           (301) 990-8729
E-mail address:            malghan@enh.nist.gov            

Other NIST Principal Investigator:  Lum, Lin-Sien
Mailing Address:                     Materials (223), A256
                                Gaithersburg, MD 20899
Telephone:                           (301) 975-3674
Fax Number:                     (301) 990-8729
E-Mail Address:                      lum@enh.nist.gov
          
Principal Investigator(s) outside NIST:  Nietfeld, G. 
Mailing Address:                     H.C. Starck GmbH & Co. KG
                                Federal Republic of Germany
                                Makio Naito
                                Research and Development Laboratory
                                Japan Fine Ceramics Center (JFCC)
                                Nagoya, JAPAN

                                Pompe, Robert
Mailing Address:                     Swedish Ceramic Institute (SCI) 
                                Goteborg, Sweden

Technical Description:

This project is aimed at developing and providing a set of commonly agreed procedures to be
used for characterization of ceramic powders used in the ceramic heat engine applications as well
as development of the understanding of the role of interfacial energy anistropy on the
microstructural evolution of ceramics.

Technical Objectives:

The overall objective of this project is to develop pre-standardization procedures for
characterization of secondary properties of powders such as those for the measurement of slurry,
pH, green density and porosity of green ceramics. 

Outcomes:

Major measurement outcomes are expected to occur: (1) collection of the procedures for
characterization of secondary properties, (2) ruggedness testing of the procedures by the
participants through the method of a interlaboratory comparison study to determine the major
variables and their impact on the resulting data, (3) refined of the procedures based on the results,
(4) development of specific and detailed procedures for characterization of secondary properties
to enhance the quality, repeatability and reproducibility of the measurements.

Impacts:

Many standards organizations such as ASTM, CEN (European Standards Committee) and JISE
(Japan Standards Association) are using the round-robin data and procedures for developing their
standards. This will lead to the development of international standards. Industrial laboratories are
using the SRMs developed from this project.

Outputs:

L.H. Lum, S.G. Malghan, and S.B. Schiller, "Standard Reference Materials for Particle Size
Analysis of Ceramic Powders by Gravity Sedimentation," Powder Technology, in press

Standard Reference Material 1978, Particle Size Distribution Standard for Sedigraph Calibration
(October 1993).

Standard Reference Material 659, Particle Size Distribution Standard for Sedigraph Calibration

PROJECT TITLE:  Sintering and Microstructure Development

PROGRAM TITLE:  Ceramic Processing

Principal Investigator(s):

NIST Staff:
Designated Project Leader:  Blendell, John
Mailing Address:           NIST
                      Materials (223), A215
                      Gaithersburg, MD  20899
Telephone:                 (301) 975-5796
Fax Number:           (301) 990-8729
E-Mail Address:            jblendell@enh.nist.gov

Other NIST Principal Investigator(s):  Vaudin, Mark
Mailing Address:                     NIST
                                Materials (223), A215
                                Gaithersburg, MD  20899
Telephone:                           (301) 975-5799
Fax Number:                     (301) 990-8729
E-Mail Address:                      mark@pruffle.nist.gov

Technical Description:

The driving force for the consolidation and densification of ceramic powders during sintering is
the difference between the energy of the free surfaces which are eliminated and the energy of the
grain boundaries which form.  While the modelling of microstructure development during
sintering of ceramics has generally assumed that all interfacial energies are isotropic,
measurements of the interfacial energies have shown that most materials are anisotropic. 
Anisotropy of these interfacial energies will lead to differences in the local rate of densification,
shape of pores and the location of pores (either attached to or separated from grain boundaries). 
When pore separation occurs, shrinkage of the pores effectively stops and a limiting density is
reached.  large differences in mobility of specific grain boundaries can result in a highly textured
microstructure consisting of elongate grains.  If a liquid phase is present, not all grain boundaries
will be wetted depending on the local energy balance.

Technical Objectives:

The understanding of the effect of interfacial energy anisotrophy on the microstructure evolution
of ceramics.  The microstructural features of concern are the pore location, the distribution of
liquid phases and the crystallographic texture.

Outcomes:

We have determinated the equilibrium (Wulff) shape of Al203 in air.  The resultant shape was
compared with the shapes predicted from theoretical calculations of the surface energy, and large
discrepancies were found.

The conditions for wetting of low angle grain boundaries in Al203 by anorthrite glass have been
measured.  It was shown that not only is the degree of grain boundary misorientation important,
but the normal to the boundary plane also controls the wetting.

A technique for measuring individual grain orientations from surface facetting using AFM
measurements has been developed.  This technique uses the observed faceting and the Wulff
shape to determine the orientation and is being calibrated using orientations determined by
electron backscatter patterns of the same grains.

Outputs:

Technical papers:

"Stability and Surface Energy of Wetted Grain Boundaries in Aluminum Oxide", D-Y. Kim, S.M.
Wiederhorn, B.J. Hockey, C.A. Handwerker and J.E. Blendell, J. Amer. Ceram. Soc. 77(2)444-
53(1994).

"Texture Measurement of Sintered Alumina using the March-Dollase Function", J.P. Cline, M.D.
Vaudin, J.E. Blendell, C.A. Handwerker, R. Jiggetts, K.J. Bowman and N. Mendendorp,
Advances in X-ray Analysis, 37, J.V. Gilfrich, ed., Plenum Press, New York, 1994, 473.

"The Equilibrium Shape of Internal Cavities in Sapphire" J-H. Choi, D-Y. Kim, B.J. Hockey,
S.M. Wiederhorn, C.A. Handwerker, J.E. Blendell, W.C. Carter and A.R. Roosen, submitted to
J. Amer. Ceram. Soc., Jan 1996.

Impact:

Allow materials development to use the anisotropy of materials to enhance/improve the properties
in specific orientations, and to use changes in anisotropy (via doping) to control microstructure. 
Development of measurement techniques for easily determining the surface energy anisotropy.

PROJECT TITLE:  Broad Based Manufacturing

PROGRAM TITLE:  Ceramic Processing

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Malghan, S. G.
Mailing Address:           NIST
                      Materials (223), A207
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6119
Fax Number:           (301) 990-8729
E-Mail Address:            malghan@micf.nist.gov

Other NIST Principal investigator(s):  Hackley, V. A.
Mailing Address:                   NIST
                              Materials (223), A203
                              Gaithersburg, MD  20899
Telephone:                         (301) 975-5790
Fax Number:                   (301) 990-8729

Principal Investigator(s) Outside NIST:  Fanelli, T.
Mailing Address:                      Allied-Signal Corp
                                 Morristown, NJ

                                 Pollinger, J.
Mailing Address:                      Allied-Signal Corp
                                 Los Angeles, CA

Technical Description:

Silicon nitride components for heat engines are under development in industry to take advantage
of their superior wear resistance and high temperature strength.  Shaping of these parts in a rapid
manner with reproducible properties is necessary to allow production at a competitive cost which
allow broad commercialization.  This project addresses fundamental measurements required for
the development of aqueous injection molding, an ATP funded program.

Technical Objectives:

This project is focused on the development of methods of characterizing the green body structure
of parts made by aqueous injection molding and development of means of measuring the
dispersion and other properties of dense suspensions of silicon nitride.

Outcomes:

This research is expected to enhance industry's capability to fabricate cost effect silicon nitride
automotive components as well as industrial gas turbine hardware.  This will be accomplished
by the development of measurement methods such as electro-acoustic sonic amplitude
measurement techniques which can be implemented by industry to control process materials.

                     ELECTRONIC AND PHOTONIC CERAMICS

The objectives of the Electronic and Photonic Ceramics program are to provide data,
measurement methods, standards and reference materials, models, and understanding of  the
fundamental aspects of processing, structure, properties, and performance of electronic and
photonic materials.  The program supports generic technologies in bulk and thin-film ceramics
in order to foster their efficient and economical use as electronic and/or photonic materials.  The
research addresses the science base underlying advanced electronic/photonic materials
technologies together with associated measurement methodology.

The principal activities of the program are directed toward materials for electronic and photonic
technology related to data processing, storage, display, and transmission.  Four aspects of this
technology being addressed are modulator materials, storage-media materials, materials for
microwave transmission, and material for compact, short-wavelength radiation sources to increase
storage density.  In the area of modulator materials, MSEL scientists are evaluating film
processing methods and their relationship to properties such as electro-optic modulator
characteristics.  In the area of storage-media materials, scientists are addressing issues in thin-film
and bulk ferroelectric and photorefractive materials, in which the storage method involves either
modification of the refractive and absorptive properties upon exposure to optical radiation or
changes in material polarization by application of an electric field.  Ferroelectric oxides are being
studied because they possess large spontaneous polarizations, large electro-optic coefficients and
large photorefractive effects.  In the area of data transmission, phase diagrams important for the
production of  low-loss, thermally stable ceramics for fabrication of components to be used in
microwave communication devices are being developed..

In the area of materials for short-wavelength sources, our studies are directed toward crystalline
materials with large bandgaps,e.g.  gallium nitride, aluminum nitride, and zinc selenide, because
a large bandgap is required if a material is to emit radiation at short wavelengths.  A key issue
is the characterization of defects at very low concentration levels.  Collaborations have been
established for the purpose of providing data that will allow manufacturers to improve the quality
of the materials.

For further information on the Electronic and Photonic Ceramics Program, please contact Grady
White at 301-975-5752 or e-mail requests to Spruce@enh.nist.gov.

PROJECT TITLE:  Molecular Chemical Synthesis of a Microwave Ferrite            

PROGRAM TITLE:  Electronic and Photonic Ceramics

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Ritter, Joseph J. 
Mailing Address:          NIST 
                     Materials (223), A256
                     Gaithersburg MD 20899
Telephone:                (301) 975-6106
Fax Number:          (301) 990-8729

Project Description:

This project focusses on the use of aqueous solution chemistry to synthesize a model microwave
ferrite material, nickel iron oxide, in fine-powder form.

Technical Objective:

The research is directed towards assisting industry to generate microwave ferrite materials
economically from commonly available chemicals.

Outcomes:

The model synthesis system developed in this work is expected to have substantial generality for
applications in the production of a variety of other, relevant microwave ferrites.  

Accomplishments:

Two model systems for the synthesis of precursors to the technologically important ferrite, nickel
iron oxide, NiFe2O4, were explored.  One used tartaric acid to form complexes with iron and
nickel ions, while the second used tartaric acid admixed with ethylene glycol. 
Spectrophotometric studies of the metal-organo complexes in solution suggested an optimum
molar ratio of metal ion-to-complexing agent of 1 : 1.  

The evolution of NiFe2O4 from the precursors as a function of temperature up to 1000 C was
explored.  During this part of the study it was noted that the addition of ethylene glycol to the
metal ion-tartaric acid complexes provided certain  advantages.  These included a lower NiFe2O4
crystallization temperature, substantially smaller particles, and minimal amounts of unreacted
hematite remaining in the final product.  

In both systems, typical yields of the product were (93 to 95)% of theoretical.  Particle sizes were
typically 1m for the tartaric acid process, and 0.5m for the tartaric acid-glycol process.  

Output:

Technical Paper: 

"Synthesis of NiFe2O4 by a Metal-Organo Complex Method",   Joseph J. Ritter and Pichai
Maruthamuthu, accepted for publication by the Journal of Materials Synthesis and Processing. 
 
Impact:

The work supplies guidelines for a simple, economically viable, chemical approach to the
production of microwave ferrites. 

PROJECT TITLE:  Phase Equilibria Studies of Dielectric Oxides for Wireless Communications

PROGRAM TITLE:  Electronic and Photonic Ceramics

Principal investigator(s):    

NIST Staff:
Designated Project Leader:  Vanderah, Terrell A.
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD   20899
Telephone:                 (301) 975-5785
Fax Number:           (301) 990 8729
E-mail:               terrell@credit.nist.gov

Other NIST Principal investigator(s):  Roth, Robert S.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD   20899
Telephone:                          (301) 975-6116
Fax Number:                    (301) 990 8729

                                Wong-Ng, Winnie
Mailing Address:                     NIST
                                Materials (223), A256
                                Gaithersburg, MD   20899
Telephone:                           (301) 975-5791
Fax Number:                     (301) 990 8729

                                Drews, Andrew R.
Mailing Address:                     NIST
                                Materials (223), A256
                                Gaithersburg, MD   20899
Telephone:                           (301) 975-5786
Fax Number:                     (301) 990 8729

Project Description:

Dielectric ceramics are used to fabricate a variety of components in cellular communications
circuits that store, filter, and/or transfer electromagnetic energy with minimal loss (e.g., resonators
(bandpass filters), circulators).  The required properties for the ceramic materials include high
dielectric constant, minimal dielectric loss (which precludes the use of ferroelectric oxides), and
essentially zero temperature dependence of dielectric properties.  Knowledge of phase equilibria
relations is important owing to the additive nature of dielectric properties; e.g. practically all
ceramic components are processed as mixtures to achieve compensation and a net overall zero
temperature coefficient.  Thus, identification and characterization of phases in equilibrium with
the dielectric ceramic are essential in order to process ceramic components that meet current
standards of tightly controlled dielectric constant (0.25%), low dielectric loss, and temperature
coefficients near zero (4 ppm/C).  Furthermore, in carrying out the determination of phase
relations in a system, the existence of previously unknown compounds with potentially useful
properties may be elucidated.  The approach taken by the phase equilibria group focusses on the
experimental determination of ternary (or higher) oxide systems containing one or more
components that are known to give rise to materials with useful properties as dielectric ceramics
for microwave communications.  Efforts are directed to synthesis, structural characterization, and
characterization of dielectric properties.

Technical Objectives: 

To determine the phase relationships in ceramic materials used in Wireless communication
devices.

Accomplishments:

  The BaO-Fe2O3-TiO2 system was chosen for determination to elucidate the phase relations
between a magnetic component and the existing Ba-Ti-O microwave ceramics.  High-dielectric-
constant ceramic magnets are fundamental to a wide variety of communication applications as
circulators and isolators.  The BaO-Fe2O3-TiO2 ternary phase diagram has been investigated at
(1250 to 1270) C in air.  X-ray diffraction studies of approximately 150 polycrystalline
specimens at room temperature confirmed the existence of sixteen ternary compounds.  Two of
these compounds, BaFe4Ti2O11 and Ba12Fe28Ti15O84, have been previously reported, four were
found to be isostructural with known chemically similar compounds, and ten apparently adopt
new structure-types.  The crystal structures of five of the new ternary phases are briefly
described.  The oxidation state of iron found in this study is similar to that reported for a study
of the BaO-Fe2O3-SnO2 system in air at 1200C.  No indications of reduction of Fe3+ to Fe2+ were
observed; however, oxidation to Fe4+ was clearly indicated in an extensive solid solution
BaTi1-xFexO3-z, x=0.06 to 0.84, with the hexagonal BaTiO3 structure.  Substantial solid solution
regions were also found for the hollandite-type structure (BaxFe2xTi8-2xO16, x=1.07 to 1.33), and
for TiO2 dissolved in the BaFe12O19 structure (end member BaFe10.8Ti0.9O19).  The complexity of
the BaO-Fe2O3-TiO2 system is attributed to the coordinative versatility of Fe3+ in a close-packed
O/Ba-O matrix and the resulting opportunity to form a wide variety of layered structures with
different stacking sequences and distortions from ideal packing.

The SrO-TiO2-Nb2O5 system is of possible importance in the formation of useful compositions
with high dielectric constant.  SrTiO3, with the cubic perovskite structure, has a very high
dielectric constant, but unfortunately it has a very negative temperature coefficient of resonant
frequency (Tf).  It has been found that cubic SrTiO3 is in equilibrium with Sr6Ti2Nb8O30 or some
solid solution of similar composition with the tetragonal tungsten bronze (KxWO3) type structure. 
The Tf of the phases in this ternary system are not known.  In addition, there are several possible
phases of hexagonal structure related to Sr5Nb4O15 which may exist on the join between SrTiO3
and Sr5Nb4O15.  The phase Sr6TiNb4O18 has been synthesized but "Sr8Ti3Nb4O24" has not been
isolated, although the phase Ba8Ti3Nb4O24 is known.  Instead, the new phase Sr7Ti2Nb4O21 was
found to exist.  Further studies will be continued in the ternary system to understand the
compatibility relations, and the dielectric constants and Tf data will be  evaluated.

Outputs:

Technical Papers:

"Magnetic Dielectric Oxides:  Subsolidus Phase Relations in the BaO-Fe2O3-TiO2 System", T.A.
Vanderah, J.M. Loezos, and R.S. Roth.

"Preparation, Crystal Structure, Dielectric Properties, and Magnetic Behavior of Ba2Fe2Ti4O13",
T.A. Vanderah, Q. Huang, W. Wong-Ng, B.C. Chakoumakos, R.B. Goldfarb, R.G. Geyer, J.
Baker-Jarvis, R.S. Roth, and A. Santoro.

"Preparation and Crystal Structure of Sr5TiNbO17", A.R. Drews, W. Wong-Ng, R.S. Roth, and
T.A. Vanderah.

PROJECT TITLE:  Ferroelectric Oxide Thin Films for Photonics

PROGRAM TITLE:  Electronic and Photonic Ceramics

Principal Investigator:  

NIST Staff:
Designated Project Leader:  Kaiser, Debra L. 
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD  20899
Telephone:                 (301) 975-6759
FAX Number:           (301) 990-8729
E-mail Address:            dkaiser@enh.nist.gov

Other NIST Principal investigator(s):  Rotter, Lawrence D.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD  20899
Telephone:                          (301) 975-6603
FAX Number:                    (301) 990-8729
E-mail Address:                     rotter@enh.nist.gov

Technical Description:

This project involves a study of the complex relationships between thin film deposition,
microstructural features and electro-optical properties of barium titanate thin films deposited by
by metalorganic chemical vapor deposition (MOCVD).  Novel electro-optical measurement
methodology is under development to determine the crystallographic orientation and polarization
state of the thin films.

Technical Objective:

The objectives are to address key scientific issues vital to the advancement of ferroelectric oxide-
based thin film photonic devices for information technology and communications industries and
to develop appropriate measurement methodology as needed to study these issues.

Outcome:

The outcome will be the establishment of microstructural characterization and electro-optical
measurement techniques needed to develop the processing/structure/property relationships of
importance for ferroelectric oxide thin films for photonic devices.

Accomplishments:

A thermal MOCVD system, designed and built at NIST for ferroelectric oxide film deposition,
has been modified to include an oxygen preheater and metalorganic bubblers with improved
temperature control.  These modifications have improved the reproducibility of the deposition
experiments.  A set of processing conditions has been established for the deposition of epitaxial
BaTiO3 films on single crystal MgO and KTaO3 substrates in the modified system.  

X-ray diffraction studies showed that the BaTiO3 films could contain either epitaxial,
polycrystalline or amorphous material, or a combination of epitaxial and amorphous or
polycrystalline and amorphous phases.  Second harmonic generation (SHG) in the films was
measured as a function of the incidence angle of the fundamental beam as well as the direction
of polarization of the fundamental beam.  The SHG data on the as-grown films were not relatable
to either the microstructure or the crystallographic orientation of the BaTiO3 grains.  Thus, SHG
was shown not to be a viable technique for determining the orientation of BaTiO3 thin films,
despite contrary reports in the literature.

Outputs:

Technical Papers:

"Epitaxial growth of BaTiO3 thin films at 600 C by metalorganic chemical vapor deposition",
D. L. Kaiser, M. D. Vaudin, L. D. Rotter, Z. L. Wang, J. P. Cline, C. -S Hwang, R. B.
Marinenko, and J. G. Gillen, Appl. Phys. Lett 66, 2801 (1995).

PROJECT TITLE:  Defect Studies in Photonic Materials

PROGRAM TITLE:  Electronic and Photonic Materials

Principal investigator(s): 

NIST Staff:
Designated Project Leader:  Steiner, Bruce
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5977
Fax Number:           (301) 990-8729
E-mail address:            bruce.steiner@nist.gov

Other NIST Principal investigator(s):  Fogarty, Gerard
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5636
Fax Number:                    (301) 990-8729
E-mail address:                     gerard.fogarty@micf.nist.gov

                               Bouldin, Charles
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-2046
Fax Number:                    (301) 990-8729

Principal investigator(s) outside NIST:  Roshko, Alexana
Mailing Address:                     EEEL

                                Garrett, Mark
                                Uhrin, Robert
                                Martin, John
Mailing Address:                     Deltronic Crystal Industries
                                Dover, NJ 07801
Telephone:                           (201) 361-2222                   
        
                                Ming, John
Mailing Address:                     Rockwell Science Center
                                Thousand Oaks, CA
Telephone:                           (805) 373-4193
                                Wong, K. K.
Mailing Address:                     Litton Industries
Telephone:                           (818)715-4704
     
Technical Description:

This project provides:1) observation, analysis, and evaluation of residual disorder in high quality
optoelectronic/photonic single crystals; 2)  determination of the effects of the various types of
disorder on optoelectronic/photonic crystal properties and performance; and, 3) through collabo-

ration with crystal growers and optoelectronic/photonic device fabricators, improved control of
those particular types of crystalline disorder that most affect optoelectronic/photonic device
performance.

Technical Objectives:

The objective of this project is the development and production of materials suitable for optical
computing, optical communications, and optical information processing.  This objective is
achieved through the exploitation of 1) special high sensitivity measurement facilities and 2)
photonic material structural interpretive expertise, neither of which is available in the private
sector.

Outcomes:

Four outcomes are anticipated:  1) improved scientific and practical understanding of optical
interactions in photonic crystals, 2) reliable structural requirements for high quality crystals
capable of producing world-class devices for optical computing, other optical information
processing, optical communications, and optical information storage; 3)  improved growth of
these crystals in the private sector, following establishment of the relevant structural
requirements; and  4) quantitative verification that the structural goals have been met.  

Accomplishments:

Through collaboration with Deltronic Crystal Industries and Tufts University we  facilitated the
commercial production of superior barium titanate and strontium barium niobate single crystals
designed for use in holographic devices for high capacity information processing and storage. 
This accomplishment required, in turn the development of the two new capabilities: 1) the first
direct observation of the storage of photorefractive information in these crystals and 2) complete
mathematical models, used successfully in the detailed interpretation of the novel x-ray
diffraction images obtained.  

Through collaboration with NZ Technologies and Tufts University we demonstrated attainment
of the first high quality epitaxy of a photorefractive oxide layers on an oxide substrate, a process
with great technological potential for new forms of optical information processing.  In doing so,
we showed that the substrates used at this point  will severely limit the performance of devices
made from these layered devices in a manner that is in addition to any further limitations that
are introduced through subsequent processing.  

Through collaboration with Deltronic Crystal Industries and the Naval Research Laboratory we
have shown that heavy doping of lithium niobate for improved photorefractive sensitivity and the
periodic poling of undoped material both are strongly correlated with the prevalent defect
structure in this material.

In collaboration with other NIST scientists we are developing an understanding of the generation
of defects as III-V layers are deposited on high quality III-V substrates.  Devices fabricated in
this manner form the basis for novel optoelectronic/photonic approaches to information
processing.

Outputs:

Some of the most important outputs of this project are the improved optoelectronic/photonic
crystals that are likely to form the basis for novel information processing and storage technology. 
Other outputs are the information that will be used by others in the scientific and technical
community to improve the performance of these and related materials and the understanding on
which still further enhancement of performance can be based.

Technical Papers:

L.D. Zhu, J. Zhao, F. Wang, Peter E. Norris, G. D. Fogarty, B. Steiner, P. Lu, B. Kear, S.B.
Kang, B. Gallois, M. Sinclair, D. Dimos, and M. Cronin-Golomb, Epitaxial electro-optical
SrxBa1-xNb2O6 films by single-source plasma-enhanced metalorganic chemical vapor deposition, 
Appl. Phys. Lett. 67, 1836-1838 (1995).
 
Bruce Steiner, L.E. Levine, Margaret Brown, and David Larson, Residual disorder in low
pressure, low thermal gradient liquid encapsulated Czochralski gallium arsenide observed in high
resolution synchrotron diffraction imaging, J. Crystal Growth, in press (1996)

G. Fogarty, B.Steiner, M. Cronin-Golomb, U. Laor, M. H. Garrett, J. Martin, and R. Uhrin,  Anti-
Parallel Ferroelectric Domains in Photorefractive Barium Titanate and Strontium Barium
Niobate Observed by High-Resolution X-Ray Diffraction Imaging",  JOSA B, in press (1996).

G. Fogarty, B. Steiner, M. Cronin-Golomb, R Uhrin, and J. Martin, High Resolution X-Ray
Diffraction Imaging of Anti-Parallel Ferroelectric Domains in Barium Titanate and Strontium
Barium Niobate",   Proc. Photorefractive Materials, Effects, and Devices Topical Meeting, Estes
Park, 9 (1995).

PROJECT TITLE:  Growth and characterization of blue/green laser materials

PROGRAM TITLE:  Electronic and Photonic materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Robins, Lawrence H.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5263
Fax number:           (301) 990-8729
E-mail address:            lrobins@enh.nist.gov

Principal Investigator(s) outside NIST:  Wickenden, Dennis
Mailing Address:                      Johns Hopkins University Applied Physics Lab
                                 Johns Hopkins Road
                                 Laurel, MD 20723-6099
Telephone:                            (301) 953-6249
Fax number:                      (301) 953-6904

Principal Investigator outside NIST:  Cantwell, Gene
Mailing Address:                   Eagle-Picher Research Labs
                              200 9th Ave., N.E.
                              Miami, OK 74354
Telephone:                         (918) 542-1801
Fax number:                   (918) 542-3223

Technical Objectives:

This project is designed to assist industry with the development of blue/green semiconductor
lasers, and other short-wavelength optical emitters, by providing data about the optical and
optoelectronic properties of the materials that form the basis for these devices.

Technical Description:

Researchers who are growing wide-bandgap semiconductor materials need feedback about how
process parameters affect the properties of their materials that are most relevant to the intended
applications.  In this project, several techniques of optical emission spectroscopy are used to
investigate the properties of wide-bandgap semiconductor materials as a function of process
parameters.  The correlation of the observed properties with material structure and composition
is examined in order to provide a more fundamental understanding of the data.  The lasers will
be used in high-density optical data storage systems; the non-laser blue/green emitters will be
used in compact full-color displays (e.g., notebook computers, instrument panels).

Accomplishments:

Several optical emission spectroscopy systems have been set up to enable the experimental
measurements needed for this project.  These include: laser photoluminescence (PL) and
photoluminescence excitation spectroscopy; time-resolved PL with a pulsed-laser source; and
cathodoluminescence (CL)  imaging and spectroscopy in a scanning electron microscope.  Sample
cooling to liquid-helium temperature, needed to observe spectral features that are not detectable
at room temperature, is a capability of both the PL and CL experiments.

Collaborations have been established with researchers outside NIST who are producing
state-of-the-art materials.  Dennis Wickenden at Johns Hopkins University Applied Physics
Laboratory is growing thin films of Aluminum Gallium Nitride (AlGaN) by metalorganic
chemical vapor deposition.  These films, which give rise to optical emission from the visible to
the deep UV, are intended for UV lasers and visible display devices.  Gene Cantwell at
Eagle-Picher Research is growing Zinc Selenide (ZnSe) wafers as substrates for blue/green
optical emitters.  Experiments performed on both AlGaN and ZnSe specimens have demonstrated
that the selected experimental techniques are applicable to these materials and provide significant
information.  Key experimental results are summarized below.

The PL and CL spectra of AlxGa1-x films (from Johns Hopkins Applied Physics Laboratory) were
investigated as a function of composition (x), temperature, and type of excitation.  The band-edge
emission energy was found to depend linearly on x, as expected; the width of the band-edge
emission peak, an indicator of residual stress, was found to increase slightly with x; and bound-
exciton emission was associated with defects localized near the film-substrate interface.  These
results will assist growers in optimizing deposition conditions for the films.
Spectrally resolved CL images of AlxGa1-x films (from JHAPL) were observed at low
temperature and room temperature.  Images of the mixed composition films (Al content x>0)
showed networks of bright lines along directions of high crystal symmetry.  These bright lines
may be due to microcracks that arise from thermal expansion mismatch between the film and
substrate.  Images of some of the lower Al content films showed bright circular rings that may
be due to screw dislocations.  The extended defects identified by CL imaging may affect
performance of the films in light-emitting and other photonic applications.
The variation of the low-temperature CL spectra of a ZnSe single-crystal boule was examined
as a function of distance from the bottom of the boule.  Peak shifts of some of the narrow
emission peaks suggest a stress that varies with distance along the growth direction.  An emission
peak ascribed to dislocations was observed to be localized within the first millimeter from the
bottom of the boule.  Mapping the spatial distribution of stress and defects in the boule will help
crystal growers produce material with lower stress and defect density.  This is important for
applications of the crystals as substrates for wide-bandgap LEDs and laser diodes.

PROJECT TITLE:  Pulsed Laser Deposition (PLD) of Ceramic Thin Films

PROGRAM TITLE:  Electronic and Photonic Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Hastie, John. W.
Mailing Address:           NIST
                      Materials (223), A215
                      Gaithersburg, MD  20899
Telephone:                 (301) 975-5754
FAX Number:           (301) 990-8729
E-mail Address:            jwhastie@enh.nist.gov

Other NIST Principal investigator(s):  Bonnell, David W.
Mailing Address:                    NIST
                               Materials (223), A215
                               Gaithersburg, MD  20899
Telephone:                          (301) 975-5755
FAX Number:                    (301) 990-8729
E-mail Address:                     bonnell@enh.nist.gov

                               Paul, Albert J.
Mailing Address:                    NIST
                               Materials (223), A215
                               Gaithersburg, MD  20899
Telephone:                          (301) 975-6004
FAX Number:                    (301) 990-8729
E-mail Address:                     ajpaul@enh.nist.gov

                               Schenck, Peter K.
Mailing Address:                    NIST
                               Materials (223), A215
                               Gaithersburg, MD  20899
Telephone:                          (301) 975-5758
FAX Number:                    (301) 990-8729
E-mail Address:                     pkschenck@enh.nist.gov

Technical Description:

This project is intended to develop measurement capabilities to monitor, in situ, processing of
thin films using PLD.  This information is intended to allow industry in-process monitoring
during film deposition and control of resultant thin film properties.

Technical Objective:

The objective of the work is to relate processing parameters to final film properties, thereby
reducing the need for time consuming empirical derivation of optimal processing conditions and
extensive post processing analysis currently used in industry.

Outcome:

The outcome of this work will be the development of in situ characterization techniques to allow
real-time analysis of the details of the deposition process during PLD.  The time dependent
deposition parameters will be related to resultant film properties.

Accomplishments:

New or improved diagnostic methods were developed for real-time observations of key
intermediate species during the PLD of electronic ceramic thin films.  These methods were based
on optical imaging and spectroscopy, coupled with mass spectrometry and their development was
enhanced by chemical-dynamic model simulations of the PLD process.  Improvements in process
understanding, optimization and control are under development as a result of these advances.

Outputs:

Tangible outputs resulting from this project included seven invited talks, given at national and
international symposia on thin film processing, together with eight research papers.

Technical papers:

"Imaging and Modeling of Pulsed Laser Ablation Plumes in Thin Film Deposition", P. K.
Schenck, J. W. Hastie, A. J. Paul, and D. W. Bonnell, Optical Eng., in press, 1995; also
Proceedings, SPIE Symposium, Laser-Induced Thin Film Processing, San Jose, Ca., Feb. 1, 1995.

"High Temperature Chemistry in Laser Generated Plumes", J. W. Hastie, D. W. Bonnell, A. J.
Paul, J. Yeheskel, and P. K. Schenck, High Temp. Science and Materials. 33, 135 (1995).

PROJECT TITLE:  Damage Accumulation in Actuator Materials

PROGRAM TITLE:  Electronic and Photonic Ceramics

Principal investigator(s):

NIST Staff:
Designated Project Leader:  White, Grady S.
Mailing Address:           NIST
                      Materials (223), A215
                      Gaithersburg, MD  10899
Telephone:                 (301) 975-5752
FAX Number:           (301) 990-8729
E-mail address:            spruce@enh.nist.gov

Other NIST Principal investigator(s):  Hill, Michael D.
Mailing Address:                    NIST
                               Materials (223), A215
                               Gaithersburg, MD  20899
Telephone:                          (301) 975-5601
FAX Number:                    (301) 990-8729
E-mail address:

Technical Description:

Actuator materials inherently undergo cyclic loading conditions which can lead to mechanical and
electronic degradation.  The degradation mechanisms and the interactions between mechanical,
electronic, and thermal behavior in the material must be understood for reliability assessment and
lifetime predictions to be meaningful.

Technical Objective:

This project is intended to identify failure mechanisms in cyclically loaded actuator materials,
so that meaningful reliability estimates can be made for smart materials systems.  The
interactions between stress and piezoelectric properties, the generation of microcracks, and the
effects of thermal excursions are all critical elements under investigation.

Outcome:

The outcome of this work will be an understanding of failure processes in lead zirconate titanate
(PZT) actuator material and, thereby, tools to allow lifetime prediction for these materials used
in hostile or critical applications.

Accomplishments:

We have determined that microcrack formation occurs during all loading conditions, but that it
appears to be in competition with domain wall motion.  Similarly, we have determined that the
onset of the reported anisotropy in macrocrack lengths, parallel and perpendicular to the poling
direction, corresponds to a discrete degree of polarization which, in turn, is correlated to the onset
on non-180 domain wall motion.  Finally, a decrease in microcrack density at T  180C from
that observed at RT with simultaneous increase in macrocrack growth appears to be tied directly
to non-180 domain wall motion and concomitant reduction in residual stresses.

Output:

Technical Papers:

The output of this work, during the past year, includes the following technical papers:

M. D. Hill, G. S. White, and I. K. Lloyd, "An Examination of Factors Influencing Crack
Extension in PZT During Cyclic Loading," submitted to the Proceedings of the 6th Symposium
on Fracture Mechanics of Ceramics," Karlsruhe, Germany (7/17-20/95).

M. D. Hill, G. S. White, and I. K. Lloyd, "Cyclic Damage in PZT," accepted by the J. Am.
Ceram. Soc. (1995).
                         EVALUATED MATERIALS DATA

The objective of the Data Technologies program is to develop and facilitate the use of evaluated
databases for the materials science and engineering communities.  Both research- and application-
directed organizations require readily available evaluated data to take advantage of the large
volume of materials information developed on public and private sponsored programs.  This
information, particularly numeric data, is available in an ever increasing number of publications
published worldwide.  The necessity to consolidate and allow rapid comparison of properties for
product design and process development underlies the database projects.

Evaluated Data projects are conducted in cooperation with the NIST Standard Reference Data
Program Office and include compilation and evaluation of numeric data as well as recently
initiated efforts directed at more effective distribution and use of data.

Database projects in MSEL include:

    Phase Diagrams for Ceramists (PDFC), conducted in cooperation with the American
     Ceramics Society;

    the Structural Ceramics Database (SCD), a compilation of evaluated mechanical and
     thermal data for nitrides, carbides, and oxides of interest to engineers and designers;

    a ceramic machinability database, coordinated with the Ceramic Machining Research
     Program;

    a high Tc superconductivity database developed in cooperation with the Japanese Agency
     for Industrial Science and Technology (see superconductivity);

    development and implementation of the STEP protocol for the exchange of materials data,
     under the auspices of the ISO 10313 activity;

    the NACE/NIST Corrosion Performance Database developed to provide a means to select
     structural alloys for corrosive applications; and

    the Crystal Data Center which provides fundamental crystallographic data on inorganic
     materials.

These projects are developed with the cooperation of the materials community and complement
various research programs.

For additional information on the Evaluated Materials Data Program, contact S. J. Dapkunas at
301-975-6119 or e-mail to Dapkunas@micf.nist.gov.

PROJECT TITLE: Phase Diagrams for Ceramists 

PROGRAM TITLE: Evaluated Materials Data

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Freiman, Stephen W.
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6119
Fax Number:           (301) 990-8729
E-mail address:            freiman@micf.nist.gov

Other NIST Principal investigator(s):  Begley, Edwin F.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6118
Fax Number:                    (301) 990-8729
E-mail address:                     begley@enh.nist.gov

                               Clevinger, M.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6109
Fax Number:                    (301) 990-8729

Principal Investigator(s) outside NIST:  Cedeno, C. L.
Mailing Address:                     NIST, American Ceramic Society
                                Materials (223), A256
                                Gaithersburg, MD  20899
                                (301)  975-6109
                                (301) 990-8729

                                Green, T. 
Mailing Address:                     NIST, American Ceramic Society
                                Materials (223), A256
                                Gaithersburg, MD 20899
                                (301) 975-6112
                                (301) 990-8729

                              Hill, K. 
Mailing Address:                   NIST, American Ceramic Society
                              Materials (223), A256
                              Gaithersburg, MD  20899
                              (301)  975-6111
                              (301) 990-8729

                                   Swanson, N.
Mailing Address:                   NIST, American Ceramic Society
                              Materials (223), A256
                              Gaithersburg, MD  20899
                              (301)  975-6117
                              (301) 990-8729

                              Hayward, E.              
Mailing Address:                   NIST, American Ceramic Society
                              Materials (223), A256
                              Gaithersburg, MD  20899
                              (301)  975-6117
                              (301) 990-8729

                              Roth, Robert
                              The Viper Group
Mailing Address:                   804 Amber Tree Court
                              Gaithersburg, MD 20878
                              (208) 787- 2939
                              (301) 990-2529

                              Ondik, Helen
Mailing Address:                   2737 Devonshire Place, NW, #317
                              Washington, DC 20008

Technical Description:

The Phase Equilibria Program sponsored jointly by the American Ceramic Society (ACerS) and
NIST was formally established in 1982.  The purpose of this cooperative effort is to provide
qualified, critically evaluated data on thousands of chemical systems relating to ceramic materials
research and processing, as well as a critical database to serve the ceramic community.   This
information serves as an objective reference for important processing data.  Approximately $1.8M
was raised by the ACerS from industry for the support of the program.  The  outputs of the
program include printed volumes of evaluated phase programs as well as software packages
containing bibliographic and graphics phase diagram data.

More recently, two stages have been planned for the development of an expert system that will
guide the customer on the use and determination of phase diagrams.  The first stage concentrates
on developing software that will enable individuals to learn or review how to interpret and use
unary, binary, ternary and quaternary phase equilibria diagrams.  The second stage will
concentrate on the implementation of an application that will provide instructions how one
develops phase diagrams.  The goal of this latter stage is to capture, using digital motion video
and audio, the relevant expertise of scientists whose research focuses on the determination of
phase-equilibria diagrams.  In this way, the expertise, particularly the laboratory techniques and
insights which do not appear in technical publications, would be preserved for future generations
and, furthermore, would be widely distributable.

The software will make extensive use of digital video technology which allows motion video and
audio signals to be digitally compressed and integrated with tradition software.  Motion video
and audio allow the user to visualize technical content to an extent not possible with a textbook. 
This would be particularly helpful in presenting crystallization sequences in ternary systems.  

Technical Objectives:

The primary goal of this project is to deliver critically evaluated phase equilibria data to
industrial and academic customers. A second goal is the development of innovative, distributable,
multimedia software incorporating interactive digital video technology to assist in the
interpretation and use of these diagrams.  This Equilibria Expert (EE) will complement phase
diagram work that has been part of almost sixty years of cooperation between NIST and the
American Ceramic Society.

Outputs:

Evaluated data:

Volume 11, focusing on oxides, particularly those of interest for electronic applications, was
completed and published in 1995.  This compilation contains 685 commentaries and 871
diagrams, which covers the period up to 1988.  The 1995 Cumulative Index was also published
which contains the author and chemical systems indexes for Volumes I-XI of Phase Equilibria
Diagrams, Annuals '91-'93, and the High Tc Superconductor Monograph.

Version 2.0 of the CD-ROM Database for Phase Diagrams for Ceramists was completed, and is
being marketed through the ACerS.  This database contains over 10,000 diagrams, including
those previously published in Version 1.0.  The Database allows search capabilities of
bibliographic information as well as powerful graphics capabilities with regards to the diagrams.

Volume 12, focusing on oxides, was worked on in 1995 and will have an early 1996 publication
date.  This volume has 443 commentaries and approximately 800 diagrams.   Also planned for
publication in early 1996 is a  new cumulative index which will contain the author and chemical
systems indexes for Volumes I-XII of Phase Equilibria Diagrams, Annuals '91-'93, and the High
Tc Superconductor Monograph.

Technical papers:
     
"A Multimedia Tutorial on Phase Equilibria Diagrams," E.F. Begley and C.G. Lindsay, Bulletin
of the American Ceramic Society, Vol. 72, No.12, pp. 103-104, December 1993.

"Multimedia Computing in Materials Science and Engineering," E.F. Begley and C.P. Sturrock,
to be published in the Journal of Materials Engineering and Performance.

PROJECT TITLE:  Structural Ceramics Database

PROGRAM TITLE:  Evaluated Materials Data

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Munro, Ronald G.
Mailing Address:              NIST
                         Materials (223), A256
                         Gaithersburg, MD 20899
Telephone:                    (301) 975-6127
Fax number:              (301) 990-8729
E-mail Address::              munro_rg@enh.nist.gov

Other NIST Principal investigator(s):  Begley, Edwin F.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6118
Fax number:                    (301) 990-8729
E-mail Address::                    begley@enh.nist.gov

                               Harris, Joyce F.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6045
Fax number:                    (301) 990-8729
E-mail Address::                    jharris@enh.nist.gov

Technical Description:

This project is designed to facilitate advances in materials science and technology by providing
evaluated thermal, mechanical, and corrosion property data for the broad class of materials
variously called advanced technical ceramics, structural ceramics, engineered ceramics, or fine
ceramics.

Technical Objectives:

The objective of this project is to provide a reliable knowledge base for understanding material
property and performance relationships.  Use of the technically evaluated data enables industry
to save substantial time and effort in the selection of materials.

Outcomes:

Several significant results are expected from this project:  (1) a comprehensive set of evaluated
data; (2) a software interface to the database; (3) standards and methodology for data evaluation;
and (4) relations and models for properties and performance characteristics.

Accomplishments:

The Structural Ceramics Database (SCD) is distributed by the NIST Standard Reference Data
Program as NIST Standard Reference Database Number 30.  Currently, version 2 is being
distributed, and the preparations for version 3 are well underway.

An agreement has been established with the Russian Research Center for Standardization,
Information, and Certification of Materials to obtain property data from Russian language
sources, and an agreement to exchange collections of property data has been established with the
advanced materials effort at Tsinghua University in China.  These agreements will enable U.S.
efforts to access important data from Russian and Chinese language research reports that would
not otherwise be readily available.

Outputs:

Database:

NIST Standard Reference Database Number 30: Structural Ceramics Database, Version 2, 1991.

Technical Papers:

"Material Specifications of Advanced Ceramics in Corrosion Studies", R. G. Munro, ASTM
Journal of Testing and Evaluation, Vol. 23 (5), 395-398 (1995).

"Material Specifications of Advanced Ceramics and Other Issues in the Use of Property
Databases with Corrosion Analysis Models," R. G. Munro, in Computerized Chemical Data
Standards: Databases, Data Interchange, and Information Systems - 2nd Volume, ASTM STP
1298, C. E. Gragg and J. Mockus, eds. (American Society for Testing and Materials,
Philadelphia, 1995).

"The Role of Corrosion in a Material Selector Expert System for Advanced Structural Ceramics,"
R. G. Munro, in Computerization and Networking of Materials Databases: Fourth Volume,
ASTM STP 1257, C. Sturrock and E. F. Begley, eds. (American Society of Testing and
Materials, 1995).

Impact:

Structural ceramics hold the key to advanced designs for high efficiency, high temperature heat
exchangers, corrosion resistant materials, and electronic packaging materials.  The SCD provides
critical property data, functions as a knowledge base for understanding property-performance
relationships, and serves as a guide to the areas most in need of supporting data or measurement
technology.
PROJECT TITLE:  STEP Materials

PROGRAM TITLE:  Evaluated Materials Data

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Carpenter, Joseph A., Jr.
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6397
Fax number:           (301) 990-8729
E-mail address:            carpent@micf.nist.gov

Principal Investigator(s) outside NIST:  Swindells, Norman and Robert
Mailing Address:                     Ferroday Ltd.
                                14 Mere Farm Road
                                Birkenhead
                                Merseyside L43 9TT
                                United Kingdom
Telephone:                           +44 151 670-0651
Fax number:                     +44 151 670-0651
E-mail address:                      rjs@ferroday.demon.co.uk
                                ns@ferroday.demon.co.uk

Technical Description:

This project develops and maintains the materials-related aspects of the ISO STEP standard for
computerized exchange of information on manufactured products.

Technical Objectives:

The immediate, near-term objective is to achieve ISO balloting approval of STEP Part 45
Materials as an ISO Standard (IS).  The longer terms objectives are to have STEP accepted
worldwide as a standard for exchange of information on materials in manufactured products and
to assess its viability for accessing distributed sources of material information.

Outcomes:

The nearest-term outcome should be the promotion of STEP Part 45 Materials to an IS status. 
This should occur in 1996.  The next nearest-term outcomes should be the use of its simplest
constructs and concepts in STEP application protocols (APs) being developed by others.  STEP
APs using its simplest constructs are underway in the areas of automotive design; electronic
circuit design; composites design and analysis; sheet metal dies design and planning; castings,
forgings, and molded products design and manufacture planning; and numerical control
machining planning.  In the longer term, a possible outcome may be the use of STEP for
accessing distributed sources of materials information.

Accomplishments:

1. Development of STEP Part 45 Materials to balloting for approval as an IS.  

2. Proper incorporation of materials technology aspects into other STEP parts and APs.

Outputs:

John Rumble, Jr. and Joseph Carpenter, Jr., "Materials 'STEP' into the Future," Advanced
Materials and Processes, Vol. 142, No. 4, October 1992, pages 23-27.

R. Swindells and J. Carpenter, "Industrial Automation Systems and Integration - Product Data
Representation and Exchange - Part 45: Integrated Resources: Materials," ISO/CD 10303-45
(International  Organization for Standardization, Geneva, Switzerland, September 2, 1993), 21
pages.

R. Swindells and J. Carpenter, "Industrial Automation Systems and Integration - Product Data
Representation and Exchange - Part 45: Integrated Resources: Materials," ISO/DIS 10303-45
(International  Organization for Standardization, Geneva, Switzerland, August 10, 1995), 34
pages.

N. Swindells, "Materials Property Data in STEP," in proceedings of CODATA Conference,
September 1994.

N. Swindells and J. Carpenter, "Reducing the Costs of Collaborative Engineering with STEP,"
The ActionLine (newsletter of the Automotive Industries Action Group), October, 1995.

Highlights:

The Draft International Standard (DIS) version of Part 45 addressing Materials in STEP was
completed and submitted for ISO balloting to IS status.

                    INTELLIGENT PROCESSING OF MATERIALS

Intelligent processing of materials (IPM) is the integration of:  (1) on-line sensors of materials
conditions or features; (2) sensors and controllers of process conditions which determine final
desired material properties; and, (3) models which relate process conditions to desired properties. 
IPM research in the Ceramics Division is focused on the measurement of characteristics of
powders and slurries.  Through the measurement of particular characteristics and the
understanding of how those characteristics relate to final properties, improved process control can
be achieved. 

Projects in this area are closely coupled with industrial and academic partners' research in the
development of processes, such as the application of research techniques to commercial practice.
NIST research addresses both the development of the measurement technique and the
understanding of the phenomena on which the technique is based.

Two projects are underway:

1.   The measurement of dispersion homogeneity in injection molding compounds by the use
     of nuclear magnetic resonance (NMR) is conducted in cooperation with industry to
     determine the role of processing parameters and binder and dispersion chemistry; and,

2.   Electroacoustic measurement to determine loading and size distribution of powders in
     dense slurries.    

For further information on IPM of ceramic materials, contact S. G. Malghan at (301) 975-6101
or e-mail malghan@micf.nist.gov

PROJECT TITLE:  Injection Molding of Ceramics

PROGRAM TITLE:  Intelligent Processing of Materials

Principal Investigator:

NIST Staff:
Designated Project Leader:  Malghan, S. G.
Mailing Address:           NIST
                      Materials (223), A207
                      Gaithersburg, MD  20899
Telephone:                 (301) 975-6101
Fax Number:           (301) 990-8729
E-Mail Address:            malghan@micf.nist.gov

Technical Description:

Injection molding is widely used in the ceramics industry to mass produce component parts of
larger assemblies.  The ability to produce parts of intricate geometry to fine levels of detail
renders this process attractive for advanced engine parts.  Typically injection molding utilizes an
organic binder to hold green parts together, and recently aqueous based binders have received
attention due to reduced environmental concerns.  Significant issues which require resolution to
make this process suitable for production of reliable structural components include: 
understanding the relationship of uniformity of binder distribution to  cracking during shrinkage,
role of binder chemistry on its distribution and rheological properties, and mechanistic
understanding of the powder-binder interactions.

Technical Objectives:

The objective of this project is to develop methods for the measurement and understanding of
the chemical and physical parameters which effect powder and binder interactions and
homogeneity as well as methods for the characterization of homogeneity.

Outcomes:

This research is expected to provide basic understanding of the role chemistry on the
homogeneity of injection molding ceramic blends.  This understanding will result in process
changes which improve properties and process yield.

Accomplishments:

Techniques have been developed to characterize the distribution of binder in injection molded
ceramic parts by NMR imaging.  NMR spectroscopic techniques have been developed to identify
the changes in molecular structure of organic binders as a result of aging.  Methods to
characterize powders during aqueous injection molding were developed.  The interactions
between powder and dispersant were delineated.

PROJECT TITLE:  Analysis of Ceramic Powder

PROGRAM TITLE:  Intelligent Processing of Materials

Principle Investigator:

NIST Staff:
Designated Project Leader:  Wang, Pu Sen
Mailing Address:           NIST
                      Materials (223), A205
                           Gaithersburg, MD 20899
Telephone:                 (301) 975-6104
Fax Number:           (301) 990-8729

Technical Description:

This project is designed to characterize Si-powder behavior in water slurries, under various
processing parameters, by NMR spectroscopy and imaging. 

Technical Objectives:

The goal of this project is to help US ceramic industry to define a set of favorable processing
parameters in producing silicon nitride parts through reaction bonding directly from Si powders.

Outcomes:

Information related to the following areas will be obtained as a result of this study: (1) chemistry,
impurity, and molecular structure of dispersants Darvan C and Betz 1190; (2) effects of these
dispersants on silicon powder behavior in water slurry, 3-D MRI pictures and 2-D profiles of Si-
powder distribution in water slurries at various concentrations and pH values. 

Accomplishments:

Through interactions with consortium members, NMR imaging studies were performed for four
types of slurries in which powders and dispersants use varies.  These studies showed the impact
of dispersant chemistry on processing of silicon and silicon nitride as well as provided data on
the chemistry of dispersants of Betz 1190 was thus performed extensively by 1H, 14N, 15N, 35Cl,
and 13C NMR at 400.140 MHz, 28.894 MHz, 50.674 MHz (from a higher frequency spectrometer
in University of Maryland), 39.193 MHz, and 100.577 MHz, respectively. The solutions analyzed
are 30% Betz 1190 in water. The results show that Betz 1190 is actually only 74.1 % pure, in
form of 2-hydroxy-3,3-ionene chloride. The other 25.9 % are either NH4-containing or a larger
polymer which has a different relaxation time (T1).  The 15N spectrum shows that a pure
component is indeed in an equal quantity of meso- and racemic- forms. 35Cl NMR suggests a
concentration dependence in chemical shift and dissociation constant. 1H T1 in solutions of pH
6 to 9 were also found to be constant.
Outputs:

Technical papers:

"NMR Characterization of Silicon Nitride: Slurry Homogeneity by T2-Weighted Proton Imaging",
Pu Sen Wang, submitted to Journal of Materials Research (1995).

"The Nitridation of a Silicon Powder Studied by XPS and Bremsstrahlung-Excited AES", Pu sen
Wang and Thomas N. Wittberg, submitted to Surface and Interface Analysis (1995).

Impact:

NIST results led some of the Powder Processing Consortium members to reconsider the
dispersants currently used. Decisions to change dispersants will depend on our future results
which will be higher in powder concentrations.
PROJECT TITLE:  Electroacoustic Characterization of Ceramic Powder Slurries

PROGRAM TITLE:  Intelligent Processing of Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Hackley, Vincent A.
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5790
Fax Number:           (301) 990-8729
E-mail Address:            vince.hackley@nist.gov

Other NIST Principal Investigator:  Mountain, Raymond
Mailing Address:                 NIST
                            Physics (221), A105
                            Gaithersburg, MD 20899
Telephone:                       (301) 975-2484
E-mail Address:                  raymo@rdm.phy.nist.gov

Technical Description:

This project is focussed on the application of non-destructive electroacoustic techniques for
characterizing particle size and charge in aqueous ceramic powder slurries, the development of
data, measurement science and computational tools to support these applications, and the
optimization of advanced ceramic processing by improvement of interfacial chemical control of
slurry properties.

Technical Objectives:

The objective of this research is to develop measurement methods and an understanding of the
surface density of ceramic powders of relevance to slury processing control.

Outcomes:

Two primary outcomes are expected to derive from this research: (1) development of
electroacoustic analysis for process control in powder processing, (2) improved understanding of
component interactions during aqueous processing of complex highly concentrated slurries.

Accomplishments:

Extensive testing and evaluation of a novel electroacoustic technique has demonstrated the
capabilities of this method for characterizing ceramic powder systems. Improvements were
derived from cooperative interaction with the instrument manufacturer. 

Polyelectrolyte dispersants, commonly used additives in aqueous processing of powders, were
studied and evaluated using electroacoustic methods in the model Si3N4/water system.
Measurements in moderately concentrated slurries provided agglomerate size and zeta potential
as a function of polymer concentration, molecular weight and suspension pH. This data will be
used to optimize conditions for improved dispersion of Si3N4 powders.

Electroacoustic measurements, along with several other surface chemical techniques, were used
to investigate the aqueous reaction-bonded silicon nitride system. This processing route begins
with metallic silicon dispersed in aqueous suspension in a complex  mixture with sintering aids,
nitriding agent, dispersants and binders. The aging of unstable silicon in water was characterized
under various conditions using electroacoustic measurements of the changing surface potential
as a function of time and pH. The interaction of dispersants and binders with the primary silicon
phase was examined extensively, leading to improvement of dispersion via chemical control of
suspension conditions. This research is on-going.

A consortium was formed in September 1993 between NIST, five manufacturers that produce
ceramic powders or components, an instrument company and a federal laboratory, in a joint effort
to improve processing of ceramic powders. Participants in this Consortium on Intelligent
Processing of Powders and Slurries include Cercom Inc. (Vista, CA), Coors Ceramics Co.
(Golden, CO), Eaton Corp. (Southfield, Mich), Kerr-McGee Corp. (Oklahoma City, OK), St.
Gobain/Norton Industrial Ceramics Co. (Northboro, MA), and instrument manufacturer, Matec
Applied Sciences Inc. (Hopkinton, MA). The Metals and Ceramics Division of the U.S.
Department of Energy's Oak Ridge National Laboratory is a participating partner.

Outputs:

"Electroacoustic Characterization of Particle Size and Zeta Potential in Moderately Concentrated
Suspensions", Hackley, V.A. and Malghan, S.G., in Ceramic Transactions, Volume 56, Advanced
Synthesis and Processing of Composites and Advanced Ceramics (American Ceramic Society,
Westerville, OH, 1995) p 283.

"Techniques for Characterization of Advanced Ceramic Powders", Malghan, S.G., Wang, P.S.
and Hackley, V.A.,  in Chemical Processing of Ceramics, Lee, B.I. and Pope, J.A., Eds., (Marcel
Dekker, NY, 1994).

"Surface Chemical Interactions of Si3N4 with Polyelectrolyte Deflocculants", Hackley, V.A.,
Premachandran, R. and Malghan, S.G., Key Engineering Materials, 89-91, 679 (1994).

"Intelligent Processing of Ceramic Powders and Slurries", Malghan, S.G., Hackley, V.A. and
Wang, P.S., in Ceramic Eng. and Sci. Proc. (American Ceramic Society, Westerville, OH, 1994)
p 527.

"The Surface Chemistry of Silicon Nitride Powder in the Presence of Dissolved Ions", Hackley,
V.A. and Malghan, S.G., J. Mat. Sci., 29, 4420 (1994).

Research results were also presented at two scientific meetings, the First International Symposium
on Advanced Synthesis and Processing of Composites and Advanced Ceramics in Cocoa Beach,
Florida, and the 1995 American Ceramic Society Annual Meeting in Cincinnati, Ohio.

Impact:

Research performed at NIST and reported to the consortium participants under the auspices of
a Cooperative Research and Development Agreement has provided new and improved
information regarding the aqueous suspension behavior of metallic silicon powders. This will
have a direct impact on processing formulations for reaction-bonded silicon nitride. NIST testing
and evaluation has provided feedback to the instrument manufacturer which resulted in system
improvements. NIST measurements have provided necessary information regarding the
application of electroacoustic methods to characterizing ceramic powders which is currently being
employed for the analysis of materials used by consortium participants. The impact of NIST
research in this area is demonstrated by the formation of new collaborations with industry which
are currently in the development stage.

PROJECT TITLE:  Environmental Stability of Infrastructural Cements

PROGRAM TITLE:  Intelligent Processing of Materials

Principal investigator(s):    

NIST Staff:
Designated Project Leader:  Allen, Andrew J. 
Mailing Address:           NIST
                      Materials (223), A163
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5982
Fax number:           (301) 990-8729
E-mail address:            allen@enh.nist.gov

Principal Investigator(s) outside NIST:  Livingston, Richard A.
Mailing Address:                     Federal Highway Administration
                                Dept. of Transportation
                                McLean, VA 22101-2296
Telephone:                           (703) 285-2903
Fax number:                     (703) 285-2766

                                Jennings, Hamlin M.
Mailing Address:                     Dept. of Civil Eng'g
                                Northwestern Univ'sity
                                Evanston, IL 60208-3109
Telephone:                           (708) 491-4858
Fax number:                     (708) 491-5282

                                Heaney, Peter J.
Mailing Address:                     Dept. of Geological Sciences
                                Princeton University
                                Princeton, NJ 08544
Telephone:                           (609) 258-2194
E-mail address:                      peter@geo.princeton.edu

Technical Description:

This project is designed to characterize the microstructural evolution during the hydration of
cements as it affects highway infrastructural concretes, to characterize their microstructural
degradation due to environmental effects, and to probe optimal additions of silica fume and other
additives that would give superior performance. 

Technical Objectives:

The objective is to assist in the production of advanced cementitious materials leading to highway
infrastructural concretes of improved durability.

Outcomes:

Three major outcomes are expected to occur:  (1) real-time, in-situ, non-destructive classification
of the microstructural evolution during hydration of highway-infrastructure cements containing
different pozzolanic additives;  (2) assessment of  aggregates, cement additives and hydration
conditions for stability of next-generation infrastructural concretes;  (3) improved optimization
of cement and concrete formulations for the highway infrastructure. A future development will
include experiments aimed at gaining a more fundamental understanding of the processes
underlying the dormant induction period, well-known in the early stages of cement hydration, and
the control of which is believed to be a key issue in the development of tailor-made
high-technology concretes.  

Accomplishments:

The effects, on the microstructural development during cement hydration, of adding pozzolanic
additives to cements and concretes, in the form of silica fume, have been extensively studied
using small-angle neutron scattering (SANS) and ultra-small-angle x-ray scattering (USAXS). 
A semi-fractal microstructural model, developed previously, has been modified to extract
statistically-significant microstructural parameters from the SANS data. Different silica fume
additives been characterized and compared, and the investigation has been extended to natural
additives which are  sometimes contained within aggregate minerals incorporated into concretes. 
These natural additives are known to engender natural pozzolanic reactions or alkali-silicate
reactions that degrade performance.

Outputs:

R. A. Livingston, D. A. Neumann, A. J. Allen and J. J. Rush; "Application of Neutron Scattering
Methods to Cementitious Materials", in Neutron Scattering in Materials Science II'. Ed. D. A.
Neumann, T. P. Russell and B. J. Wuensch. MRS Symp. Proc. 376 (Materials Research Society,
Pittsburgh, PA., 1995) 459-469.

A. J. Allen and R. A. Livingston; "Small-Angle Scattering Study of Concrete Microstructure as
a Function of Silica Fume, Fly Ash or Other Pozzolanic Additions", (SP 153-62) in Proc. 5th
CANMET/ACI International Conference on Fly Ash, Silica Fume, Slag and Natural Pozzolans
in Concrete, June 1995. Ed. V. M. Malhotra. American Concrete Institute, Detroit, MI. 1179-1200
(1995).

R. A. Livingston and A. J. Allen; "Application of Small-Angle Neutron Scattering Method to the
Study of the Durability of Historic Brick and Mortar", in Ceramics in Architecture', Proc. 8th
CIMTEC World Ceramics Congress and Forum on New Materials. Ed. P. Vincenzini. CIMTEC,
Faenza, Italy. Vol. A ???-??? (1995).

Impact:

The studies are enabling a quantitative assessment of the microstructural modifications underlying
the variable effectiveness of different silica fume additives in forming cements and concretes of
improved strength and durability.

                MECHANICAL PROPERTIES OF BRITTLE MATERIALS

Mechanical properties are the source of some of the greatest benefits as well as the most serious
limitations of ceramics.  With their great strength-to-weight ratio, their relatively inert behavior
in aggressive environments, and their ability to withstand much higher temperatures than metals
or polymers, ceramics potentially offer major improvements for component design in a wide
range of applications.  On the debit side, brittle fracture, creep at elevated temperatures,
environmentally enhanced failure, and the lack of techniques which can detect and quantify
critical flaws before failure occurs, impede their more wide-spread uses.  Problems in controlling
and controlling failure of ceramics stems from three sources:  lack of understanding of the failure
processes, limited standard test techniques to permit inter-laboratory comparisons of material
behavior, and inadequate statistical techniques for reliability and lifetime estimation.  The
Mechanical Properties program  has components specifically addressing each of these issues.  
Basic understanding of mechanical behavior of ceramics is being investigated for both ambient
and elevated temperature applications.  Effects of cyclic loading and  microcrack
formation/coalescence are being studied for lead zirconium titanate (PZT), a technologically
important actuator material.  Mechanical properties and failure processes in fiber-reinforced
ceramic matrix composites are being investigated as a function of both temperature and fiber
loading. Residual in stresses associated with crack bridging in both fiber-reinforced composites
and microstructurally toughened alumina are being measured via micro-Raman techniques.  In
addition, environmentally enhanced fracture remains an important subject from both an
experimental and a theoretical (see Theory and Modeling section) viewpoint.  At elevated
temperatures, the basic mechanisms responsible for creep in silicon nitride are being investigated.

An important aspect of the program is the development of standards.  New standard test
techniques for hardness and toughness are being developed and tested in round-robin
experiments; these will eventually lead to ASTM and ISO standards.  For elevated temperatures,
a new creep specimen design has been developed which concentrates more of the applied load
in the gage length and reduces the chance of failure from non-gage portions of the specimen.  
Finally, techniques to predict lifetimes of ceramics under constant or cyclic loading conditions
are being developed.  The nonparametric bootstrap  approach to lifetime  prediction is being
applied to a number of materials.  A parametric model to predict lifetimes of  PZT under cyclic
loading is also under development.  This latter model does not restrict the material to
environmentally enhanced fracture behavior since experimental evidence has demonstrated that
other, albeit unknown, processes are also active during cyclic loading.  

For further information about the Mechanical Properties of Brittle Materials Program, please
contact Edwin Fuller at 301-975-5795 or e-mail requests to erfuller@enh.nist.gov.

PROJECT TITLE:   Creep of Ceramics

PROGRAM TITLE:  Mechanical Properties of Brittle Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Hockey, Bernard J.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-5780
Fax number:           (301) 990-8729

Other NIST Principal investigator(s):  Chuang, Tze-jer
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5773
Fax number:                    (301) 990-8729
E-mail address:                     tze-jer.chuang@nist.gov

                               Krause, Ralph F. Jr.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5781
Fax number:                    (301) 990-8729
E-mail address:                     ralph.krause@nist.gov

                               Luecke, William E.
Mailing Address:                    NIST
                               Materials (223), B309
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5744
Fax number:                    (301) 990-8729
E-mail address:                     william.luecke@nist.gov

Technical Description:

This project is designed for three purposes: (1) to develop standard testing methodologies for
ceramics at elevated temperature, particularly for a tensile mode of loading; (2) to develop an
engineering data base on high-temperature strength, creep, creep rupture properties, and crack
growth behavior for advanced, structural ceramic materials; and (3) to investigate and elucidate
effects of material microstructure on elevated temperature mechanical behavior.

Technical Objectives:

This research is designed to assist industry in the evaluation, design, and development of
advanced, structural ceramics as high-temperature components in land-based heat engines for
power generation or for vehicle applications, and in development of measurement methodologies
for the evaluation of high-temperature mechanical properties.

Outcomes:

Major outcomes of this research are expected to include: (1) development of failure mechanism
maps of relevant materials for the evaluation and design of ceramic engine components;
(2) development of standardized tensile testing methodologies for material comparison; and
(3) elucidation of the relationship between material's microstructure and mechanical behavior to
guide material development and reliability assessment.

Accomplishments:

NIST and General Electric Corporation signed a CRADA in September, 1994 to investigate the
creep, creep rupture, and strength properties of two commercial grades of in-situ toughened
silicon nitride.  The project represents one of the widest ranging attempts to gather data on single
grades of engineering ceramic.  We have combined room-temperature strength tests, intermediate-
temperature (800 C to 1000 C) stress rupture tests, and high-temperature (1000 C to 1400 C)
creep-rupture tests to produce failure mechanism maps for these materials.  Although we have
discontinued tests on one of the materials, due to poor specimen to specimen repeatability, the
other material exhibits excellent and highly repeatable properties.  Over one hundred samples of
this material have been tested and selected creep samples are currently being examined by
analytical transmission electron microscopy.  Initial results indicate that the improved creep
rupture behavior may be related to the atypical absence of cavitation within the narrow interfaces
separating adjacent grains.

Through work on several other grades of silicon nitride, we have developed a new model for
tensile creep deformation of silicon nitride.  The model recognizes the fact that the silicon nitride
grains themselves are undeformed by the creep process.  Rather, redistribution of the silicate
binding phase from cavitating multi-grain junctions to uncavitated pockets produces the observed
extension.  Sliding of the silicon nitride accommodates the redistribution.  The model readily
explains the hundred to thousand-fold increase in creep resistance in compression over tension. 
In compression, the applied stress opposes the volume increase of the interstitial silicate volume. 
When this mechanism is suppressed, the silicon nitride deforms by ordinary solution-
reprecipitation creep.

We have used finite element techniques to develop two new tensile specimen geometries to add
to a third already in use.  Each represents a significant improvement over previous designs,
allowing us to conduct tests at much higher stresses than previously possible.  One specimen is
specifically designed to be amenable to fabrication from existing engineering components.  This
test ability will make it possible to verify the engineering properties of the components
themselves.  We have experimentally verified that the three geometries yield identical creep
properties.

We have selected one of the newly designed specimens for an inter-laboratory round robin for
creep testing.

Outputs:

Technical papers:

William E. Luecke, Sheldon M. Wiederhorn, Bernard J. Hockey, Gabrielle G. Long, and Ralph
F. Krause Jr., "Cavitation Contributes Substantially to  Creep in Silicon Nitride,"  J. Am. Ceram.
Soc, 78, 2085-2096 (1995).

S. M. Wiederhorn, W. E. Luecke, B. J. Hockey, and G. G. Long, "Creep-Damage Mechanisms
in Si3N4," pp. 305-326 in Tailoring of High Temperature Properties of Si3N4 Ceramics, M. J.
Hoffman and G. Petzow, eds. Kluwer Academic Publishers, Dordrecht, The Netherlands, 1994.

S. M. Wiederhorn, J. D. French, and W. E. Luecke, "High-Temperature Reliability of Structural
Ceramics," pp. 145-155 in 5th International Symposium on Ceramic Materials and Components
for Engines, D. S. Yan, X. R. Fu and S. X. Shi, eds. World Scientific Publishing Co., Singapore
(1995).

S. M. Wiederhorn and W. E. Luecke "The Importance of cavitation to the creep of structural
ceramics," to be published in Proceedings of the Symposium on Plastic Deformation of Ceramics,
Snowbird Utah, August 7-12, 1994. Sponsored by The Engineering Foundation, 1995.

S. M. Wiederhorn, J. D. French, and W. E. Luecke, "A Comparison of Fracture Mechanism Maps
with the Larson-Miller Method of Predicting Lifetime," Ceram. Eng. Sci. Proc, in press (1995).

J. D. French and S. M. Wiederhorn, "Tensile specimens from Ceramic Components," J. Am.
Ceram. Soc, 1995, in press.

Technical papers submitted for publication:

William Luecke and J. D. French, "Strain measurement uncertainty during flag-based      
extensometry," submitted to J. Am. Ceram. Soc, 1995.

B. A. Fields and S. M. Wiederhorn, "Creep and Cavitation in a Siliconized Silicon Carbide,"
submitted to J. Am. Ceram. Soc. 1995.

Impact:

The creep and rupture data gathered in this project demonstrate that silicon nitrides can have the
structural properties necessary for use in high-temperature heat engines.
PROJECT TITLE:  Mechanical Test Development

PROGRAM TITLE:  Mechanical Properties of Brittle Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Quinn, George D.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-5765
Fax number:           (301) 990-8729
E-mail address:            geoq@enh.nist.gov

Other NIST Principal investigator(s):  Krause, Ralph F. Jr.
Mailing Address:                   NIST
                              Materials (223), A329
                              Gaithersburg, MD 20899-0001
Telephone:                         (301) 975-5781
Fax number:                   (301) 990-8729
E-mail address:                    ralph.krause@nist.gov

Technical Description:

This project is designed to created, developed, improved, refined, and standardized mechanical
testing methods for brittle ceramic materials. 

Technical Objectives:

This research is designed to assist industry and in-house programs by developing procedures for
characterizing ceramic materials and for generating lifetime and reliability data.  Standard test
methods are prepared for ASTM and ISO.  Our goal is to develop procedures that are as
technically rigorous as possible while remaining practical and usable by industry.

Outcomes:

Guidelines and test procedures are created and/or refined so that accurate and precise results for
mechanical property data can be obtained by NIST, industry, government labs, and academia. 
Wherever possible, standard practices or test methods are prepared in the appropriate forum. 
Emphasis is on preparing ASTM and ISO standards.  This project also provides guidance and
prestandarization work relevant to Standard Reference Material projects.  Round robin projects
are conducted as necessary.

Accomplishments:

Four ASTM standards have been adopted by Committee C-28 since 1991 in large part due to
work done in this project:

    1.    ASTM C 1198-91  Dynamic Young's Modulus, Shear Modulus, and Poisson's Ratio for
          Advanced Ceramics by Sonic Resonance,

    2.    ASTM C 1161-90  Standard Test Method for Flexural Strength of Advanced Ceramics
          at Ambient Temperature,

    3.    ASTM C 1211-92  Standard Test Method for Flexural Strength of Advanced Ceramic at
          Elevated Temperature, 

    4.    ASTM C 1239-94a  Standard Practice for Reporting Strength Data and Estimating
          Weibull Distribution Parameters.

In addition, work on this task has contributed to the following standards which are now being
balloted in ASTM:

    6.    ASTM C-xxxx  Standard Test Methods for the Determination of Fracture Toughness of
          Advanced Ceramics, 

    7.    ASTM C-xxxx  Standard Test Method for Knoop Indentation Hardness of Advanced
          Ceramics,

    8.    ASTM C-xxxx  Standard Test Method for Vickers Indentation Hardness of Advanced
          Ceramics,

    9.    ASTM C-xxxx  Standard Practice for Fractography and Characterization of Fracture
          Origins in Advanced Ceramics.

Outputs:

Outputs include standard test methods and practices as listed above.  Round robin projects and
reports not only measure the robustness of the methods and furnish information for precision and
bias statements, but also serve to spread knowledge about the methods.  Technical papers and
reports support the standards.

Technical papers published:

C. Tracy and G. Quinn, "Fracture Toughness by the Surface Crack in Flexure (SCF) Method,"
Ceram. Eng. and Sci. Proc., Vol. 15, [5], 1994, pp. 837-845.

G. Quinn, R. Gettings, and J. Kbler, "Fracture Toughness of by the Surface Crack in Flexure
(SCF) Method: Results of the VAMAS Round Robin," Ceram. Eng. and Sci. Proc., Vol. 15, [5]
1994, pp. 846-855.

J. Swab and G. Quinn, "Results of a Round Robin Exercise on the Fractography of Advanced
Structural Ceramics," Ceram. Eng. and Sci. Proc., Vol. 15, [5], 1994, pp. 867-876.

G. Quinn, J. Kbler, and R. Gettings, "Fracture Toughness of Advanced Ceramics by the Surface
Crack in Flexure (SCF) Method: A VAMAS Round Robin," VAMAS Technical Report #17,
NIST, June, 1994.

G. D. Quinn and C. A. Tracy, "Fracture Toughness of Advanced Ceramics as Measured by the
Surface Crack in Flexure Method," in Ceramics: Charting the Future, ed. P. Vincenzini,
Proceedings of the 8th World Ceramic Congress, CIMTEC, Techna, Faenza, 1995.

J. J. Swab and G. D. Quinn, "Fractography and Characterization of Fracture Origins in Advanced
Ceramics, A VAMAS Round Robin," pp. 569-576 in New Horizons for Materials, Proceedings
of the 8th World Ceramic Congress, CIMTEC, Florence, Italy, ed P. Vincenzini, Techna, Faenza,
1995.

G. D. Quinn, J. J. Kbler, and R. J. Gettings, "Fracture Toughness of Advanced Ceramics: A
New VAMAS Round Robin," pp. 577-584 in New Horizons for Materials, Proceedings of the
8th World Ceramic Congress, CIMTEC, Florence, Italy, ed P. Vincenzini, Techna, Faenza, 1995.

J. J. Swab and G. D. Quinn, "Fractography of Advanced Structural Ceramics: Results From Topic
#2 of the VAMAS Round Robin Exercise," in Proceedings of Jan. 1995 Meeting ACS, Cocoa
Beach, Ceram. Eng. and Sci. Proc., 1995, in press.
R. J. Gettings and G. D. Quinn, "Surface Crack in Flexure (SCF) Measurements of the Fracture
Toughness of Advanced Ceramics," in Proceedings of Jan. 1995 Meeting ACS, Cocoa Beach,
Ceram. Eng. and Sci. Proc., 1995, in press.

J. J. Swab and G. D. Quinn, "Fractography of Advanced Structural Ceramics, Results from the
VAMAS Round Robin Exercise," VAMAS Report #19, June, 1995.  (Also published as U.S.
Army Technical Report, ARL-TR-656, Dec., 1994.)

C. R. Brinkman, G. D. Quinn, and R. W. McClung, "Overview of ASTM Standard Activities in
Support of Advanced Structural Ceramics Development," Ceram. Eng. and Sci. Proc., 1995, in
press.

G. D. Quinn, R. J. Gettings, and J. J. Kbler, "Fracture Toughness of Ceramics by the Surface
Crack in Flexure (SCF) Method," in 6th International Symposium on Fracture Mechanics of
Ceramics, Karlsruhe, July, 1995, in press.

G. D. Quinn, R. J. Gettings, and J. J. Kbler, "Fractography and the Surface Crack in Flexure
(SCF) Method for Evaluating Fracture Toughness of Ceramics," in Proceedings of the Third
Alfred Conference on Fractography of Glasses and Ceramics," July, 1995, in press.

J. J. Swab and G. D. Quinn, "The VAMAS Fractography Round Robin: A Piece of the
Fractography Puzzle," in Proceedings of the Third Alfred Conference on Fractography of Glasses
and Ceramics," July, 1995, in press.

Impact:

Refined and standardized test methods are now available.  The ceramics community now has
procedures that generate data of high quality and data which is readily comparable between
laboratories.  This has benefitted both the industrial and research communities.  This was not the
case 10 years ago when data was of mixed quality and could not be readily compared between
laboratories. 

Data suitable for design is now easily obtained and data bases are being developed on the basis
of the standards.

Tangible benefits also include significant cost savings.  For example, the adoption of standard
specimen sizes and surface preparation treatments has driven the cost of flexure specimens (the
bread and butter strength test for ceramics) from $15-20 per specimen to $8 per specimen, a 50%
savings.

As another example, fractography of ceramics has heretofore been a highly interpretive art.  
Work in this project has standardized some of the more routine aspects of fractographic analysis. 
Consistent results and interpretations are more readily obtained and can be related better to
mechanical property results.  The standard practice for fractographic analysis is now used as a
teaching aid in courses at several universities and by a course offered by The American Ceramic
Society.
PROJECT TITLE:  Fracture Behavior of Ceramic Matrix Composites

PROGRAM TITLE:  Mechanical Properties of Brittle Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Braun, Linda M.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-5777
Fax number:           (301) 990-8729
E-mail address:            lmbraun@enh.nist.gov

Other NIST Principal investigator(s):  Fuller, Edwin R. Jr.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5795
Fax number:                    (301) 990-8729
E-mail address:                     edwin.fuller@nist.gov

Technical Description:

This project is designed to elucidate failure modes, damage generation, and damage accumulation
in fiber-reinforced ceramic matrix composites.  Fracture in the composite matrix, individual
fibers, fiber bundles, and at the fiber/matrix interface is studied as a function of processing
methodology and microstructure.

Technical Objectives:  

This research project is designed to assist industry by assessing the applicability of fracture
mechanics in the description of failure modes and reliability of fiber-reinforced ceramic matrix
composites.  Goals are to relate damage and fracture behavior to microstructure, and to develop
a testing methodology to quantify damage.

Outcomes:

The major outcomes expected from this research are: (1) development of testing methodologies
to quantify damage in fiber-reinforced ceramic matrix composites; and (2) reliable damage and
failure property data for design and manufacture of fiber-reinforced ceramic matrix composites. 

Accomplishments:

Strength, fracture toughness, and the failure mode in SCS-6 SiC-fiber reinforced Si3N4 matrix
composites were investigated as a function of fiber volume fraction, controlled flaw size
(indentation load) and temperature.  Matrix-cracking stress and ultimate strength of the
composites were found to decrease with increasing temperature, but their temperature sensitivity
decreased with increased fiber volume fraction.  The tendency for non-catastrophic failure
increased with fiber volume fraction, while the tendency for catastrophic failure increased with
temperature.  The failure mode was demonstrated to be determined by the fiber bundle strength
and the matrix cracking stress.  Catastrophic failure at high-temperatures was found to be mainly
a result of fiber strength loss.  

A constrained shear test was used to investigate damage in SiC/SiC fiber-reinforced composites. 
A bonded interface technique has allowed for direct observation of shear-induced distributed
damage in these materials.  Load-displacement curves are directly related to the amount of
generated damage.

Outputs:

Several research papers were produced from the technical advancements, which were made.

Technical papers published:

H. H. Xu, C. P. Ostertag, E. R. Fuller, Jr., L. M. Braun, and I. K. Lloyd, "Fracture Resistance
of SiC-Fiber-Reinforced Si3N4 Composites at Ambient and Elevated Temperatures," J. Am.
Ceram. Soc., 78 [3], 698-704 (1995).

H. H. Xu, L. M. Braun, C. P. Ostertag, R. F. Krause, Jr., and I. K. Lloyd, "Failure Modes of
SiC-Fiber/Si3N4-Matrix Composites at Elevated Temperatures," J. Am. Ceram. Soc., 78 [2], 388-
94 (1995).

Impact:

NIST measurements will provide reliable damage and failure property data for the design and
manufacture of fiber-reinforced ceramic matrix composites.  This data will be used to improve
reliability assessment models for fiber-reinforced ceramic matrix composite.

PROJECT TITLE:   Lifetime Prediction Methodology

PROGRAM TITLE:  Mechanical Properties of Brittle Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  White, Grady S.
Mailing Address:           NIST
                      Materials (223), A215
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-5752
Fax number:           (301) 990-8729
E-mail address:            spruce@enh.nist.gov

Other NIST Principal investigator(s):  Braun, Linda M.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5777
Fax number:                    (301) 990-8729
E-mail address:                     lmbraun@nist.gov

                               Wallace, Jay S.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5984
Fax number:                    (301) 990-8729
E-mail address:                     jay.wallace@nist.gov

                               Fuller, Edwin R. Jr.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5795
Fax number:                    (301) 990-8729
E-mail address:                     edwin.fuller@nist.gov

Technical Description:

This integrated experimental and analytical research project is designed to provide confirmed
methodologies for service life estimation on a variety of engineering components used by
industry for performing critical functions so that interruption can be avoided.

Technical Objectives:

The objectives of this project are to elucidate and to characterize time-dependent failure
mechanisms in ceramic systems.  This includes development of damage evolution laws and
understanding of kinetics and driving forces leading to damage accumulation, including the role
of environment, temperature, stress, and other physical properties.  

Outcomes:

Outcomes include the adoption of reliable lifetime prediction methodologies by industry (e.g.,
aerospace, electronic, energy, etc.) leading to improved reliability, savings in maintenance, and
enhanced safety.

Accomplishments:

Predictions of long-term reliability of residually stressed InP have been made.  A non-parametric
bootstrap method  has provided new insight into uncertainties associated with lifetime predictions
for materials with minimal environmentally enhanced crack growth.  A new form of controlled
crack growth has been observed in InP; presently, its implications for reliability predictions are
not understood.

Output:

Transfer of the non-parametric bootstrap method to AT&T has been achieved.  In addition, two
technical manuscripts have been written:

Technical papers submitted for publication:

G. S. White and L. M. Braun, "Environmentally Enhanced Fracture Behavior of InP," J. Am.
Ceram. Soc., submitted.

E. R. Fuller, Jr., G. S. White, L. M. Braun, and W. C. Carter, "Lifetime Predictions and
Confidence Levels Using a Nonparametric Bootstrap Technique,"  J. Am. Ceram. Soc., to be
submitted.

Impact:  

AT&T has used the results of the nonparametric bootstrap method to evaluate and modify
qualification procedures for InP optical couplings.

PROJECT TITLE:  Micro-Raman Stress Measurements

PROGRAM TITLE:  Mechanical Properties of Brittle Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Braun, Linda M.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-5777
Fax number:           (301) 990-8729
E-mail address:            lmbraun@nist.gov

Other NIST Principal investigator(s):  White, Grady S.
Mailing Address:                    NIST
                               Materials (223), A215
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5752
Fax number:                    (301) 990-8729
E-mail address:                     spruce@enh.nist.gov

Technical Description:

This project is designed to develop micro-Raman techniques for characterizing macroscopic and
microstructural stresses in select ceramic systems.  Stresses are determined by shifts of peak
positions in the Raman spectra.  Lateral resolution of a few micrometers is obtained. 

Technical Objectives:

This research project is designed to assist industry in the measurement of localized residual
stresses which can control mechanical, electrical and optical properties over a wide range of
industrial applications.  

Outcomes:

Three major outcomes are anticipated for this work.  The first is the development of standardized
calibration procedures allowing the technique to provide quantitative stress values for a wide
variety of material systems.  The second is the adoption of stress measurement procedures by
electronic packaging industry.  The third is the securing of accurate stress data leading to
improved models for material system design and reliability assessment.

Accomplishments:

Measurements have been made in a number of ceramic materials systems.  In alumina, changes
in stress associated with crack-bridging grains and stress variations within individual grains have
been detected.  Preliminary work has begun in which stress measurements in alumina grains have
been correlated with microstructural simulations.  Stress changes in metal-organic films have been
correlated with changes in stress state in sapphire substrates.  Changes in stress state have been
observed in siliconized-SiC composites after high-temperature tensile creep deformation.  

Most importantly, applied stress versus peak shift curves of single crystal sapphire specimens
with known orientation have demonstrated that calibration curves are orientation dependent. 
Therefore, in general, a crystallite orientation must be known before its stress state can be
accurately determined.
PROJECT TITLE: Micro-Tribology

PROGRAM TITLE:  Mechanical Properties of Brittle Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader: Hsu, Stephen M.
Mailing address:          NIST
                     Materials (223), A256
                     Gaithersburg, MD 20899
Telephone Number:    (301) 975-6120
Fax Number:          (301) 990-8729
E-mail address:           hsu@micf.nist.gov

Other NIST Principal investigator(s):  Gates, Richard S.
Mailing address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone Number:              (301) 975-3677
Fax Number:                    (301) 990-8729
E-mail address:                     gates@micf.nist.gov

                               McGuiggan, Patty
Mailing address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone Number:              (301) 975-4599
Fax Number:                    (301) 990-8729
E-mail address:                     pmmcg@enh.nist.gov

                               Fischer, Daniel A.
Mailing address:                    Brookhaven National Laboratory
                               Building 510E
                               Upton, NY 11973
Telephone Number:              (516) 344-5177
Fax:                           (516) 344-5419
E-mail address:                     daniel.fischer@nist.gov

Technical Description:

This project is to provide measurement techniques and standards of surface properties
(mechanical and tribological) of advanced materials and systems from nano-meter scale to macro-
scale.  The initial focus is on magnetic hard disk information storage industry.

The National Storage Industry Consortium (NSIC) consists of 34 companies, 25 universities and
government laboratories.  Its aim is to foster pre-competitive generic research in information
technologies.  We work closely with the Tribology research group of NSIC to explore surface
chemistries, textural designs, and to develop test techniques for measuring the effects of mono-
molecular films.  During last year, we have set up a state-of-the-art laboratory facility to measure
friction, stiction, and wear of magnetic hard disks.  Several new techniques were developed to
measure the effect of mono-molecular film on superflat disks.

Experiments were done on a model system as well as on the actual disks.  Stearic acid monolayer
and submonolayer were deposited on a copper surface and examined using Fourier Transform
Infrared Spectroscopy, Time-resolved Raman Spectroscopy, and Ultra-soft X-ray Absorption
Spectroscopy.  The combination of these techniques allows the determination of the molecular
orientation, inclined angle, and the nature of the bonding of the stearic acid with the surface. 
These molecular parameters were correlated with the friction and wear performance of the model
system to elucidate surface protection mechanisms.  

Various organic monolayers and mono-molecular films were dipped coated on the NSIC CHx
coated surfaces as well as the CNx coated surfaces.  The coated disks were evaluated for friction
and durability studies both at NSIC and NIST.  Some films were found to perform much better
than the current commercial practice.

Measurement techniques were also developed to measure thin film properties using Atomic Force
Microscope, nano-indentor, nano-scratch tester, and ball-on-inclined plane apparatus.  

Technical objectives:

This research project is designed to assist industry in providing critical measurement tools
necessary for the development of new generation of data storage technology of 62 Mbit/MM2 (40
Gbit/in2). 

Outcomes:

Two anticipated outcomes are expected to occur: (1) development of laboratory scale test
procedures to evaluate new materials, coatings, and lubricant chemistry of the magnetic hard disk
system, (2) understanding of how mono-molecular films interact and protect the magnetic disks,
(3) determine the relationship between thin film structures and their mechanical properties.

Outputs:

"A Spectroscopic Study of a Copper Surface Under Boundary Lubrication: Chemisorbed Stearic
Acid Multilayers," Z. H. Hu, P. S. Wang, S. M. Hsu,  J. of Lubrication Science, 7-4, 293-307,
1995.

"Asperity-Asperity Friction as Measured by a Two-Ball Collision Apparatus," T. N. Ying and
S. M. Hsu,  Tribology Trans, 39, 1, 33-42, 1996.

"Tribochemistry and Lubrication," S. M. Hsu and R. S. Gates, Invited paper in the Proceedings
of the Tribochemistry Forum in International Tribology Conference, Yokohama, Japan, Japanese
Society of Tribologists, 1995.

"Molecular Orientation and Bonding of Monolayer Stearic Acid on a Copper Surface in Air," D.
A. Fischer, Z. Hu, and S. M. Hsu, submitted to Tribology Letters.

"Tribochemical and Thermochemical Reactions of Stearic Acid on Copper Srufaces in Air as
Measured by Ultra-Soft X-ray Absorption Spectroscopy," D. A. Fischer, Z. Hu, and S. M. Hsu,
submitted to Tribology Letters.

                         NANOSTRUCTURED MATERIALS

Materials with microstructures, e.g., grain sizes, on the order of nanometers have been cited as
having potentially improved strength and, for ceramics, superplastic behavior which could be
beneficial as a low-cost forming technique.  Difficulties have been recognized in consolidating
nano-sized ceramic powders to full density.  This difficulty has limited researchers ability to fully
evaluate these materials.  A high-risk project to consolidate nanostructured materials without
sintering aids has been undertaken in cooperation with Sandia National Laboratory and Rutgers
University.  The approach taken at NIST utilizes high pressure compaction with liquified gas as
a powder lubricant.

For further information on nanomaterial consolidation, please contact S. G. Malghan at (301)
975-6101 or e-mail to malghan@micf.nist.govPROJECT TITLE:  Low Temperature Fabrication of Transparent Silicon Nitride  

PROGRAM TITLE:  Nanstructured Materials   

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Malghan, Subhas 
Mailing Address:           NIST
                      Materials (223), A213
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6101
Fax Number:           (301) 990-8729
E-Mail Address:            malghan@enh.nist.gov

Other NIST Principal investigator(s):  Gonzalez, Eduardo J.
Mailing Address:                    NIST                    
                               Materials (223), A221
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6102
Fax Number:                    (301) 990-8729
E-Mail Address:                     egonzalez@enh.nist.gov

                               Piermarini, Gasper J.
Mailing Address:                    NIST
                               Materials (223), A221
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5734
Fax Number:                    (301) 990-8729                        
E-Mail Address:                     gasper@enh.nist.gov

Technical Description: 

This project is designed to characterize and evaluate the effects of high pressure compaction on
the consolidation and densification of nanosize powders, including silicon nitride and aluminum
oxide.

Technical Objectives:

This project is designed to assist industry indirectly in the development of processing technology
for the production of advanced nanostructured materials possessing mechanical and functional
properties superior to those commonly found in ceramic materials. 

Outcomes: 

The major outcome expected is the development of a high pressure compaction fabrication
process for making fully dense nanostructured ceramic materials. Another is the process for
fabricating ceramic materials with controlled porosity for a wide range of nanoscale filtration
applications. The technology may also permit the fabrication of transparent ceramics by virtue
of their nanoscale microstructures. 

Accomplishments:

In this work, we have demonstrated the concept that simple molecular liquids can enhance
densification in the compaction process by providing a lubricating medium for the nanosize
particles. For example, green density of Si3N4 compacts  fabricated by high pressure compaction
of nanosize amorphous powder using liquid N2 can be enhanced by as much as 10% over dry
powder compaction permitting attainment of nearly full random packing density of the green
body. However, on sintering, full densification without grain growth was not achieved.
Furthermore, crystallization of the amorphous Si3N4 powder also occurred complicating the
microstructural development during the sintering process. Similar studies on y phase nanosize
alumina powder showed that increased compaction pressure results in a corresponding increase
in green body density, specifically from 54% theoretical at 1 GPa to 65% theoretical at 2.5 GPa.
From this work two conclusions can be drawn: (1) Increased compaction pressure enhances the
y-to- phase transition, effectively increasing the nucleation rate or alternatively lowering the
transition temperature to the 1000 C range, and (2) increased compaction pressure leads to
increased densification upon heat treatment.   

Outputs:

Several research papers were produced as a result of the technical advancements made here:

W. Chen, A. Pechenik, S. J. Dapkunas, G. J. Piermarini and S. G. Malghan, "Novel Equipment
for the Study of the Compaction of Fine Powders", J. Am. Ceram. Soc., 77 [4] 1005-1010 (1994). 

Eduardo J. Gonzalez, Gasper Piermarini, Bernard Hockey and Subhas G. Malghan  "Low
Temperature Fabrication From Nanosize Ceramic Powders", Final Report to DOE, ORNL/Sub/92-
22041/02, April 28, 1995

M. R. Gallas and G. J. Piermarini, "The Bulk Modulus and Young's Modulus of Nanocrystalline
y-Alumina," J. Am. Ceram. Soc., 77 [11] 2917-20 (1994).

M. R. Gallas, B. Hockey, A. Pechenick, and G. J. Piermarini, "Fabrication of Transparent y-
Al2O3 from Nanosize Particles", J. Am. Ceram. Soc., 77 [8] 2107-12 (1994).

A. Pechenik, G. J. Piermarini, and S. C. Danforth, "Low Temperature Densification of Silicon
Nitride Nanoglasses," Nanostructured Materials, 2, 479 (1993).

Accomplishment:

Utilizing conventional low pressure compaction procedures, nanosize ceramic powders cannot be
pressed to high density green bodies.  The present work demonstrated that high pressure
compaction is an effective method to produce transparent high density green bodies of nanosize
ceramic powders. The high density and nanostructure of these green bodies reduces the
temperature and time normally needed for sintering thereby retaining the original nanostructure.
Retention of the nanostructure promises feasibility of high temperature forming by superplastic
deformation permitting near net shaping of complex ceramic pieces.   

                       STANDARD REFERENCE MATERIALS

Standard Reference Materials (SRMs) are required for the calibration of analytical instruments. 
Projects underway in the Division either address the needs of the ceramics industry specifically
or utilize the Division's capabilities for more broadly applicable SRMs.  SRM project addition
and production is conducted in cooperation with the  Standard Reference Materials Program
Office.  Standard reference materials projects in the Division include:

    calibration standards for x-ray diffractometers;

    ceramic calibration blocks for high microhardness measurement;

    size, chemistry, and phase content SRMs for use in the ceramics processing field;

    zirconia powder size standards for use in the plasma-spray coating industry; and

    standards for the measurement of glass properties.

These projects are conducted in cooperation with applicable industries and are an integral part
of the Division research program.

For additional information on the Standard Reference Materials program, contact S. J. Dapkunas
at 301-975-6119 or e-mail to Dapkunas@micf.nist.gov.
PROJECT TITLE: SRMs for Powder Diffraction

PROGRAM TITLE:  Standard Reference Materials

Principal investigator(s): 

NIST Staff:
Designated Project Leader:  Cline, James P.
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975 5793
Fax Number:           (301) 990 8729
E-Mail Address:            Cline@credit.nist.gov

Other NIST Principal investigator(s):  Deslattes, Richard D.
Mailing Address:                    NIST
                               Physics, A141
                               Gaithersburg, MD 20899
Telephone:                          (301) 975 4841

                               Staudenmann, Jean-Louis
Mailing Address:                    NIST
                               Physics, A141
                               Gaithersburg, MD 20899
Telephone:                          (301) 975 4866

                               Toby, Brian H.
Mailing Address:                    NIST
                               Reactor, E151
                               Gaithersburg, MD 20899
Telephone:                          (301) 975 4297

Principle Investigator(s) outside NIST:  Von Dreele, Robert B.
Mailing Address:                     LANSCE, MS-H805
                                Los Alamos National Laboratory
                                Los Alamos, NM 87545
Telephone:                           (505) 667 3630
E-Mail Address:                      VonDreele@lanl.gov

                              Kalceff, Walter
Mailing Address:                   University of Technology, Sydney
                              Dept of Applied Physics
                              Level 12, Bld 1 
                              PO BOX 123 Broadway
                              NSW, 2007, Australia

                              Armstrong, Nicholas
Mailing Address:                   University of Technology, Sydney
                              Dept of Applied Physics
                              Level 12, Bld 1 
                              PO BOX 123 Broadway
                              NSW, 2007, Australia

Technical Description:

In the most general sense, powder diffraction patterns consist of a set of intensity values, x-ray
or neutron, measured over a range of crystallographic d-spacings.  These patterns exhibit peaks
which result from the interference of coherent scattering of incident radiation from the periodic
crystal structure of the specimen.  The form of the pattern indicates the qualitative, quantitative,
crystallographic, and microstructural aspects of the sample.  Therefore, proper analysis of
diffraction patterns can provide considerable information about the specimen, giving rise to a
wide range of applications for this technique.

In order to gain this information, the effects from aberrations which are a result of the optical
character of the equipment must be deconvolved from the observations to yield the desired
measurement data.  A function of NIST powder diffraction SRMs is to allow for the description,
and possible removal, of the effects of equipment optics.  NIST SRMs accomplish this by
providing traceability of user measurements to fundamental physical constants or, alternatively,
to values determined through round robin studies.

The three variables associated with diffraction equipment which can be evaluated with NIST
powder diffraction SRMs are: 1) the d-spacing or line position, 2) line intensity as a function of
position, or instrument sensitivity, and 3) instrumental and sample contributions to the shape of
reflection profiles.  Additional powder diffraction SRMs are designed for quantitative analysis
with the use of the internal standard method.  In order to serve as an SRM for powder
diffraction, a material must be environmentally stable, particularly with respect to certified
property.  The microstructure must be such that errors in the user measurements, such as
preferred orientation and particle counting statistics, etc., are minimized.  Certification
measurements are designed to determine the certified property as accurately as possible and
ensure that the SRM is homogeneous.

Line Position SRMs

There are two SRMs, certified with respect to lattice parameters, which are intended primarily
for line position measurement; SRM 640b (silicon powder), and SRM 675 (fluorophlogopite). 
The latter is for large d-spacing measurements.  The certified values of these SRMs are traceable
to the fundamental length standard through the wavelength of the x-ray source used for the
original measurements.  We are presently pursuing a new generation of line position SRMs which
will be certified via a robust linkage to the iodine stabilized HeNe laser length standard.  This
project has involved the construction of a multi-axis diffractometer with a rotational resolution
in the arc-second range.  In order to obtain independence from sample position errors, the
equipment utilizes a graded multilayer parabolic mirror to focus the divergent beam from the
conventional x-ray source into a high intensity parallel  beam.  The silicon powder to be used
for the SRM is being prepared from electronic grade P type single crystal boules.  The lattice
parameters of the single crystal material are being investigated with respect to interstitial, vacancy
and impurity concentration; these concentrations are considerably less than a part per billion.  The
surface character of the powder is also being considered; the surface energy will result in stresses
on the particles which will effect the measured lattice parameter.  We anticipate that the lattice
parameters will be certified to the parts per million range.

Instrument Sensitivity SRM 1976

This SRM consists of a sintered  Al2O3 plate which is certified with respect to 12 relative
intensity values from (25 to 145) degrees two theta (Cu K).  It was designed for sensitivity,
intensity as a function of two-theta, calibration of conventional x-ray diffraction equipment via
conventional methods, though it is also certified with respect to lattice parameters.  Use of the
SRM involves the collection of a set of intensity data which are then compared to the certified
values.  The Al2O3 plates of this SRM exhibit uniform levels of preferred orientation which
required the use of tolerance intervals for the statistical analysis of the certification
measurements.  Hence the data should be considered collectively to determine if trends indicate
whether or not a calibration curve should be applied.  The sensitivity of the equipment used for
certification was determined to be correct through a round robin study sponsored by the
International Centre for Diffraction Data, ICDD, thus anchoring the certified data of the SRM.

Line Profile SRMs

The observed diffraction profile  from the diffractometer consists of a sample profile convolved
with an instrument profile and superimposed with noise.  We can think of the sample profile as
being "embedded" in the observed profile and the aim of the problem is to numerically determine
the sample profile in the most general and complete manner.  The sample profile characterizes
the broadening due to crystallite size and micro-strain effects within the sample.  Although there
exist several methods of determining the sample profile they often require specific assumptions
concerning the functional form of the sample profiles being made or result in ill-conditioned
solutions.  The approach which has been developed to solve this problem is to apply the
Maximum Entropy method (MaxEnt). The MaxEnt method incorporates the a priori information
about the instrument profile, noise distribution as constraints and determines the solution which
maximizes the entropy with respect to these constrains. 

Once, the sample profile is determined the microscopic properties, such as the crystallite size and
micro-strain can be determined using the standard methods such as the Warren-Averbach (WA)
method.  However, the corresponding crystallite size and micro-strain analysis has revealed
limitations in the above method.  These limitations are: 1) that the micro-strain can only be
interpreted in terms of a Gaussian probability distribution function, 2) the crystallite size is
sensitive to experimental errors in the data and  3) the probability distribution for crystallite size
cannot be determined from the experimental data.

At present research work is concentrating on developing a generalized MaxEnt/Bayesian method
which could be applied to deconvolving and separating overlapped profile peaks and adopted for
crystallite size and micro-strain analysis. 

The instrumental contribution to observed line profile shape from x-ray diffraction equipment can
be characterized with SRM 660 (LaB6).  This material was selected through an ICDD sponsored
round robin which found that it was free of peak broadening due to crystallite size and micro-
strain effects.  Refinements of the SRM's evenly spaced, high intensity diffraction lines yield
precise values for parameters of the selected profile shape function.  Due to its certified lattice
parameters, SRM 660 can also be used for determining instrumental parameters through a
Rietveld refinement.  Under development is an SRM which will display the effects of particle
size induced profile broadening

Quantitative Analysis SRMs

Conventional methods of quantitative analysis are based on the Reference Intensity Ratio, RIR,
method.  This method entails the determination of the intensities of various diffraction line
profiles and relating them to quantitative data through the use of calibration mixtures.  The
baseline for this method is the presumed purity of the components of the calibration mixtures. 
A more accurate and precise method is Quantitative Rietveld Analysis, QRA, in which the
powder diffraction data are analyzed with Rietveld method.  This method entails the calculation
of the pattern from crystallographic, microstructural and equipment characteristics.  These
characteristics are related to the form of the pattern through a series of model functions.  The
difference between the calculated and observed pattern is then minimized by sequentially refining
the physical parameters contained in the model functions to obtain an accurate and precise
description of the specimen.  The baseline for this method is the quality of the fit between the
calculated and observed patterns.  

While both of these methods can be used to perform quantitative analysis without the use of an
internal standard, this is predicated by the assumption that the specimen has no amorphous
component.  In order to perform an accurate quantitative analysis which includes the amorphous
content, a standard of known phase purity must be used.  Thus, a major focus of the work in this
area has been the development of a measurement and certification method for the amorphous
content of SRM 676, a non-orienting alumina powder which is presently certified with respect
to lattice parameters and eight relative intensity values.  

The experimental approach is based on the comparison of the phase abundance of two phase
mixtures determined from the preparation procedure using an analytical balance, which includes
the amorphous component, to that determined from the diffraction data, which does not. 
Specimens consisted of 50-50 mixtures of SRM 676 and the silicon of SRM 640b.  This silicon
was crushed and jet milled from single crystal, electronic grade boules.  The data were collected
via neutron time-of-flight, TOF, and conventional x-ray powder diffraction.  The data were
interpreted with the assumptions that: 1) all amorphous material in the silicon was confined to
the surface and 2) that the surface area of the silicon was sufficiently small, relative to the
alumina, that the amorphous component of the silicon could be ignored altogether.  Analysis is
the refinements indicated that the TOF data were unbiased and thus the amorphous content of
the alumina was credibly determined.  Further experiments which are currently being performed
with specimens made from five lots of silicon wherein the surface area was systematically varied. 
This will allow for a rigorous test of possible systematic errors in the amorphous content
determination. 

SRM 674a consists of a set of five powders:  Al2O3, ZnO, TiO2 (rutile), Cr2O3, and CeO2,
which range in x-ray mass attenuation coefficients from (126 to 2203) cm-1 (Cu K).  The
materials available with this SRM permit the minimization of absorption contrast between the
standard and the specimen.  SRMs 1878a ( Quartz) and 1879a (cristobalite) were certified with
respect to amorphous content for analysis of silica containing materials in accordance with health
and safety regulations.  Quantitative analysis of the silicon nitride system can be performed with
SRM 656 which consists of two powders, one high in  content while the other is high in . 
They are certified with respect to / ratio and amorphous content.  

Technical Objectives:

Improve the accuracy and precision of powder diffraction measurements.

Accomplishments:

New methods of improved accuracy and precision have been developed.

Outcome:

The ability of researchers to establish linkage between a result obtained from powder diffraction
and a material property is improved.

PROJECT TITLE: Particle Size Distribution Measurements

PROGRAM TITLE:  Standard Reference Materials

Principal Investigator:

NIST Staff:
Designated Project Leader:  Kelly, James
Mailing Address:           NIST
                           Materials (223), A256
                      Gaithersburg, MD  20899
Telephone:                 (301) 975-5794
Fax Number:           (301) 990-8729

Technical Description:

Powder materials are generated with specific physical characteristics of shape, size, and chemical
inertness.  The particle size distributions for these materials are measured using  microscopic
imaging techniques .

Technical Objectives:

This research project is designed to assist industries utilizing powder materials.  Knowledge of
the particle size distributions of the powders is often a key factor in their industrial performance. 
NIST makes available powders of known size for calibration and testing of commercial sizing
equipment.

Output:

Standard reference materials of glass beads are now available in several ranges of particle sizes.

Impact:

Approximately 500 units per year of these size distribution standards are purchased by industry
for use in their quality control test programs.
PROJECT TITLE:  Development of Microhardness Standards

PROGRAM TITLE:  Standard Reference Materials

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Quinn, George D.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899
Telephone:                 (301) 975 5765
Fax number:           (301) 990 8729
E-mail address:            geoq@enh.nist.gov

Other NIST Principal investigator(s):  Pothier, Brian
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5778
Fax number:                    (301) 990-8729
E-mail address:                         

Technical Description:

Ceramic blocks with certified Knoop and Vickers hardnesses are prepared.  One hundred of each
Knoop and Vickers indenter ceramic hardness blocks are prepared.  These are Standard Reference
Materials (SRM) #2830 and #2831, respectively.  Each block has five indentations made and
measured by NIST.  The hardness is certified by NIST.  These SRM's will support two ASTM
hardness standards being developed concurrently. 

Technical Objectives:

The objective of this project is to provide the ceramic community with hardness SRMs for
calibration of testing machines.

Outcomes:

Certified hardness blocks for sale by the SRM office.  Supporting technical papers and reports
document the procedures used to prepare and use the SRM's.  Two ASTM standard test methods
based on this work are being balloted.

Accomplishments:

The Knoop SRM #2830 run was completed in December, 1995.  The blocks were made available
for sale in January, 1996.  

A new ASTM Standard Test Method for Knoop Indentation Hardness of Advanced Ceramics,
which relies in part on SRM 2830, was adopted as C 1326-96 in January, 1996.

A new ASTM Standard Test Method for Vickers Indentation of Advanced Ceramics, which relies
in part on SRM 2831, was adopted as C 1327-96 in January, 1996.

A hardness round robin was conducted in 1994 and verified that both SRM's are completely
satisfactory.  The round robin also furnished useful precision and accuracy information that was
incorporated into the ASTM standards.

A new VAMAS (Versailles Project on Advanced Materials and Standards) round robin has been
organized for 1996 to study instrumented (recording) hardness.  A borosilicate glass and
prototype silicon nitride SRM 2830 specimens will be used.

Outputs:

Outputs include SRM #2830 and, in mid-1996, SRM #2831.  Round robin projects and reports
measured the robustness of the methods and furnished information for precision and bias
statements in two new ASTM standards.  The round robins also spread knowledge about the
SRM's.  Technical papers and reports support the standards:

R. J. Gettings, G. D. Quinn, A. W. Ruff, and L. K. Ives, "Development of Ceramic Hardness
Reference Materials," pp. 617-624 in New Horizons for Materials, Proceedings of the 8th World
Ceramic Congress, CIMTEC, Florence, Italy, ed P. Vincenzini, Techna, Faenza, 1995.

R. J. Gettings, G. D. Quinn, A. W. Ruff, and L. K. Ives "Hardness Standard Reference Materials
(SRM's) for Advanced Ceramics," VDI Berichte 1194, 1995, pp. 255-264.  Proceedings of the
International Symposium on Hardness Testing in Theory and Practice," Dusseldorf, Nov. 1995.

R. Gettings, G. Quinn, W. Ruff, and L. Ives, "New Hardness Standard Reference Materials
(SRM's) for Advanced Ceramics," Ceram. Eng. and Sci. Proc., Vol. 15, #5, 1994, pp. 717-826.

ASTM C 1326-96, Standard Test Method for Knoop Indentation Hardness of Advanced
Ceramics, January, 1996.

ASTM C 1327-96, Standard Test Method for Vickers Indentation Hardness of Advanced
Ceramics

Impact:

Hardness is a frequently measured property used to characterize one of the key attributes of
ceramics.  The state of the art of hardness testing of ceramics is such that much published data
is unreliable or worthless.  The advent and propagation of these SRM's in conjunction with two
supporting ASTM standards will rectify this state of affairs.  Reliable, accurate and precise data
should become the norm.

These SRM's and the ASTM standards are expected to have a worldwide impact and already are
influencing work on a draft ISO standard in ISO Technical Committee 206, Fine Ceramics.

PROJECT TITLE: Glass Standards and SRMs

PROGRAM TITLE: Standard Reference Materials

NIST Staff:
Designated Project Leader:  Cellarosi, Mario
Mailing Address:           NIST
                      Materials (223), A256
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-6123
Fax Number:           (301) 975-8729
E-Mail Address:            Cellarosi @ENH.NIST.GOV

Principal investigator(s) outside NIST:  Hagy, H.E.
Mailing Address:                     Corning Inc.
                                5 Fox Lane West
                                Painted Post, N.Y. 14870
Telephone:                           (607) 974-2166

Technical Description:

This project provides technical support in collaborations with industrial laboratories in the
development of glass SRMs and related methodologies related to glass and glass products.

Glass SRMs and standards priorities are established through formal ballots by producer/user
industries and other interests. Current activities span across a list of endeavors for new and
replacement SRMs.

Glass SRMs and related measurements are very important to the Glass Industry for R&D,
productivity, quality control, and also to other industries using glass in high technology
applications such as electrical and electronics products, communication, TV, and electro-optics
and fiber optics devices.  Technical activities include the identification of appropriate candidate
materials, procurement of materials, homogeneity studies, organization and coordination of round
robins, measurements protocols, interpretation of data, and fitting the data to predictive models.

Technical Objectives:

The objective of this program is to assist industry in the development of measurements, standards
and SRMs related to glass and glass products.

Outcomes:

In the near term, principal outcomes of this program involve the development of new glass SRMs
for Viscosity for a Lead-Silica composition, Thermal Conductivity/Diffusivity of a Glass
Ceramic, Glass Density SRMs for Soda-Lime and Borosilicate compositions and Quartz, and
Viscosity Fixpoints for Annealing, Softening and Strain Point of Quartz. Over the longer term,
the current list of priorities includes SRMs for Thermal Expansion, Heat Capacity, Glass
Transition, Crystallization, and Remelt Temperatures, and Stress Analysis. 

Accomplishments:

SRM 717A for the Viscosity of Borosilicate Glass was certificated in 1995, and this SRM is now
available for sale by NIST.

This SRM will play an important role in R&D, quality control in manufacturing, pollution
control, and in optimization of energy usage which is a large cost factor in glass melting. 

Outputs:

The results of this research program and rationale for priorities are discussed and reviewed in full
with industrial and academic collaborators on a semi-annual basis.

Technical Publications: 

Certificate for SRM on Viscosity of a Borosilicate Glass, Sept. 1995

                             SUPERCONDUCTIVITY

A significant program in high-Tc (critical transition temperature) superconductivity is being
conducted in MSEL and other Laboratories at NIST.  The primary focus of the MSEL Program 
is on bulk superconducting materials for wire and magnet applications.  In conducting this
program, researchers in MSEL work closely with their counterparts in other NIST Laboratories,
and collaborators in U.S. industry and other National Laboratories.

The primary thrusts of the program are as follows:

    Phase equilibria - Work is being conducted in close collaboration with the U.S.
     Department of Energy (DOE) and its national laboratories to provide the phase diagrams
     necessary for processing these unique ceramic materials.  A prime objective is the
     development of  the portions of the phase diagram for the Pb-Bi-Sr-Ca-Cu-O system
     relevant to production of  the high Tc materials.

    Flux pinning - This project makes use of a unique magneto-optical imaging facility to 
     examine flux pinning in a variety of materials.  Much of this work is being conducted in
     conducted in collaboration with American Superconductor Corporation.  In addition
     techniques for better interpretation of magnetic measurements are being developed.

    Damage mechanisms - Work is being conducted under a joint CRADA (cooperative
     research and development agreement) with American Superconductor Corporation as part
     of the "Wire Development Group" which involves a number of DOE National
     Laboratories and the University of Wisconsin to elucidate the effects of strain on the loss
     of current in superconducting wires.  The primary tool being employed is the use of
     microfocus radiography available at the NIST beamline at the Brookhaven National
     Laboratory.

    Database - A high-Tc superconductor database has been developed in collaboration with
     the National Research Institute for Metals (NRIM) in Japan.  The High-Temperature
     Superconductor Database (HTSD) includes evaluated open-literature data on numerous
     physical, mechanical, and electrical properties of a variety of chemical systems.  The first
     version of the database is now for sale by the Office of Standard Reference Data.

    Crystal structure - Thermal neutron diffraction techniques and profile refinement analyses
     are being utilized to investigate crystal and magnetic structures, composition, and crystal
     chemical properties.  This research is being carried out in collaboration with a number
     of industrial and university experts.

For further information about the High-Tc Superconductivity Program, please contact S. W.
Freiman at 301-975-6119 or e-mail requests to Freiman@micf.nist.gov.

PROJECT TITLE:  Phase Equilibria Relations of High Tc Superconductors

PROGRAM TITLE:  Superconductivity

Principal investigator(s):  

NIST Staff:
Designated Project Leader:  Vanderah, Terrell A.
Mailing Address:              NIST
                         Materials (223), A256
                         Gaithersburg, MD 20899
Telephone:                    (301) 975-5785
Fax Number:              (301) 990 8729
E-mail Address:               terrell@credit.nist.gov

Other NIST Principal investigator(s):  Wong-Ng, Winnie
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899 
Telephone:                          (301) 975-5791
Fax Number:                    (301) 990-8729

                               Cook, Lawrence P.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899

                               Drews, Andrew R.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5786
Fax Number:                    (301) 990-8729

Technical Objectives:

Conduct phase-equilibria studies of superconducting materials with emphasis on regions pertinent
to the processing of bulk conductors.  Determine the primary crystallization field of the bismuth-
strontium-calcium-copper oxide "2212" superconductor in air and investigate the effect of silver
impurities.  Investigate phase relations of thallium 1223-type superconductors with emphasis on
melting behavior and associated thallia vapor pressures.  Conduct high-temperature X-ray powder
diffraction studies of Pb-BiSCCO "2223" wire precursor material as a function of oxygen partial
pressure.  

Accomplishments

The approximate primary crystallization field of the BiSCCO "2212" superconductor has been
determined in air and encompasses a mole fraction compositional range of (20 to 42)% BiO1.5,
(15 to 35)% SrO, (2 to 25)% CaO, and (20 to 43)% CuO.  Ag enters the melts at saturation
levels of (6 to 8)% and depresses the solidus by as much as 26C.  Cu also substitutes into Ag,
lowering its melting temperature.  The 2212 BiSCCO superconductor melts incongruently to
liquid plus alkaline-earth-rich phases and exhibits a eutectic at 825C (Bi:Sr:Ca:Cu =
41.7:16.1:22.3:19.9).  Melt compositions and associated thallia vapor pressures have been
determined for three different thallium 1223-type superconducting compositions; thallia vapor
pressures were found to be highly variable with substituent type.  In contrast, the compositions
of the melts were relatively insensitive to substituent-type and characteristically Cu-, Pb-, and Bi-
rich and alkaline-earth-poor.  High-temperature X-ray diffraction studies of Pb-BiSCCO 2223
wire precursor were conducted on silver foil under varying oxygen partial pressure and at
different heating rates.  Melting, recrystallization, and orientation phenomena were found to be
markedly dependent on heating rate, the presence of silver, and oxygen partial pressure.

Outputs:

"Melting Equilibria of the Bi-Sr-Ca-Cu-O (BSCCO) System in Air.  I.  the Primary
Crystallization Phase Field of the "2212" Phase and the Effect of Ag Addition", W. Wong-Ng,
L.P. Cook, and F. Jiang.  In final preparation.

"Melting Equilibria of the Ba-Y-Cu-O System in the Vicinity of the Ba2YCu3O6+x Phase Field",
W. Wong-Ng and L.P. Cook.  Submitted to Journal ACerS.

"Comparative Melting and Vaporization Behavior of Doped Thallium 1223 Phases:  Preliminary
Results in Oxygen", L.P. Cook and W. Wong-Ng.  Submitted to NIST Journal of Research.

"High-Temperature X-ray Studies of Growth and Texturing of Bi-2223 on Silver", A.R. Drews,
J.P. Cline, T.A. Vanderah, and K. Salazar.  In final preparation.

PROJECT TITLE:  Microstructural Characterization of Bi-2223/Ag Tapes

PROGRAM TITLE:  Superconductivity

Principal Investigator:

NIST Staff:
Designated Project Leader:   Spal, Richard D.
Mailing Address:               NIST     
                          Materials (223), A163
                          Gaithersburg, MD 20899
Telephone:                     (301) 975-4028
FAX number:               (301) 990-8729
E-mail Address:                rspal@tiber.nist.gov

Principal Investigator(s) outside NIST:     Riley, Bart
Mailing Address:                     American Superconductor Corp.
                                Two Technology Drive
                                Westborough, MA 01581
Telephone:                           (508) 836-4200
FAX number:                     (508) 836-4248
E-mail address:                      briley@asc.mhs.compuserve.com

Technical Description:

Multifilamentary Bi-2223/Ag composite tapes are tensilely strained on axis from (0 to 1)%, and
the damage is studied in-situ and nondestructively by means of synchrotron-radiation
microradiography at 24.4 keV.  An asymmetric Bragg diffraction microscope is used to obtain
digital microradiographs with a pixel size of 0.5 m.  The crack density, the dimensions of the
crack opening and the strain distribution are determined.  Displacements as small as 0.2 m can
be resolved by sub-pixel interpolation.

Technical Objectives:

The broad objective is to characterize strain-induced damage in composite tapes and to relate it
to electrical performance.  A specific objective is to identify the microstructure which maintains
a continuous superconducting path through tapes that are strained well beyond the elastic limit
of the superconductor.  Such high strain should crack the brittle superconductor and disrupt the
superconducting path, but surprisingly the critical current is reduced by only one order of
magnitude.

Outcomes:

This project is expected to reveal ways to increase the critical strain, defined as the strain at
which the critical current begins to degrade, beyond the present value of about 0.5%, and thereby
broaden the range of commercial applications for superconducting composite tapes.

Accomplishments:

A model microstructure of tapes strained past the critical strain, featuring no continuous
superconducting path through the tape, was proposed based on microradiography and optical
microscopy data.  However, the calculated electrical resistance of the model tape disagrees
strongly with measurements.  To achieve agreement, while maintaining consistency with the
imaging results, the existence of a narrow superconducting bridge across the cracks is proposed.
Microradiographs of tapes strained to 1% show cracks extending across the full width of
individual filaments and repeating about every 0.75 mm along the tape.  Optical micrographs of
a longitudinal section of one tape confirm these results, and show that a crack in one filament
is generally accompanied by (and aligned with) cracks in every other filament in the section.  The
crack opening dimensions, determined from the microradiographs, account for most of the
macroscopic strain, suggesting that the filament segments between the cracks may be undamaged.

These results, taken alone, suggest that there is no continuous superconducting path through the
tapes, implying that they should exhibit electrical resistance due to current flow in the silver
around the cracks.  However, the measured resistance at low (ideally infinitesimal) current is over
one order of magnitude smaller than that calculated for an appropriate model geometry.  This
large discrepancy suggests that there is a superconducting bridge across the cracks, which is
consistent with the imaging results only if the bridge has significantly smaller cross section than
a filament, making it hard to observe.  It is reasonable to suspect that the bridge exists at the
silver interface, where the microstructure may differ from inside the filament.

Impact:

In cooperation with industrial partners, a more realistic model for the microstructure of
superconducting composite tapes, which has resulted from this project, has been used to obtain
a better understanding of the relationship between the tape microstructure and the electrical
properties. 

PROJECT TITLE:  Magneto-Optic Imaging of High Temperature Superconductors

PROGRAM TITLE:  Superconductivity

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Kaiser, Debra L.
Mailing Address:              NIST
                         Materials (223), A329
                         Gaithersburg, MD 20899
Telephone:                    (301) 975-6759
Fax Number:              (301) 990-8729
E-mail Address:               dkaiser@enh.nist.gov

Other NIST Principal investigator(s):  Turchinskaya, Marina (Guest Scientist)
Mailing Address:                   NIST
                              Materials (223), A329
                              Gaithersburg, MD 20899
Telephone:                         (301) 975-4073
Fax Number:                   (301) 990-8729

Technical Description:

A magneto-optic imaging system originally developed in Russia has been placed into operation
at NIST in order to study flux pinning mechanisms in high temperature superconductors.  High
flux pinning densities are needed for increasing the electrical current carrying capabilities of high
temperature superconductors.  Magneto-optic imaging is proving to be highly useful in visualizing
and evaluating flux pinning densities.

Technical Objectives:

To provide U.S. industry with evaluation techniques and data which will accelerate the
commercialization of high temperature superconductors for electrical power transport.

Accomplishments:

Magneto-optic has been very useful in evaluating the performance of cast tapes of the
superconductor Bi2Sr2CaCu2Oz (hereafter called BSCCO), a leading candidate material for
electrical power applications.

Microscopic flux flow in undoped and Li-doped BSCCO cast tapes before and after neutron
irradiation was studied by means of a magneto-optical imaging technique in order to correlate
flux flow with the microstructure.  Flux penetration was very nonuniform, indicating that current
flow in the specimens is inhomogeneous.  The neutron irradiation treatment increased flux
pinning in both the undoped and Li-doped tapes.  These results are important in understanding
the effect of microstructure and irradiation on the critical current density of BSCCO.

More recently, the magneto-optical imaging system was used to study magnetization and
demagnetization in composite tapes from American Superconductor Corporation that are
composed of superconducting BSCCO filaments embedded in a silver matrix.  BSCCO filaments
located up to 112 m below the unpolished surface of a composite tape could be imaged directly
through the outer silver sheath.  The magneto-optical images provided information on the
morphology and alignment of the upper layer filaments in the tape, the relative depths of these
filaments from the tape surface, and the homogeneity of the magnetic flux distribution within
these filaments.  These characteristics should prove useful in predicting the performance of the
composite in service.  Furthermore, our results demonstrate that magneto-optical imaging could
be a routine diagnostic tool for these materials.  These measurements demonstrate the utility of
that magneto-optical imaging for nondestructive analysis of composites containing high Tc
superconductors.  

Outputs:

Technical Papers:

"Magnetic Flux Penetration in Undoped and Li-Doped Bi2Sr2CaCu2Oz Cast Tapes Before and
After Neutron Irradiation," M. Turchinskaya, D. L. Kaiser, A. J. Shapiro, and J. Schwartz,
Physica C 246, 375 (1995).

"Magneto-transport Behavior of Polycrystalline YBa2Cu3O7: A Possible Role for Surface
Barriers," Shi Li, M. Fistul, J. Deak, P. Metcalf, G. F. Giuliani, M. McElfresh, and D. L. Kaiser,
Phys. Rev. B. in press.

Impact:

The NIST measurements are enabling American Superconductor Corporation to monitor progress
in developing tapes made of high temperature superconductors for transmission of electrical
power.

PROJECT TITLE:  Materials Property Database for High Temperature Superconductors

PROGRAM TITLE:  Superconductivity

Principal investigator(s):

NIST Staff:  
Designated Project Leader:  Munro, Ronald G.
Mailing Address:               NIST
                          Materials (223), A256
                          Gaithersburg, MD 20899
Telephone:                     (301) 975-6127
Fax number:               (301) 990-8729
E-mail address:                Munro_rg@enh.nist.gov

Other NIST Principal investigator(s):  Begley, Edwin F.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6118
Fax number:                    (301) 990-8729
E-mail address:                     begley@enh.nist.gov

                               Chen, Hailong (Guest Scientist)
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-4277
Fax number:                    (301) 990-8729
E-mail address:                     hailong@enh.nist.gov

                               Harris, Joyce F.
Mailing Address:                    NIST
                               Materials (223), A256
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-6045
Fax number:                    (301) 990-8729
E-mail address:                     jharris@enh.nist.gov

Principal Investigator(s) Outside NIST:

Project Leader (Japan):  Nishijima, Satoshi
Mailing Address:          NRIM
                     2-3-12, Nakameguro, Meguroku
                     Tokyo 153, Japan

                    Asada, Yuji
Mailing Address:         NRIM
                    2-3-12, Nakameguro, Meguroku
                    Tokyo 153, Japan

Technical Description:

This project is designed to facilitate technological advances in materials science by providing
evaluated thermal, mechanical, and superconducting property data for the broad class of materials
commonly called high temperature superconductors.

Technical Objectives:

The objective is to provide industry a reliable knowledge base for understanding material
property and performance relationships.  Use of the technically evaluated data enables industry
to save substantial time, effort, and precious funds.

Outcomes:

Several significant results are expected from this project:  (1) a comprehensive set of evaluated
data; (2) a software interface to the database; (3) standards and methodology for data evaluation;
and (4) relations and models for properties and performance characteristics.

Accomplishments:

The first version of the database has been designated as NIST Standard Reference Database 62:
High Temperature Superconductors (HTS), Version 1.  All phases of the development and testing
of the database have been completed, and the database packages are now being distributed by the
NIST Standard Reference Data Program.  This is the first publicly available materials property
database on HTS materials.

An agreement to collaborate with a similar project in Japan, at the National Research Institute
for Metals (NRIM) has been signed by representatives of NIST and NRIM to provide a more
efficient coverage of the worldwide effort.  This collaboration will enable U.S. efforts to access
important data, particularly from Japan, that would not otherwise be readily available.

Outputs:

Database:

NIST Standard Reference Database Number 62: High Temperature Superconductors, Version 1,
1995.

Technical Papers:

Reference Relations for the Evaluation of the Materials Properties of Orthorhombic YBa2Cu3Ox
Superconductors, R. G. Munro and H. Chen, J. Am. Cer. Soc. (1995).

Impact:

High temperature superconductors form the most intensely studied class of materials among all
the types of materials that may be considered advanced or high-technology materials.  The
average publication rate since the discovery of the materials in 1986 has been on the order of
5000 papers per year.  The resulting abundance of data has created serious challenges to
accessing the essential data and to resolving the wealth of inconsistencies that may be found
among the sets of property data.  The HTS database provides a significant effort to overcome
these barriers to the key technological information.

                           SYNCHROTRON RADIATION

The Materials Microstructural Characterization Group in the Ceramics Division operates two x-
ray experimental stations at the National Synchrotron Light Source (NSLS), where researchers
from NIST, industry, universities and other government laboratories carry out state-of-the-art
measurements on ceramic, semiconductor, photonic, metallurgical, biological, and other materials
of high scientific or technological interest.  X-ray measurement capabilities include ultra-small-
angle scattering (USAXS), topography, diffraction-imaging microscopy, x-ray absorption fine
structure spectroscopy (XAFS), standing-wave x-ray scattering (SWXR), and reaction-kinetic
surface science measurements.  

The range of studies performed over the past year include processing-microstructure relationships
in plasma-sprayed ceramic deposits, sintering of nanostructured ceramics, strain-induced
microcracking in high-Tc superconducting composite tapes, grain-size/pore-size trajectories within
ceramic microstructures during processing, diffraction imaging of ZnSe, strain and bond distortion
in ultra-thin semiconductor films, and the determination of atomic-scale and molecular-scale
structures at technologically important surfaces and interfaces.  

In addition, as part of a national facility, time on the NIST instruments at the NSLS is made
available to qualified researchers based on peer-reviewed proposals.  In the past year, researchers
from chemical, aerospace, energy and materials production industries as well as from NIST
laboratories, other government laboratories and universities have completed experiments that
could not have been performed elsewhere in the United States.  The long-term goal of research
at these facilities is to enable researchers to address basic issues so that U.S. manufacturers can
provide superior materials based on structural information not available elsewhere.  

Looking toward the future, the NIST Materials Science and Engineering Laboratory (MSEL) has
entered a Collaborative Access Team (CAT) agreement with the University of Illinois, Oak Ridge
National Laboratory, and U.O.P. Corporation, the purpose of which is to build and operate x-ray
instruments on sector 6 at the Advanced Photon Source (APS) now under construction at the
Argonne National Laboratory.  The CAT is called UNI-CAT in recognition of the University,
National Laboratory, and Industrial components of this team.  This partnership is particularly
attractive to us at NIST because there is significant overlap with current and future NIST
interests.  

The APS will offer a 102-104 increase in brilliance compared to the best synchrotron x-ray
sources of today.  In the years to come, the APS will supplant the NSLS as this nation's premier
x-ray source.  The APS beamlines now being built by UNI-CAT incorporate the newest
technology which will not only enable NIST scientists to improve significantly our real-time x-
ray microscopy, ultra-small-angle x-ray scattering, in-situ x-ray topography and EXAFS
capabilities, but will also offer opportunities for cutting-edge experiments in structural
microcrystallography (and time-resolved structural scattering), surface/interface scattering, diffuse
scattering, and magnetic scattering.  NIST scientists will extend our present portfolio of
characterization capabilities to include an even wider range of materials measurement of
importance to materials scientists and to U.S. industry.  

For further information on the Synchrotron Radiation Program, contact Gabrielle Long at 301-
975-5975 or e-mail to gabrielle@enh.nist.gov.

PROJECT TITLE:  Materials Science at the NSLS

PROGRAM TITLE:  Synchrotron Radiation

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Long, Gabrielle G.
Mailing Address:           NIST
                      Materials (223), A163
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5975
FAX number:           (301) 990-8729
E-mail Address:            gabrielle.long@nist.gov

Other NIST Principal investigator(s):  Allen, Andrew, J.
                               Black, David R.
                               Burdette, H. E.,
                               Fischer, Daniel A.
                               Spal Richard D.
                               Woicik, Joe G. 
Mailing Address:                    NIST
                               Materials (223), A163
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5972
Fax number:                    (301) 990-8729

Technical Description:

The Materials Microstructural Characterization Group operates two x-ray experimental stations
at the National Synchrotron Light Source (NSLS) where researchers from NIST, industry,
universities and government laboratories carry out state-of-the-art measurements on ceramic,
semiconductor, photonic, polymeric, biological, and other materials of scientific and/or
technological interest.  In addition, a new soft-x-ray materials-science end station for the study
of materials containing carbon, nitrogen, oxygen and fluorine has been designed, built and
commissioned.  This experimental station, which delivers state-of-the-art intensity, resolution, and
detection sensitivity, is the product of a collaboration between NIST, The Dow Chemical Co.,
the Physics Department at Brookhaven National Laboratory, and two industrial awardees of
SBIRs.  Problems which are currently being investigated include model catalyst systems, polymer
surfaces and their interfaces, and self-assembled monolayers.

Technical Objectives:

The objectives are to investigate processing / microstructure / property relationships in ceramic
materials of high technologocal interest; to perform state-of-the-art diffraction imaging of
semiconductor, superconductor and photonic single crystals; to develop a model of
tensile-strained high-TC superconducting tapes; to probe bulk and surface structures of important
low-atomic-number materials in a reactive environment.

Outcomes:

Through the use of the NIST portfolio of leading-edge materials science experiments, researchers
will address basic issues regarding processing/microstructure/property  relationships; will
determine the structure at the surfaces of materials containing carbon, nitrogen, oxygen, and
fluorine, including active-site chemical  analysis;  will be able to understand the electrical
conductance around cracks which develop during tensile straining; and will correlate the defect
structures in single crystals with the product properties.

Accomplishments:

1.   The effects, on the microstructural development during cement hydration, of adding
     pozzolanic additives to cements and concretes, in the form of silica fume, have been
     extensively studied using small-angle neutron scattering (SANS) and ultra-small-angle
     x-ray scattering (USAXS).

2.   A model microstructure of tapes strained past the critical strain, featuring no continuous
     superconducting path through the tape, was proposed based on microradiography and
     optical microscopy data.

3.   Small-angle scattering was applied to the quantitative characterization of the crack and
     pore microstructure of plasma-sprayed deposits.  The anisotropic character  of the
     microstructure has been observed and the methods and techniques for separating the
     intralamellar crack population from the interlamellar pore population have been 
     developed, in which the surface areas and volume of each are derived.

4.   A detailed chemical and structural understanding of the lubricant-to-substrate interface
     was obtained for stearic acid.
 
5.   The defect density of selected areas of undoped ZnSe grown by SPVT was found to be
     as low as (103 to 104) cm-2, which is comparable to defect densities now achievable for
     other compound semiconductor materials.  Devices grown on wafers from this particular
     boule were observed to have the longest measured lifetime.
 

6.   The characteristic microstructure of each of the classes of diamond has been identified
     and the relationship between substrate quality and film defects has been documented.

7.   The strain and bond distortions in epitaxial InAs, InGaAs and thicker InAs films have
     been studied via x-ray standing-wave and x-ray-absorption fine structure measurements. 
     The results indicate that, for both InAs and InGaAs monolayers, strain and bond
     distortions are accurately described by macroscopic elastic theory.

Outputs:

Technical Papers:

A. J. Allen and R. A. Livingston; "Small-Angle Scattering Study of Concrete
Microstructure as a Function of Silica Fume, Fly Ash or Other Pozzolanic Additions", (SP
153-62) in Proc. 5th CANMET/ACI International Conference on Fly Ash, Silica Fume, Slag and
Natural Pozzolans in Concrete, June 1995. Ed. V. M. Malhotra. American Concrete Institute,
Detroit, MI. 1179-1200 (1995). 

J. Ilavsky, H. Herman, C. C. Berndt, A. N. Goland, G. G. Long, S. Krueger, and A. J.
Allen,"Porosity in Plasma-Sprayed Alumina Deposits" in Thermal Spray Industrial Applications,
C. C. Berndt and S. Sampath, Eds. (ASM International, 1994) 709-714.

D. A. Fischer, Z. Hu, and S. M. Hsu, "Molecular Orientation and Bonding of Monolayer Stearic
Acid on a Copper Surface in Air,"  for submission to Tribology Letters.

D. A. Fischer, Z. S. Hu, and S. M. Hsu, "Tribochemical and Thermochemical Reactions of
Stearic Acid on Copper Surfaces in Air as Measured by Ultra Soft X-ray Absorption
Spectroscopy, " for submission to Tribology Letters.

D. B. Eason, Z. Yu, W. C. Boney, J. W. Cook, Jr., J. F. Schetzina, D. R. Black,
G. Cantwell, and W. C. Harsch, "High-brightness light-emitting diodes grown by MBE on ZnSe
substrates," Proc. Of PCSI Conf., Phoenix, AZ, Jsn. 9 - 13, 1995.

D. Black, H. Burdette, and G. Cantwell,  "X-ray diffraction imaging of ZnSe,"
Symp. On Nondestructive Wafer Characterization for Compound Semiconductor Materials, Reno,
NV, May 21 - 26, 1995.

D. R. Black, H. E. Burdette and W. Banholzer, "X-ray diffraction imaging of man-made and
natural diamond," Diamond and Related materials 2 (1993) 121 - 125.

L. Robins, M. A. Plano, M. D. Moyer, M. A. Moreno, L. S. Pan, D. R. Kania, and W. F.
Banholzer, "The defect microstructure of thick homoepitaxial diamond films," Advances in New
Diamond Science and Technology, S. Saito, N. Fujimori, O. Fukunaga, M. Kamo, K. Kobashi
and M. Yoshikaswa, Eds. (MYU, Tokyo, 1994) p. 251

M. A. Plano, M. D. Moyer, M. A. Moreno, D. Black, H. Burdette, L. Robins, L. S. Pan, D. R.
Kania, and W. F. Banholzer, "Properties of thhick homoepitaxial diamond films," in Diamond,
SiC, and Nitride Wide-Bandgap Semiconductors, Materials Research Society Proceedings Vol.
339, C. Carter, Jr., G. Gildenblat, S. Nakamura and R. Nemanich, Eds., (MRS, Pittsburgh, 1994)
p. 307.

D. Black, H. Burdette, R. Linares and P. Doering, "X-ray diffraction imaging of free-standing
single-crystal CVD diamond films," in Proc. Fourth Int'l. Symp. On Diamond Materials, (May,
1995, Reno).

D. Black, H. Burdette, M. A. Plano, M. D. Moyer, M. Moreno, J. Ager, and A. Chen,
"Observation of individual defects in a homoepitaxial diamond film," in Proc. Fourth Int'l. Symp.
on Diamond Materials, (May, 1995, Reno).

PROJECT TITLE:  UNI-CAT Construction at the APS

PROGRAM TITLE:  Synchrotron Radiation

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Long, Gabrielle G.
Mailing Address:           NIST
                      Materials (223), A163
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5975
Fax number:           (301) 990-8729
E-mail Address:            gabrielle.long@nist.gov

Other NIST Principal investigator(s):  Allen, Andrew, J.
                               Black, David R.
                               Burdette, H. E.
                               Fischer, Daniel A.
                               Spal Richard D.
                               Woicik, Joe G. 
Mailing Address:                    NIST
                               Materials (223), A163
                               Gaithersburg, MD 20899
Telephone:                          (301) 975-5972
Fax number:                    (301) 990-8729

Technical Description:

The NIST Materials Science and Engineering Laboratory has entered into a Collaborative Access
Team (CAT) agreement with the University of Illinois, Oak Ridge National Laboratory and UOP
Corporation, the purpose of which is to build and operate x-ray experiments on Sector 33 of the
Advanced Photon Source (APS), now nearing completion at Argonne National Laboratory.  In
the years to come, the APS will become this nation's premier x-ray source for high-brightness
hard x-radiation.  The APS experimental stations now under construction will enable NIST
scientists to improve significantly our ultra-small-angle x-ray scattering and our real-time x-ray
imaging capabilities.  There will also be opportunities for cutting-edge experiments in structural
crystallography, diffuse scattering, surface/interface scattering, and magnetic scattering.

Technical Objectives:

The technical objectives are: (1) research at the cutting edge of the fields of materials science,
physics, chemistry, biology, chemical engineering, polymer science and geology, with emphasis
on close collaboration among scientists and engineers from universities, industries and national
laboratories.

Outcomes:

The NIST portfolio of synchrotron radiation capabilities will  be expanded to include: 
high-resolution diffraction and spectroscopy; diffuse x-ray scattering; surface and interface
diffraction and scattering during reconstruction, relaxation, roughening transitions, melting,
chemical reactions and phase transitions; magnetic x-ray scattering; as well as significantly
improving our present capabilities in ultra-small-angle x-ray scattering, x-ray diffraction
microscopy, and in situ XAFS.

Accomplishments:

On the UNI-CAT Insertion Device beam line, the first optical enclosure, the second optical
enclosure and both experimental hutches have been built. The monochromator and the
beam-conditioning table are in the final stages of construction.

PROJECT TITLE:  Microstructure of single-crystal and thin-film diamond

PROGRAM TITLE:  Synchrotron Radiation

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Black, David R.
Mailing Address:           NIST
                      Materials (223), A163
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5976
Fax number:           (301) 990-8729
E-mail Address:            david.black@nist.gov

Technical Description:

This project makes use of x-ray diffraction imaging (topography) to characterize the defect
microstructure of high-temperature/high-pressure (HTHP) diamonds, natural diamonds, and
homoepitaxial chemical-vapor- deposited (CVD) diamond films grown on single-crystal material.
Diamonds have an unusual combination of properties which would be extraordinarily useful in
electronic device technology.  CVD diamond offers an opportunity to create materials with both
high quality and low costs.  Limiting factors include the inability to grow single-crystal films by
heteroepitaxy, and the general material quality.  Presently, small diamond substrates are used to
grow homoepitaxial films to study the properties of CVD diamond. One way to reduce the cost
and increase the size of substrate crystals is known as the "tiling" method.  In this technique,
homoepitaxial CVD diamond films are grown and then removed from the single-crystal
substrates.  Several films are then arranged in a tiling to form a mosaic substrate for further CVD
growth of a larger crystal.   The effects on CVD diamond film quality of the recently-developed
electrochemical liftoff method to produce the free-standing crystals for tiling are being
investigated, and the tiling process is being examined to understand the effects of substrate
misorientation, crystallographic quality, strain and surface finish on the quality of the product
CVD crystal.

Technical Objectives:

The goals of this project are to: characterize the defect microstructure of the four classes of
diamond; evaluate each as substrates for deposition of homoepitaxial CVD diamond films;
investigate the relationships between defects in the substrates, growth processes and film quality;
relate film quality to electronic properties; and evaluate new methods for growing large area
single-crystal diamond films.

Outcomes:

It is expected that an increased understanding of the relationships between substrate quality,
growth processes and CVD diamond properties will improve the development of high-quality
diamond films for high-technology applications.

Accomplishments:

The characteristic microstructure of each class of diamond has been identified and the
relationship between substrate quality and film defects has been documented.

Outputs:

Technical Papers:

D. R. Black, H. E. Burdette and W. Banholzer, "X-ray diffraction imaging of man-made and
natural diamond," Diamond and Related materials 2 (1993) 121 - 125.

L. Robins, M. A. Plano, M. D. Moyer, M. A. Moreno, L. S. Pan, D. R. Kania, and W. F.
Banholzer, "The defect microstructure of thick homoepitaxial diamond films," Advances in New
Diamond Science and Technology, S. Saito, N. Fujimori, O. Fukunaga, M. Kamo, K. Kobashi
and M. Yoshikaswa, Eds. (MYU, Tokyo, 1994) p. 251.

M. A. Plano, M. D. Moyer, M. A. Moreno, D. Black, H. Burdette, L. Robins, L. S. Pan, D. R.
Kania, and W. F. Banholzer, "Properties of thick homoepitaxial diamond films," in Diamond,
SiC, and Nitride Wide-Bandgap Semiconductors, Materials Research Society Proceedings Vol.
339, C. Carter, Jr., G. Gildenblat, S. Nakamura and R. Nemanich, Eds., (MRS, Pittsburgh, 1994)
p. 307.

D. Black, H. Burdette, R. Linares and P. Doering, "X-ray diffraction imaging of free-standing
single-crystal CVD diamond films," in Proc. Fourth Int'l. Symp. On Diamond Materials, (May,
1995, Reno, Nevada).

D. Black, H. Burdette, M. A. Plano, M. D. Moyer, M. Moreno, J. Ager, and A. Chen,
"Observation of individual defects in a homoepitaxial diamond film," in Proc. Fourth Int'l. Symp.
on Diamond Materials, (May, 1995, Reno, Nevada).

Impact:

The improved understanding of the relationships between substrate quality, growth processes and
CVD diamond properties has had a positive influence on the development of high-quality
diamond films for high-technology applications.

PROJECT TITLE:  Strain and Relaxation in InAs and InGaAs Films on GaAs (001)

PROGRAM TITLE:  Synchrotron Radiation

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Woicik, J. C.
Mailing address:           Brookhaven National Laboratory
                      Building 510 E
                      Upton, NY 11973
Telephone:                 (516) 344-5236
Fax number:           (516) 344-5419
E-mail Address:            joseph.woicik@nist.gov                     

Other NIST Principal investigator(s):  Pellegrino, J. G.
Mailing Address:                    NIST
                               Technology (225), A305
Telephone:                          (301) 975-2123
E-mail address:                     joseph.pellegrino@nist.gov

Technical Description:

One of the primary obstacles hampering epitaxial growth is the fundamental limit of strain
accommodation in the overlayer film.  As more layers are added, the strain energy increases
proportionally, and above a critical thickness, it becomes energetically favorable for the film to
collapse through a network of misfit dislocations.  In this project, x-ray standing wave
measurements and x-ray absorption fine structure measurements are combined to determine the
atomic displacements and the bond lengths within buried interfaces grown epitaxially  on  single
crystal GaAs.  

Technical Objectives:

The objective of this research is to determine the bond lengths within buried interfaces of  InAs
and InGaAs grown epitaxially on GaAs (001) to determine the strain and relaxation at the buried
interfaces and to test the limits of elastic theory. 

Outcomes:

Despite the fundamental importance of strain accommodation in electronic materials, relatively
little work has been performed to understand the geometrical aspects.  The present research is
expected to resolve the ongoing controversy concerning the effects of strain on both lattice
constants and on bond lengths in thin films.

Accomplishments:

The strain and bond distortions in epitaxial InAs, InGaAs and thicker InAs films have been
studied via x-ray standing-wave and x-ray-absorption fine structure measurements.  The results
indicate that, for both InAs and InGaAs monolayers, strain and bond distortions are accurately
described by macroscopic elastic theory.  Thicker InAs films are found to collapse beyond a
critical thickness of about 2 monolayers, accompanied by a large degree of structural disorder
and bond-length relaxation.

Outputs:

Technical Paper:

J. C. Woicik, K. E. Miyano, J. G. Pellegrino, P. S. Shaw, S. H. Southworth, and B. A. Karlin,
"Strain and relaxation in InAs and InGaAs films grown on GaAs (001),"  Phys. Rev. B. (in
press).

Impact:

The present research has resolved an ongoing controversy concerning the effects of strain on both
lattice constants and on bond lengths in thin films.  The research has been able to demonstrate,
surprisingly, that macroscopic elastic theory can accurately account for the strain observed in an
atomic monolayer.
                            THEORY AND MODELING

Design and processing of advanced materials, such as monolithic fine ceramics with
heterogeneous microstructures, as well as fiber-reinforced metal/intermetallic/ceramic matrix
composites, is labor intensive, costly and still in the developmental stage.  Computational
materials theory, modeling, and computer simulations provide powerful new paradigms for
rationally designing, processing, characterizing, and prototyping these advanced materials.  Such
research ranges from the molecular design and understanding of these materials via first-
principles quantum mechanical calculations to micro-physical modeling of heterogeneous
microstructural features and properties to computer simulations of microstructural evolution and
subsequent physical properties   

Modeling and computer simulations at the mesoscopic or microstructural level is an exciting new
aspect of computational materials theory.  Such simulations, in orchestrated collaboration with
experimental development, provide an efficient stratagem for minimizing costs, time-to-
application in ultimate production strategies of ceramic components, and lifetime prediction
methodologies.  They generally involve four elements:  (1) simulation and/or representation
(usually digital) of a microstructure;  (2) simulation of important processing and physical
properties;  (3) comparison with experimentally measurable properties and (4) application to
design-improved microstructures for specific applications.

The projects in the Ceramics Division in materials theory, modeling, and computer simulations
are focused in two areas:  (1) first principles calculations of ceramic phase diagrams;
parameterization of microstructural properties; and (2) modeling of microstructures.

For further information on the Theory and Modeling program, please contact E. Fuller at (301)
975-5795 or e-mail to erfuller@enh.nist.gov. 

PROJECT TITLE:  Modeling of Microstructures

PROGRAM TITLE:  Theory and Modeling

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Fuller, Edwin R. Jr.
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-5795
Fax number:           (301) 990-8729
E-mail address:            Edwin.Fuller@nist.gov

Other NIST Principal investigator(s):  Carter, W. Craig
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-3971
Fax number:                    (301) 990-8729
E-mail address:                     wcraig@pruffle.nist.gov

                               Roosen, Andrew R.
Mailing Address:                    NIST
                               Materials (223), A329
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-6166
Fax number:                    (301) 990-8729
E-mail address:                     roosen@borax.nist.gov

Technical Description:

This project is designed to elucidate the essential physics of microstructural evolution and to
develop computationally efficient algorithms for simulations of microstructural development.

Technical Objectives:

This research is designed to assist industry in developing new paradigms for elucidating
microstructural evolution through models of the essential physics and identification of
computationally feasible algorithms.  Particular objectives are to model large collections of
microstructural objects so as to capture the complexities which occur in materials, and to develop
and implement new mathematical techniques for modeling microstructural evolution.

Outcomes:

Major outcomes of this research are expected to include: (1) better, more useful, more robust and
more predictive models of materials processes, microstructures, and microstructural evolution;
(2) implementation of developed algorithms by industrial researchers; and (3) deeper
understanding of the fundamentals of materials behavior.

Accomplishments:

Simulation of anisotropic grain growth in silicon nitride illuminated the role of  microstructural
development in increasing the toughness of this material.  Statistics and process control
parameters are being understood at a microstructural level.

The physical processes associated with reactive wetting were clarified through studies of diffusion
and interface growth during reactive wetting.  This research has provided physical insight for
designers of joining techniques for ceramic materials.  Such techniques are a key technological
component in materials utilization.

Effects of stress, both applied and self-generated, were modeled for the sintering process. 
Sintering is the most important ceramic processing technique; this research represents the first
time that stress has been reckoned with physically rigorous approaches in realistic powder
compacts.

Classical thermodynamics associated with anisotropic surfaces and interface growth were
developed.  Beautiful and elegant mathematical techniques of convexification were used to unify
the description of diverse fundamental aspects in the field of ceramics: multicomponent phase
diagrams, anisotropic surface energies, and crystal growth shapes.  This important topic now has
a solid theoretical foundation which can only benefit the understanding and the application of
technological materials.

Outputs:

Several important outputs were derived from this project.  A letter of appreciation was received
from the duPont and IBM corporations signifying their appreciation for our successful efforts. 
Several research papers were produced from the technical advancements, which were made.

Technical papers published:

J. W. Cahn and W. C. Carter, "Crystal Shapes and Phase Equilibria: A Common Mathematical
Basis," Met. and Mat. Trans., in press.

R. M. Cannon, E. Saiz, A. P. Thomsia, and W. C. Carter, "Reactive Wetting Taxonomy"  MRS
Proc., 357, 279-291 (1995).

J. W. Bullard and W. C. Carter, "Numerical Determination of Critical Strain Rate for Neck
Rupture for Evaporation-Condensation Sintering of Isotropic Particles," in Proc. Sintering `95,
in press.

J. W. Bullard, E. J. Garboczi, W. C. Carter, and E. R. Fuller, Jr., "Numerical Methods for
Computing the Mean Curvature of an Interface," Comput. Mater. Sci., Vol. 4, 103-116 (1995).

Technical papers submitted for publication:

A. W. Searcy,  J. W. Bullard, and W. C. Carter, "Possible Explanations of Transient Neck
Formation between Pairs of 110 Faceted Particles," J. Am. Ceram. Soc., submitted.

J-H Choi, D-H Kim, B. J. Hockey, S. M. Weiderhorn, C. A. Handwerker, J. E. Blendell, W. C.
Carter, A. R. Roosen, "The Equilibrium Shapes of Cavities in Sapphire," J. Am. Ceram. Soc.,
submitted.

Impact:

DuPont is now using mathematical techniques developed at NIST to design better sintering
processes.  Many industrial researchers have asked that we model their particular problems and
have asked for use of our developed codes.

PROJECT TITLE:  Prediction of Phase Diagrams

PROGRAM TITLE:  Theory and Modeling

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Burton, Benjamin P.
Mailing Address:           NIST
                      Materials (223), A215
                      Gaithersburg, MD 20899-0001
Telephone:                 (301) 975-6043
Fax number:           (301) 990-8729
E-mail address:            burton@ilmenite.nist.gov

Other NIST Principal investigator(s):  McCormack, Ryan
Mailing Address:                    NIST
                               Materials (223), A215
                               Gaithersburg, MD 20899-0001
Telephone:                          (301) 975-5786
Fax number:                    (301) 990-8729
E-mail address:                     ryan@lurch.nist.gov

Technical Description:

This project is designed to calculate phase diagrams of technologically important ceramic
materials from first principles and to develop the theoretical techniques necessary to further these
calculations.

Technical Objectives:

This research is designed to assist industry by providing information on phase equilibria and
order/disorder configurations of technologically important classes of solid-solution ceramics. 
Such information is critical to the application of these materials because their ferroelectric,
magnetic, and transport properties can be sensitive functions of composition and quenched-in
cation order.  The information is provided via first-principles phase diagram calculations with
experimental verification of the results.  A technical objective is to assess the relative merits of
various techniques for calculating formation energies of ceramic compounds.

Outcomes:

Major outcomes of this research are expected to include: (1) first principles phase diagrams of
important relaxor ferroelectrics, (2) improved techniques for calculating formation energies of
ceramic compounds.

Accomplishments:

A first-principles calculation of the Pb(Sc0.5Ta0.5)O3-PbTiO3 (PST-PT) quasi-binary phase diagram
was completed using a Potential-Induced-Breathing/Cluster-Variational-Method (PIB/CVM). 
Results from these calculations include:

(a)  Predictions of three new unexpected ordered phases, their enthalpies of formation, and the
     maximum temperatures for which they are stable.

(b)  Ground-state analysis for the PST-PT system based on an 18-site cluster.

(c)  Calculation of a complete theoretical phase diagram for the PST-PT  system.

Preliminary results of the calculations for PST-PT solid solutions were published in
Ferroelectrics, and a final paper was published in Phys. Rev. B. 

Outputs:

This project has produced several research papers from the technical advancements which were
made.

Technical papers published:

B. P. Burton and R. E. Cohen, "Nonempirical calculation of the PST-PT Pb(Sc0.5Ta0.5)O3-xPbTiO3
quasibinary phase diagram," Phys. Rev. B52, 792 (1995).

B. P. Burton and R. E. Cohen, "First principles study of cation ordering in the system
Pb(ScTa)O3, and (1-x)Pb(ScTa)O3-xPbTiO3," Ferroelectrics 164, 201-212, (1995).

Technical papers submitted for publication:

P. D. Tepesch, A. F. Kohan, G. D. Garbulsky, G. Ceder, C. Coley, H. T. Stokes, L. L. Boyer,
M. J. Mehl, B. P. Burton, K. Cho, and J. Jannopoulos, "A model to compute phase diagrams in
oxides with empirical or first-principles energy methods and application to the solubility limits
in the CaO-MgO system,"  J. Am. Ceram. Soc., submitted.

                              OTHER PROJECTS

PROJECT TITLE:  Diamond film Research

PROGRAM TITLE:  Other Projects

Principle NIST Investigators:

NIST Staff:
Designated Project Leader:  Feldman, Albert
Mailing Address:           NIST
                      Materials (223), A329
                      Gaithersburg, MD 20899
Telephone:                 (301) 975-5740
Fax Number:           (301) 990-8729
E-Mail Address:            feldman@micf.nist.gov

Technical Description:

Carbide cutting tools coated with CVD diamond have lifetimes ten times or greater than those
of uncoated carbide tools provided that the coating does not delaminate.  At the present time,
delamination failure is detected only by lifetime testing under machining conditions, a time
consuming procedure.  We are currently investigating whether nondestructure techniques, thermal
wave imaging (Ceramics Division), scanning acoustic microscopy (Metallurgy Division) and
contact acoustic nonlinearity (Materials Reliability Division) can be used to predict premature
delamination failure.  The use and analysis of thermal imaging data may lead to an new method
of measuring thermal conductivity/diffusivity in CVD diamond.

Technical Objectives:

The objective of this project is to determine whether nondestructive procedures can be used to
predict premature debonding failure of cutting tools coated with chemical vapor deposited (CVD)
diamond.

Accomplishments:

As part of a working group on standardizing thermal conductivity measurements on CVD
diamond, NIST is assisting in coordinating an interlaboratory comparison (round robin) of
thermal conductivity measurement on a given set of specimens.  The purpose of the round robin
is to ascertain the most appropriate methods for measuring the thermal conductivities of chemical
vapor deposited (CVD) diamond specimens.  Measuring the thermal conductivity of CVD
diamond can be difficult because its thermal conductivity is higher than any material at room
temperature.  Ten laboratories have participated to date.  The results indicate a significant spread
in values obtained by the different laboratories.  It is believed that specimen inhomogeneity is
the main cause of much of the variability.  This activity is an outgrowth from a series of NIST
sponsored workshops on characterizing diamond films that has been held at NIST over the past
several years.

In order to provide a forum for exchange of scientific information, NIST serves as host to The
Applied Diamond Conference, ADC'95, the 3rd International Conference on the Applications of
Diamond Films and Related Materials.  Registered attendance was 385 with participation from
21 countries.  The topics covered included cutting tools, active electronics, cubic boron nitride,
diamond-like carbon, economic analyses, electronic packaging, heat management, negative
electron affinity, performance evaluation, sensors, optics, etc.

Outputs:

"Proceedings of the Applied Diamond Conference 1995, Applications of Diamond films and
Related Materials:  Third International Conference," NIST Special Publication 885 (USGPO,
1995)  A. Feldman, Y. Tzeng, W.A. Yarbrough, M. Yoshikawa, and M. Murakawa editors.

NISTIR 5692, Supplement to NIST Special Publication 885, Proceedings of the Applied Diamond
Conference 1995 (1995), A. Feldman, Y. Tzeng, W.A. Yarbrough, M. Yoshikawa, and M.
Murakawa editors.

"The Promise of Diamond Optics," A. Feldman and D. C. Harris in Laser Damage in Optical
Materials:  1994, H. E. Bennett, A. H. Guenther, M. R. Kozlowski, B. E. Newnam, M. J.
Soileau, Editors, Proc. SPIE 2428, pp. 580-590 (1994).

"A Closed CVD System for the Deposition of Diamond Films,"  E. N. Farabaugh, G. R. Lai, A.
Feldman, and L. H. Robins in NIST Special Publication 885, Applications of Diamond Films and
Related Materials:  Third International Conference, A. Feldman, M. Yoshikawa, Y. Tzeng, and
M. Murakawa, Editors (USGPO, 1995) p. 361-364.

"Round Robin Thermal Conductivity Measurements on CVD Diamond,"  by A. Feldman in NIST
Special Publication 885, Applications of Diamond Films and Related Materials:  Third
International Conference, A. Feldman, M. Yoshikawa, Y. Tzeng, and M. Murakawa, editors
(USGPO, 1995) p. 627-630.

Outcomes:

There are two possible outcomes of this research:  1) development of a nondestructive adhesion
test for diamond coated cutting tools to replace operational testing; 2) development of a new
method to measure thermal conductivity/diffusivity.

PROJECT TITLE:  Advanced Technology Program (ATP) Assessment and Support

PROGRAM TITLE:  Other Projects

NIST Staff:
Designated Project Leader:  Dapkunas, S. J.
Mailing Address:           NIST
                      Materials (223), A259
                      Gaithersburg, MD  20899
Telephone:                 (301) 975-6119
Fax Number:           (301) 990-8729
E-Mail Address:            dapkunas@micf.nist.gov

Other NIST Principal investigator(s):  Carpenter, J. A.
Mailing Address:                   NIST
                              Materials (223), A263
                              Gaithersburg, MD  20899
Telephone:                         (301) 975-6397
Fax Number:                   (301) 990-8729
E-Mail Address:                    carpent@micf.nist.gov

Technical Description:

ATP general competitions which included materials topics and a focussed competition on
Materials Processing for Heavy Manufacturing were held to select projects of a high risk nature
which, if successful, would enhance the technological and competitive position of domestic
industry.  Ceramics Division staff, supported the ATP staff in development of the focussed
competition and in the evaluation of proposals to both solications.

Technical Objectives:

The broad objective is to improve the capability of U.S. industry by the development of advanced
materials and materials procession methods.  This precompetitive research is directed toward the
resolution of significant technical barriers of to the extent that industrial participants can proceed
to commercialization after completion of the ATP portion of development with reduced risk.

Outcomes:

Projects selected for support address applications such as stationary power generation, solid oxide
fuel cells and earth moving equipment.  Materials under investigation include ceramic coatings,
welded steel and aluminum components.

PROJECT TITLE:  NIST Industry Fellow

PROGRAM TITLE:  Other Projects

Principal investigator(s):

NIST Staff:
Designated Project Leader:  Dapkunas, S. J.
Mailing Address:           NIST
                      Materials (223), A259
                      Gaithersburg, MD  20899
Telephone:                 (301) 975-6119
Fax Number:           (301) 990-8729
E-Mail Address:            dapkunas@micf.nist.gov

Principal Investigator outside NIST:  Yee, Bill G. W.
Mailing Address:                  Pratt & Whitney
                             Materials and Mechanics Engineering
                             West Palm Beach, FL  33410
Telephone:                        (407) 796-6470
Fax Number:                  (407) 796-6477

Technical Description:

S. J. Dapkunas was detailed to the Pratt & Whitney Materials and Mechanics Engineering
Department for a period of six months to develop an understanding of the institutional aspects
of materials development in high technology industry.

Technical Objectives:

The objective of this project was to identify the barriers to transitioning a new material from
laboratory concept to commercial production and to determine the potential role of NIST research
in facilitating that transition.

Outcome:

Specific issues which must be addressed in the development of materials for gas turbine/jet
engine applications were identified.  These include timeliness for engine testing and robust
processing with few steps.  NIST contributions to the transition process consist of the
development of immediately usable products such as Standard Reference Materials, test methods,
data on material systems under development and models specific to material processing methods
used by the engine industry.

Accomplishments:

A report summarizing findings was written and briefings held at NIST to inform staff and
management of these results.  As a consequence of this interaction, projects have been initiated
to:  determine the availability of specific thermodynamic data necessary for the modeling phase
diagrams of superalloy systems; development of an SRM for ppb level measurement of sulfur
in superalloys; and, measurement of thermal conductivity of microlaminate thermal barrier
coatings.

Impact:

Projects of value to the gas turbine industry, which would not otherwise have been initiated, are
underway.

                              RESEARCH STAFF
                                    AND
                            FIELDS OF INTERESTDIVISION OFFICE

Fogarty, Gerard                   Non-linear optical processes
                             Nature, genesis, distribution, and effects of
                              irregularities in monolithic crystals and multilayers
                             High-resolution diffraction imaging

Freiman, Stephen W.          Electronic ceramics
                             Mechanical properties
                             Superconductivity

Steiner, Bruce W.                 High-resolution diffraction imaging
                             Defects in monolithic crystals and multilayers
                             Non-linear optical processes 

POWDER CHARACTERIZATION AND PROCESSING

Cline, James P.                   Standard reference materials
                             High-temperature x-ray diffraction
                             Microstructural effects in x-ray diffraction
                             Rietveld refinement of x-ray diffraction data

Hackley, Vincent A.               Electrokinetic and electroactive measurement
                             Slurry rheology
                             Surface chemistry of powders.

Kelly, James F.                   Quantitative scanning electron microscopy
                             Image analysis
                             Microstructure analysis
                             Powder standards

Lum, Lin-Sien H.                  Powder characterization
                             Instrumental analysis

Malghan, Subhas G.                Powder and dense slurry characterization
                             Colloidal processing and forming
                             Interfacial and surface chemistry of
                              powders
                             Standards development

Minor, Dennis B.                  Analytical scanning electron microscopy of ceramics
                              and particulates
                             Powder test sample preparation
                             Powder characterization

Pei, Patrick T.                   Spectroscopic and thermal characterization
                             Chemical coating
                             Powders characterization

Ritter, Joseph J.                 Chemistry of powders synthesis
                             Specialty powders synthesis
                             Nanomaterials

Wang, Pu Sen                 Solid-state nuclear magnetic resonance
                             Spectroscopic characterization

MECHANICAL PROPERTIES
  
Braun, Linda M.                   Raman stress measurements
                             Ceramic matrix composites
                             Toughening mechanisms

Carter, Craig W.                  Materials thermodynamics
                             Advanced mathematical and computational techniques
                             Computation of materials processes

Chuang, Tze-Jer                   Creep/creep rupture 
                             Fracture mechanics
                             Finite-element modeling
                             Lifetime predictions

Fuller, Edwin, R., Jr.            Influence of microstructure on fracture
                             Toughening mechanisms
                             Microstructural modeling and simulation

Gettings, Robert J.               Mechanical properties
                             Hardness and fracture toughness

Hockey, Bernard J.                Electron microscopy
                             High-temperature creep

Jahanmir, Said               Ceramic machining 
                             Mechanisms of material removal
                             Mechanics of contacts
                             Effects of machining on mechanical properties

Kauffman, Dale A.                 Glass melting

Krause, Ralph F., Jr.             Creep in flexure and tension
                             Fracture mechanics
                             Hot pressing
                             Chemical thermodynamics

Quinn, George D.                  Mechanical property test standards
                             Standard reference materials
                             Creep testing

Roosen, Andrew J.                 Microstructural modeling
                             Computer simulation

Selinger, Robin L.                Microstructural modeling
                             Computer simulation

Smith, Douglas T.                 Surface forces
                             Charge transfer at interfaces
                             Adhesion and friction
                             Colloidal processing

Wallace, Jay S.                   Processing and microstructure
                             Silicon nitride densification
                             Thermal analysis

PHASE EQUILIBRIA

Burton, Benjamin P.               Calculated phase diagrams
                             Dielectric ceramics  

Cook, Lawrence P.                 High-temperature chemistry
                             Phase equilibria

McCormack, Ryan P.           Phase Equilibria Calculations

Vanderah, Terrell A.              Solid-state chemistry
                             Phase equilibria of microwave dielectrics

Wong-Ng, Winnie                   X-ray crystallography and reference patterns
                             Phase equilibria/crystal chemistry of high-Tc
                              superconductors
                             Molecular orbital calculations

ELECTRONIC MATERIALS

Blendell, John E.                 Ceramic processing and clean-room processing
                             Sintering and diffusion controlled processes
                             Processing high-Tc ceramic superconductors
                             Activation chemical analysis

Bonnell, David W.                 Computer automation
                             Molecular-beam mass spectrometry
                             Thermodynamic modeling
                             Laser/plasma sputtering

Chiang, Chwan K.                  Electronic ceramics
                             Thermoelectric power measurements
                             Electrical measurements

Gonzalez, Eduardo                 Ceramic Processing
                             Nano-scale sintering
                             Texture analysis

Hastie, John W.                   High-temperature chemistry
                             Phase equilibria thermochemistry
                             Molecular-beam mass spectrometry
                             Thin-film deposition
                             Vapor deposition process control and modeling

Hill, Michael D.                  Mechanical properties of PZT            
                                  Ceramic processing

Paul, Albert J.                   Laser physics
                             Plasma diagnostics
                             Laser spectroscopy
                             Laser mass spectroscopy
                             Gasdynamic modeling

Piermarini, Gasper J.                  Ceramic processing and high-pressure sintering
                                  Pressure-induced transformation toughening
                                            High-pressure physical properties and structures
                                  High-pressure x-ray diffraction and spectroscopy

Sessoms, Arthur B.                Molecular beam mass spectroscopy
                             Thin film deposition

Schenck, Peter K.                 Emission and laser spectroscopy
                             Thin-film deposition
                             Computer graphics and image analysis
                             Laboratory automation
                             Plasma monitoring and control

Vaudin, Mark D.                   Electron microscopy
                                            Microscopy and diffraction studies of interfaces
                                            Computer modelling of grain-boundary phenomena
                             Dielectric films

White, Grady S.                        Thin films
                                            Nondestructive evaluation
                                            Subcritical crack growth
                             Stress measurements
                             Cyclic fatigue

OPTICAL MATERIALS

Bouldin, Charles E.                X-ray absorption spectroscopy
                              Diffraction anomalous fine structure
                              GeSi heterojunction bipolar transistors

Farabaugh, Edward N.              Chemical vapor deposition of diamond
                             Structure and morphology analysis
                             Scanning electron microscopy

Feldman, Albert                   Chemical vapor deposition of diamond
                             Thermal properties
                             Modelling thermal wave propagation
                             Thin-film optical properties

Kaiser, Debra L.                  Physical properties and structures of high-temperature
                              superconductors
                             Interfaces in high-temperature superconductors
                             Chemical vapor deposition of ferroelectric oxide
                              thin films

Robins, Lawrence H.          Defect identification and distribution
                             Cathodoluminescence imaging and
                              spectroscopy
                             Photoluminescence spectroscopy
                             Raman spectroscopy

Rotter, Lawrence D.               Measurement of electro-optic coefficients
                             Photorefractive effect
                             Optical spectroscopy of thin films

MATERIALS MICROSTRUCTURE CHARACTERIZATION

Allen, Andrew J.                  Small angle x-ray scattering
                             Ceramic microstructure analysis

Black, David R.                Defect microstructure in diamond
                            Polycrystalline diffraction imaging
                            X-ray imaging of photonic materials

Burdette, Harold E.                X-ray optics
                            X-ray diffraction imaging
                            Crystal growth
                            Instrumentation

Fischer, Daniel A.                 X-ray absorption fine structure
                            X-ray scattering
                            Surface science

Long, Gabrielle G.                 Small-angle x-ray and neutron scattering
                            Ceramic microstructure evolution as a
                             function of processing
                            X-ray optics

Spal, Richard D.               X-ray optics
                            Diffraction physics
                            X-ray scattering

Woicik, Joseph C.              UV photoemission
                            X-ray standing waves
                            Surface and interface science

SURFACE PROPERTIES

Gates, Richard S.             Tribo-chemistry
                           Surface chemical properties of ceramics

Hsu, Stephen M.               Ceramic wear mechanisms
                           Engineered ceramic surfaces
                           Lubrication and machining of ceramics

McGuiggan, Patricia M.        Microtribology
                           Surface force measurement

Ives, Lewis K.                Wear of materials
                           Transmission electron microscopy
                           Machining of ceramics

Ruff, Arthur W.               Wear of materials
                           Microstructure effects
                           Mechanical behavior

DATA TECHNOLOGIES

Begley, Edwin F.              Database management methods
                           Engineering database structures
                           Digital video interactive technology

Carpenter, Joseph A., Jr.         Functional ceramics applications
                                      Technical assessments
                                      Industrial liaisons

Cellarosi, Mario              Glass standards

Clevinger, Mary A.                Phase diagrams for ceramists
                                      Computerized data

Dapkunas, Stanley J.          Structural ceramics applications
                           Technical assessments
                           Coatings

Harris, Joyce F.              Data acquisitions
                           Digitization and data entry

Munro, Ronald G.              Materials properties of advanced ceramics
                           Data evaluation and validation
                           Analysis of data relations
                  GUEST SCIENTISTS AND GRADUATE STUDENTS

Armstrong,  Nicholas           University of Technology, Sydney

Bell, Michael I.               Naval Research Laboratory

Belmonte,  Manuel              Autonoma University, Spain

Bernik, Slavko                     University of Ljubljana

Blackburn, Douglas                 Consultant

Brower, Daniel                 Optex Corporation

Bogatin, Oleg                  Institute of Nonmetallic Materials

Cedeno, Christina              American Ceramic Society

Chen, Hailong                  University of Tokyo

Chu, Steven                    State University of New York at Stony Brook

Cordero Cabrera, Mario         Centro National de Metrologia (CENAM)

Dai, Yongshan               Smithsonian Institute

Diao, Jianli                   University of Maryland

Domingues, Louis               Trans-Tech, Inc.

Drews, Andrew R.               Naval Research Laboratory

Fischman, Gary                 FDA

Frederiske, Hans               Consultant

Green, Thomas               American Ceramic Society

Haller, Wolfgang               Abbott Laboratories

Harmer, Martin                 Lehigh University

Hayward, Evans                 American Ceramic Society

Hill, Kimberly                     American Ceramic Society

Hwang, Cheol-Seong             Seoul National University

Ilavsky, Jan                   State University of New York at Stony Brook

Jemian, Peter                  University of Illinois at Urbana/Champaign

Jiang, Feng                    University of Maryland

Job, Lenox                     University of Maryland

Kerch, Helen                   Department of Energy

Kim, Bong-Ho                   Changwan National Laboratory  

Krebs, Lorrie                  Johns Hopkins University

Kruger, Jerome                 Johns Hopkins University

Kubler, Jakob                  Swiss Federal Research Laboratories

Larsen-Basse, Jorn                 National Science Foundation

Lee, Byeong                    Hanyang University 

Levinson, Lionel               General Electric

Liu, Daqing                    Columbia University

Liu, Haiyan                    University of Maryland 

Loezos, John M.                University of Maryland

Maruthamuthu, Pichai           University of Madras, India

Maskara, Alok               University of New Mexico

McMurdie, Howard               Joint Center for Powder                                   
                            Diffraction Studies

Mobley, Morris                 Alfred University

Nagarajan, Mala                University of Maryland

Nagarajan, Venkatta                Indian Institute of Science

Ondik, Helen                   American Ceramic Society

Orlando, Stefano               Instituto Materiali speciali del (CNR)

Paik, Ungyu                    Changwan National Laboratory

Paulik, Steven                     Northwestern University

Perez, Joseph                  Penn State University

Peterson, Marshall                 Wear Sciences

Pothier, Brian                     Army Research Laboratory

Pradip                      Tata Research Development Design Centre

Premachandran, Ramannair Sarasamma Indian Institute of Technology, Madras

Raman, Rajkumar                BDM Federal

Ritchie, Kevin                     University of Maryland

Roberts, Ellis                     Consultant

Roth, Robert                   Viper Group

Russell, Thomas                Naval Surface Warfare Center

Shechtman, Dan                 Johns Hopkins University

Shen, Ming                     University of Illinois

Smith, Wallace                 Office of Naval Research

Swab, Jeffrey                  Army Research Laboratory

Swanson, Nils                  American Ceramic Society

Natarajan, Venkata                 Indian Institute of Science

Wachtman, John                 Consultant

Wang, Jun                   University of Maryland

Wang, Tong                     Jiao Tong University

Wang, Yen                   University of Illinois

Wang, Yinglong                 University of Maryland

Wei, Lanhua                    Wayne State University

Xu, Huakun                     University of Maryland

Yeheskel, Jacob                Nuclear Research Center of the Negev

Ying, Tsi-Neng                 University of Maryland

Zhang, Guangming               University of Maryland

Zhang, Jun                     Lanzhou Institute of Chemical Physics

                         OUTPUTS AND INTERACTIONS
                         CERAMICS DIVISION PATENTS

1995

Process for Multilayer Ceramic Modules (MLC) (D)      M. Cellarosi

A Method of Obtaining High Green Density Ceramics          S. G. Malghan
from Powders (P)                                 R. S. Premachandran

Chemically Assisted Process for the                        J. Wang 
Machining of Ceramics U.S. Patent 
No. 5,447,466, September 5, 1995                           S. M. Hsu

1994

A Process for the Controlled Preparation of a              J. J. Ritter
Composite of Ultra-fine Magnetic Particles
Homogeneously Dispersed in a Dielectric Matrix, 
U. S. Patent No. 5,316,699, May 31, 1994

A Process for the Chemical Preparation of                  J. J. Ritter
Bismuth Telluride and Bismuth Telluride Composite 
Thermoelectric Materials (P)

A Method for Obtaining High Density Green             S. G. Malghan
Ceramics (P)                                                         R. S. Premachandran

Method of Adhering Substrates, U.S. Patent 5,368,942       D. T. Smith
November 29, 1994                                A. Grabbe
                                            R. G. Horn
Methods of Reducing Wear on SiC Ceramic Surfaces      D. E. Deckman
U. S. Patent No. 5,344,577, Sept. 1994                          S. M. Hsu

Ultraviolet Faraday Rotator Glass (D)                           Dexter
                                            Cooper
                                            D. G. Blackburn
                                            D. A. Kauffman
                                            D. C. Cranmer

A Method of Obtaining High Green Density Ceramics          S. G. Malghan
from Powders (P)                                 R. S. Premachandran

1993

Oxygen-Containing Organic Compounds as Boundary       R. S. Gates
Lubricants for Silicon Nitride Ceramics (D)                S. M. Hsu 

Method of Producing a Smooth Plate of Diamond              A. Feldman
U. S. Patent No. 5,221,501, July 25, 1993                  E. N. Farabaugh

Asymmetric Bragg diffraction microscope                    R. Spal
U. S. Patent No. 5,259,013, November 2, 1993

Method for Fabrication of Dense Compacts from              A. Pechenik 
Nanosize Particles Using High pressures and Cryogenic      G. J. Piermarini
Temperatures (P)

Friction and Wear Resistant Coating                        S. M. Hsu
for Titanium and Its Alloys (D)                                 J.-M. Gu

A Cutting Fluid Additive for Machining                     S. Jahanmir
of Ceramics (D)                                  G. Zhang

(D) = INVENTION DISCLOSURE
(P) = PENDING DECISION BY PATENT OFFICE
(A) = INVENTION ALLOWED BY PATENT OFFICE

CONFERENCES AND WORKSHOPS SPONSORED

International Workshop on Instrumented Indentation
Sponsors:  NIST Standard Reference Materials Program (SRMP) and Institute for Mechanics and
Materials (IMM)
Attendance:  96
April 22-23, 1995, San Diego, CA
Organized by:  D.T. Smith, NIST

Workshop in Rational Design and Processing of Advanced Ceramics
Sponsors:  NIST Center for Theoretical and Computational  Materials Science (CTCMS) and
Institute for Mechanic and Materials (IMM)
Attendance:  approximately 70
June 21-23, 1995, La Jolla, CA
Organized by:  Edwin R. Fuller, Jr. NIST, Joanna M. McKittrick, University of California, San 
Diego, and Tze-Jer Chuang, NIST

Objective:  To elucidate the new paradigm of mesoscopic compute simulations in the
microstructural design and processing of advanced ceramic materials and to forge collaborations
between experimental and computational material scientists to develop efficient stratagems for
tailoring and processing advanced materials and components.

Workshop on Large Scale computational Issues in Materials Science
Sponsors:  NIST Center for Theoretical and Computational Materials Science (CTCMS)
Attendance:  approximately 50
August 28-30, 1995, Gaithersburg, MD
Organized by:  W. Craig Carter, NIST and Rob Almgren, University of Chicago

Symposium on Fracture:  Instability Dynamics, Scaling, and Ductile/Brittle Behavior
Symposium Q, 18995 Fall Meeting, Materials Research Society (MRS)
Sponsors:  Materials Research Society and Office of Naval Research (ONR)
Attendance:  approximately 300
November 27 to December 1, 1995, Boston, Massachusetts
Organizers:  Edwin R. Fuller and Robin Selinger, NIST

Objective:  To bring together diverse groups from physics theory, experimental materials science,
and computer simulations to discuss common research in fracture behavior:  dynamical
instabilities in crack propagation; scaling phenomena and fractal geometry in both brittle and
ductile materials; and atomic scale mechanisms/criteria for brittle vs. ductile behavior in bulk
crystalline solids and at interfaces.

Workshop on High Temperature Superconductor Phase Diagrams II
Sponsor:  NIST
Attendance:  approximately 50
October 31 to November 2, 1994, Gaithersburg, MD
Organizers:  Terrell A. Vanderah, NIST

Workshop on Materials and Measurements for Wireless Communications
Sponsor:  NIST
Attendance:  approximately 50
November 7-8, 1995, Gaithersburg, MD
Organizers:  Terrell A. Vanderah, NIST

Applications of Diamond Films and Related Materials:  Third International Conference
Sponsor:  NIST
Attendance:  approximately 200
August 21-24, 1995, Gaithersburg, MD
Organizers:  A. Feldman, NIST

Workshop on Large-Scale Computation and Realistic Microstructure
Sponsor:  NIST
Attendance:  approximately 25
August 28-30, 1995
Organizers:  Craig Carter, NIST

Objective:  To advance the state of the art in techniques for computing realistic microstructures
in solidification problems.

                       STANDARD REFERENCE MATERIALS

The Division provides science, industries, and government a central course of well characterized
materials certified for chemical composition of physical or chemical properties.  These materials
are issued with a certification and are used to calibrate instruments, to evaluate analytical
methods, or to produce scientific data which can be referred to a common base.
   
                                        SRM
   DESCRIPTION                              NUMBER

   Abrasive Wear                            1857
   Alumina Glass Anneal Point                     714
   Alumina Melting Point                          742
   Barium Glass Anneal Point                      713
   Borosilicate Glass Composition                       93A
   Borosilicate Glass Thermal Expansion                731
   Calibrated Glass Beads                        1003B
   Calibrated Glass Beads                        1004A
   Calibrated Glass Spheres                 1017B*
   Catalyst Package for Engine Simulation (IIID)      1817
   Catalyst Package for Engine Simulation (IIID)      1817C
   Catalyst Package for Engine Simulation (IIIE)      8501
   Catalyst Package for Lubricant Oxidation           2567*
   Chlorine in Base Oil                     1818A
   Container Glass Composition                    621
   Container Glass Leaching                  623
   Copper Thermal Expansion                  736L1
   Fused Silica Thermal Expansion                 739L1
   Glass Analytical Standard                     1835
   Glass Dielectric Constant                      774
   Glass Electrical Resistance                    624
   Glass Fluorescence Source                      477
   Glass Liquidus Temperature                     773
   Glass Refractive Index                        1820
   Glass Sand (High Iron)                          81A
   Glass Sand (Low Iron)                          165A
   Glass Stress Optical Coefficient                         709
   High Boron Glass Viscosity                     717
   Intensity XRD Set                         674A
   Lead Barium Glass Composition                    89
   Lead Glass Anneal Point                   712
   Lead-Silica Glass High Temperature Resistivity     1414
   Lead Glass Viscosity                      711
   Line Profile                              660
   Low Boron Glass Composition                     92
   Mica X-Ray Diffraction                    675
   Neutral Glass Anneal Point                     716
   Opal Glass Composition                     91
   Particle Size Distribution Standard                1978
   Refractive Index Glass                        1822
   Respirable Cristobalite                       1879
   Silicon X-Ray Diffraction                      640
   Silicon Nitride Particle Size                       659
   Silicon Nitride Powders for 
     Quantitative Analysis by Powder Diffraction       656*
   Soda Lime Flat Glass Composition                   S620
   Soda Lime Float Composition                   1830
   Soda Lime Float Viscosity                      710A
   Soda Lime Sheet Composition                   1831
   Soda-Lime-Silica Glass                         710A
   Sulfur in Oil                            1819A
   Toluene 5 ML                              211C
   Total Nitrogen in Oils                        1836
   Wear Metals in Oil                       1084A
   Wear Metals in Oil                       1085A
   X-Ray Diffraction Instrument Sensitivity           1976
   X-Ray Diffraction Intensity                    676
   X-Ray Diffraction Intensity Set                     674A

*New in FY-1995            SELECTED TECHNICAL/PROFESSIONAL COMMITTEE LEADERSHIP

Advanced Photon Source
   Steering Committee
          G. Long, Member

Alfred University
   Center for Advanced Ceramics
          S. Freiman, Member of External Advisory Board.

American Association for the Advancement of Science
   Physics Section
          B. Steiner, Representative of the Optical 
          Society of America

American Ceramic Society
   Glass Division
       Committee on Glass Standards Classification and
       Nomenclature
          M. Cellarosi, Chairman
       Editorial Committee
          S. Wiederhorn, Subchairman
   Basic Science Division
          E. Fuller, Vice-Chair
       Editorial Committee
          B. Lawn, Chairman

ASM International
   Energy Division
          S. Dapkunas, Past Chairman, Division Council Member
   Journal of Materials Engineering and Performance
          S. Dapkunas, Editorial Board 
   Journal of Thermal Spray Technology
          S. Dapkunas, Editorial Board
   Washington D.C. Chapter Yearbook Committee
          J. A. Carpenter, Jr., Chairman  

American Society for Engineering Education
   Postdoctoral Review Committee
          A. Feldman, Member

American Society for Testing and Materials
   C14:   Glass and Glass Product
          M. Cellarosi, Chairman
          G. Quinn, Member

American Society for Testing and Materials
   C14.01:  Nomenclature of Glass and Glass Products
          M. Cellarosi, Chairman
   C28.  Advanced Ceramics
          G. D. Quinn, Chairman
   C28.05:  Powder Characterization
          S. Malghan, Working Group Chairman
   D2:  Petroleum Products and Lubricants
          S. M. Hsu, Member
   E29.01:  Advanced Ceramics, Organizational Meeting
          M. Cellarosi
   E42:  Surface Science
          G. G. Long, Member  
   E49:  Computerization of Material and Chemical Property Data
          R. G. Munro, E. F. Begley, Members
   E-08:  Fracture & Fatigue
          G. Quinn, Member
   F-04:  Medical and Surgical Materials and Devices
          G. Quinn, Member
   Fl:02:  Lasers
          A. Feldman, Subcommittee Editor

American Society of Mechanical Engineers
   Research Committee on Tribology
          S. Jahanmir, Member
              S. Hsu, Member
   Subcommittee on Tribology in Manufacturing
          S. Jahanmir, Chairman

Applied Diamond Conference
          A. Feldman, Executive Committee

Ballistic Missile Defense Organization Technology Applications Office (BMDO/TA)
     Materials and Electronics Panel
              J. Carpenter, Member 

Center for Advanced Ceramic Technology, Alfred University
          S. W. Freiman, Member of Oversight Committee

Diamond Films and Technology
   Editorial Advisory Board
          A. Feldman, Member

Dow Chemical Company Synchrotron Radiation Spectroscopy Team
          D. A. Fischer, Member and Outside Advisor

Federation of Materials Societies
          D. L. Kaiser, Trustee

High Temperature Science Journal
          J. W. Hastie, Editorial Board Member

IEEE Lasers and Electrooptics Society
   Washington-Northern Virginia Chapter
          B. Steiner, Treasurer

IGES/PDES Organization
   Materials Committee
          J. Carpenter, Chairman

International Center for Diffraction Data
   High Tech Materials Task Group
          W. Wong-Ng, Chairman
   Ceramic Subcommittee
          W. Wong-Ng, Chairman
   Editorial Board, Powder Diffraction File
          W. Wong-Ng, Consulting

International Conference Series on High Temperature Materials Chemistry
   Organizing Committee
          J. W. Hastie, Member

International Energy Agency
   Subtask 8 International Standards
          S. Malghan, Overall Task Leader on Powder Characterization      
   Subtask 8 Powder Characterization Subgroup
                  S. Malghan, U. S. Task Leader

International Standards Organization (ISO)
   Technical Committee 206 Fine Ceramics
   Working Group 1, Particle Size
          S. Malghan, Member

   Working Group 2, Flexure Strength
          G. Quinn, Chairman
   Working Group 3, Hardness
          G. Quinn, Member

   Technical Committee 184 Industrial Automation Systems and Integration, 
   Subcommittee 4 Industrial Data and Global Manufacturing Programming Languages
   Working Group 3, Project 4 Materials
          J. Carpenter, Jr., Chairman

International Union of Pure and Applied Chemistry Commission II-3
   High Temperature and Solid State Chemistry
          J. W. Hastie, Titular Member

Journal of Non Crystalline Solids
   Editorial Board
          S. Freiman, Member

Journal of Physical Chemical Reference Data
          D. W. Bonnell, Editorial Board Member

Journal of Smart Materials
   Editorial Board
          S. Freiman, Member

Materials Research Society
          G. Long, Council

Minerals and Metallurgical Processing Journal
     Editorial Board 
          S. G. Malghan, Member

National Materials Advisory Board, National Academy of Sciences
   Committee on Superhard Materials
          A. Feldman, Member
   Committee on High Temperature Coatings
          S. J. Dapkunas, Member

National Science Foundation
   Instrumentation Development Advisory Panel
          D. A. Fischer, Member
   Young Investiators' Award Selection Panel
          J. A. Carpenter, Jr., Member

National Synchrotron Light Source
   Housing Committee
          C. E. Bouldin, Member
   User Executive Committee
          Daniel Fischer, Chairman
   EXAFS Special Interest Group
          C. E. Bouldin, Chairman
   Proposal Study Panel on Imaging
          B. Steiner, Member
   Housekeeping Committee
          J. C. Woicik, Member

   Organizing Committee for Annual Users' Meeting
          D. A. Fischer, Member

NIST Cold Neutron Research Facility
          G. G. Long, Program Advisory Committee Member

Powder and Bulk Engineering Journal
          S. Malghan, Member Editorial Advisory Board

Powder X-Ray Diffraction Data
          W. Wong-Ng, Consulting Editor

Research Advisory Committee (RAC)
          G. Long, Chairman

Society of Photooptical Instrumentation Engineers
   Kingslake Award Committee
          B. Steiner, Member

Society of Tribologists and Lubrication Engineers
   Education Committee
          S. Jahanmir, Member
   Fellows Committee
          S. Jahanmir, Member

Stevens Institute of Technology
   Materials Science and Eng. Dept.
          S. Jahanmir, Member of Advisory Board

Superconductor Applications Association
          E. Fuller, Jr., Member of Advisory Board

Tribology International
   Editorial Advisory Board
          S. Jahanmir, Member

Tribology Letters
   Editorial Advisory Board
          S. M. Hsu, Member

University of Delaware
   Dept. of Mechanical Engineering
          S. Jahanmir, Member of Advisory Board

University of Florida Fine Particles Research Center
          S. G. Malghan, Member, Advisory Council

U. S. Department of Energy
   Review Panel for Office of Basic Energy Sciences on "Structural Ceramics and Mechanical
   Behavior of Ceramics:  Emphasis on Mechanical Behavior"
          E. Fuller, Jr., Chairman
   Review Panel for Office of Basic Energy Sciences' Materials Science Program in X-ray
   Absorption Spectroscopy
          D. A. Fischer, Member

U. S. Bureau of Mines Communication Research Center
          S. G. Malghan, Member, Advisory Panel

Versailles Project on Advanced Materials and Standards (VAMAS)
   Technical Working Area on Ceramics 
              G. D. Quinn, U. S. Representative and International              
                      Chairman
   Technical Working Area on Wear Test Methods
          S. Jahanmir, Co-chairman
   Technical Working Area on Materials Databanks
          J. Carpenter, Member
                   INDUSTRIAL AND ACADEMIC INTERACTIONS

INDUSTRIAL

ACTIS, Inc.

   An agreement exists between NIST and ACTIS, Inc. for a joint research and development
activity related to comprehensive computerized tribology databases.  These databases are
evaluated by NIST and marketed by ACTIS, Inc.  Other participants in the program are DOE,
U.S. Army, U.S. Air Force, ASME and STLE.

Advanced Technology Materials

   G. Stauf and P. Van Buskirk of ATM are collaborating with C.-S. Hwang, L. H. Robins, L.
D. Rotter, M. D. Vaudin and D. L. Kaiser in studies of the processing/structure/property
relationships in BaTiO3 thin films deposited by MOCVD.
  
   Specimens of silicon carbide single crystal provided by ATM have been examined for defect
content by cathodoluminescence (L. H. Robins) and x-ray diffraction imaging (D. R. Black).

   Raman spectroscopy was used to characterize the structure of barium titanate thin films grown
by Advanced Technology Materials, EMCORE, and NZAT.  Interactions with these companies
were initiated by D. L. Kaiser and L. D. Rotter in conjunction with their work (see above) on
the MOCVD growth and electro-optic properties of barium titanate films (see above).

Allied Signal Corporation

   S. G. Malghan is conducting collaborative studies with J. Pollinger of Allied Signal Ceramic
Components on the interactions of powder-binder-sintering aid in gelcasting of silicon nitride
powders.  

Aldrich Chemical Company

   J. J. Ritter provided Aldrich with documentation on the use of chemical flow reactors to
generate commercial quantities of YBCO precursor powders.

American Ceramic Society

   P. Schenck is collaborating with the American ceramic Society (ACerS) and the industrial
sponsors of the NIST-ACerS phase diagram optimization program, in the development of a
graphical phase diagram database for ceramic and other inorganic systems.

American Superconductor  

    M. D. Vaudin is involved in a collaboration to investigate by means of x-ray diffraction
techniques the preferred crystallographic orientation of BiSSCO 2223 superconductor in Ag-
swaged wires and tapes.  

   Flux flow in silver-sheathed BiSCCO 2223 wires produced by American Superconductor is
being correlated with microstructure by means of a novel magneto-optical imaging technique used
by M. Turchinskaya and D. L. Kaiser.

   R. D. Spal is studying the effect of mechanical strain on the electrical properties of silver-
sheathed bismuth superconductor (BSCCO-2223) tapes.

   The efforts above are parts of a larger project to investigate correlations between the
mechanical and electrical properties of the BiSSCO wires and tapes the textures induced in them
by fabrication.

American Xtal Technology, Inc.

   Collaboration in the characterization of the crystalline order of gallium arsenide substrates
grown with a greatly increased degree of regularity by a new commercial process, vertical
gradient freeze, is being carried out by B. W. Steiner with M. Young of AXT.

Argonne National Laboratory

   U. Balachandran of ANL collaborates with W. Wong-Ng in the melting characterization of
the high-Tc 2223 phase in the Bi(Pb)-Sr-Ca-Cu-O system.

AT&T Bell Laboratories

   J. C. Woicik collaborates with C. King of Bell Labs on the growth, characterization and the
consequences of strain in SiGe and other group IV semiconductor quantum structures, and with
J. Patel on standing-wave x-ray studies of Pb on Ge.

     G. S. White, L. M. Braun, W. C. Carter, and E. R. Fuller, Jr. are collaborating with Bell Labs
on lifetime predictions for InP in water and in 50% RH.
  
   T. Vanderah collaborates with T. Siegrist of Bell Labs in the structural characterization of
microwave dielectric ceramics.

Battelle Columbus Laboratories

   W. Glaeser at Battelle and A. W. Ruff are involved in a joint activity to prepare a wear atlas
from selected literature and research findings at Battelle Columbus Laboratories, NIST, and the
German Bundesanstalt fur Materialprufung.   

Brookhaven National Laboratory

   B. W. Steiner and G. Fogarty are collaborating on the characterization of crystalline order and
its relation to the magnetic coupling in rubidium calcium trifluoride crystals with J. Hill of
Brookhaven National Laboratory.

Caterpillar Company

   The Surface Properties Group at NIST is working with Caterpillar Company in several areas. 
F. Kelly of Caterpillar is working with S. M. Hsu in the area of advanced lubrication, diesel
particulate reduction and engine simulations.  He is also working with A. W. Ruff to improve
the wear resistance of tractor under-carriage linkage.  S. M. Hsu is also working with K. Bruk,
B. Hockman, and R. Nevinger of Caterpillar on the design of ceramic valve seat inserts.

Ceradyne, Inc.

   J. Mangles of Ceradyne collaborates with S. Jahanmir in the Ceramic Machining Consortium.

Cincinnati Milacron, Inc.

   C. Yoon of Cincinnati Milacron collaborates with S. Jahanmir in the Ceramic machining
Consortium.

Containerless Research, Inc.

   D. Bonnell is collaborating with S. Krishnan of Containerless Research regarding levitation
of liquid metals, pyrometric, emissivity, and laser ellipsometric measurements at high
temperatures, and related studies.

Continuous Electron Beam Accelerator Facility (CEBAF)

   D. Bonnell is collaborating with L. Phillips on development of new technologies for
producing superconducting RF accelerator cavities as part of the goal of a world-wide consortium
of government, academic and industrial groups.  In addition, there is also a joint interest in
possible adoption of NIST-developed PLD deposition techniques as an attractive alternate route
to fabricating niobium alloy-based thin film superconducting RF cavities.
  
Corning, Inc.

   Merle Adler of Corning collaborates with S. Jahanmir in the Ceramic Machining Consortium.

Crystacomm

   Characterization of defects in InP wafers is carried out in a collaboration between G. Antypas
of Crystacomm and D. R. Black.

Crystallume

   L. H. Robins and D. R. Black collaborate with M. A. Plano and others in
cathodoluminescence and x-ray topography characterizations of strain and defect generation in
thick diamond films CVD-grown homoepitaxially on a synthetic diamond substrates.

Cummins Engine Company

   S. M. Hsu is working with J. Wang, M. Naylor, and T. Gallant of Cummins Engine on the
lubrication of new materials, evaluation of chemistries and development of advanced lubrication
concepts for future engines.  New chemistries are being developed and these chemistries are
being evaluated in prototype engines by Cummins.

Deltronic Crystal Industries

   G. Fogarty and B. W. Steiner collaborate in the growth and characterization of crystalline
order of barium titanate and strontium barium niobate with R. Uhrin, M. Garrett, and J. Martin
of Deltronic Crystal Industries.

DOW Chemical Company

   G. Mitchell and B. Dekoven of Dow have begun a research collaboration with D. A. Fischer
to study polymer surfaces and metal-polymer interfaces using ultra soft x-ray absorption
spectroscopy.  The materials studied include poly(acrylic acid), poly(butyl methacrylate),
polystyrene, polycarbonate, poly(ethylene terephthalate), and model acrylic coatings.  

   T. Parsons of Dow collaborates with S. Jahanmir in the Ceramic Machining Consortium.
 
DuPont 

   P. Schenck, J. Hastie, D. Bonnell, and A. Paul are collaborating with D. Kountz, A. Lauder,
and other members of the DuPont Superconductivity Group as part of a CRADA to develop
process control technology for laser and sputter deposition of complex oxide thin films.

   L. P. Cook is collaborating with DuPont in their (partially ATP-supported) research on
problems in processing and characterizing thallium-containing high-Tc superconductors, especially
as related to the phase equilibria of these materials and their interaction with ferroelectrics in
thin-film devices.

Eagle-Picher

   A collaboration has been initiated between Eagle-Picher Research Laboratory (G. Cantwell)
and NIST (L. H. Robins and D. R. Black) to characterize defects and dopant impurities in zinc
selenide single crystals, being developed (in part under an ATP grant) as substrates for blue-green
light-emitting diodes and laser diodes. 

Eaton

   J. Edler of Eaton is collaborating with S. Jahanmir in the Ceramic Machining Consortium.

EG&G Instruments

   B. W. Steiner collaborates in the growth, device processing, and characterization of crystalline
order of mercuric iodide with L. van den Berg of EG&G Instruments.

Eonic, Inc.

   B. French of Eonic collaborates with S. Jahanmir in the Ceramic Machining Consortium.
  
Exxon Research and Engineering

   G. Meitzner and J. Sinfelt of Exxon are collaborating with D. A. Fischer to study the
electronic structure of adsorbed carbon monoxide and hydrocarbons on platinum-supported
catalysts using near-edge spectroscopy above the carbon K-edge.

Eastman Kodak Company

       D. T. Smith has been collaborating informally with R. Sharma of Kodak's Polymer
Research Laboratory to study the surface charging properties of thin insulating films of potential
industrial interest to Kodak.

Edge Technology Inc.

   Artificial diamonds to be used as machine tools were supplied to D. R. Black, who correlated
(for purposes of quality control) topographic examination of the crystals to optically observed
defects.

Ford Motor Company

   K. Carduner and M. Rokosz of Ford Motor Company have been active with P. S. Wang in
the application of NMR spectroscopy and imaging to characterization of ceramic materials. 
Efforts so far have involved data exchange of Si-29 CP/MAS NMR for phase composition
determination of silicon nitride and carbide powders; in the future, we plan to exchange imaging
capabilities. 

   R. Allor of the Ford Scientific Research Lab is collaborating with S. Jahanmir in the Ceramic
Machining Consortium.
  
Gas Research Institute

   R. G. Munro continued interactions with the Gas Research Institute to provide evaluated data
fo the use of advanced ceramics in heat exchangers and gas-fueled engines.

General Electric

   W. Banholzer of GE has been collaborating to evaluate a single-crystal diamond wafer by
spatially resolved cathodoluminescence spectroscopy (L. H. Robins) and by x-ray diffraction
imaging (D. R. Black).

   K. Kumar of GE Superabrasives is collaborating with S. Jahanmir in the Ceramic Machining
Consortium.  

   D. Hurley of the GE Corporate Research Center and D. R. Black are performing defect
characterization on isotopically-controlled man-made diamond crystals.  This is part of a larger
study of the relationship of defects to ultrasonic measurements on these materials.
   
   V. Krishnamurthy of the GE Corporate Research Center and J. J. Ritter explored the potential
of the Cyclic Dip and Fire process as a low-cost approach to apply ferrite films for use in
integrated microwave circulator devices.

General Motors Corporation

     R. Fouts of GM's AC Delco Systems collaborates with S. Jahanmir in the Ceramic
Machining Consortium.

Hauptman-Woodward Medical Research Institute, Inc.

   George DeTitta is the co-investigator with W. Wong-Ng for the development of a standard
reference material for the alignment of single crystal x-ray diffractometers.

IBM, Almaden Research Laboratory
 
   W. Wong-Ng interacts with T.C. Huang of IBM on investigations of the x-ray property of
PZT and BaTiO3 thin films prepared at NIST using the laser deposition technique. 

International Centre for Diffraction Data

   W. Wong-Ng is Chairperson of the Ceramics Subcommittee and the High-Tech Materials
Task Group of the ICCD.  Efforts have been initiated to organize the inorganic materials of the 
X-ray Powder Diffraction File (PDF) into minifiles according to their functions, properties or
structure.  W. Wong-Ng also serves as a consulting editor for the PDF.

Johns Hopkins University Applied Physics Laboratory

   D. Wickenden of the JHUAPL is collaborating with L. H. Robins in a project for
characterizing defects and dopant impurities in thin films of gallium nitride and AlxGa1-xN by
spatially resolved CL.  These materials are being developed for short-wavelength laser and LED
devices.  The specimens, grown via MOCVD at JHUAPL, are being characterized at NIST.

   D.T. Smith is collaborating with R. Cammarata on mechanical properties measurements (using
nanoindentation) of nanoscale iron films.

Kennemetal Inc.

   S. M. Hsu is cooperating with the machining group at Kennemetal (R. F. Upholster) on
jointly developing chemically assisted technology of ceramics.  Samples were exchanged and
many discussions were held.  Some of the more promising chemistries may be tested at their
facility.
  
   G. D. Quinn, L. K. Ives, R. Gettings and A. W. Ruff have collaborated with Kennemetal in
modeling tungsten carbide disks which will be used as Vickers hardness standard reference
materials.

Kobe Steel Electronic Research Center

   Characterization of defects in natural diamond substrates and in doped homoepitaxial diamond
films is currently the subject of a collaboration between D. R. Black and B. Fox of Kobe Steel.

Lawrence Livermore Laboratories 

   As part of a study with P. Johnson of Lawrence Livermore Laboratories (LLL) of the
cohesive strength of grain boundaries in Ni3Al as a function of grain boundary misorientation and
symmetry, alloy stoichiometry and boron concentration, grain orientations in test bars have been
measured by M. D. Vaudin) prior to mechanical testing.

   Collaboration on the crystal growth of potassium dihydrogen phosphate for high power lasers
is being carried out by B. W. Steiner with J. DeYoreo and C. Ebbers of LLL.

Marlow Industries

   J. J. Ritter has held discussions with Marlow, a major U.S. supplier of thermoelectric
elements, to disclose chemical methods used to synthesize and modify bismuth telluride-based
thermoelectric materials.

Matec Applied Sciences

   This cooperative research is related to the development of electrokinetic sonic amplitude
measurement for dispersion of powders in dense slurries.  Research at NIST under the direction
of S. G. Malghan will be utilizing hardware and software developed by Matec Applied Sciences
for on-line measurement of dispersion.

Morgan-Matroc

   In collaboration with Morgan-Matroc, damage in PZT-8 due to cyclic loading has been
investigated.  Morgan-Matroc supplied the specimens and information regarding their
piezoelectric properties and G. S. White, M. D. Hill, C.-S. Hwang provided information on the
mechanical response to loading. 

Nanophase Technology Inc.

   J. Parker of Nanophase Technology is collaborating with G. G. Long and S. Krueger (Reactor
Radiation Division) in the investigation of microstructure evolution during densification of
nanophase ceramics.

NASA Consortium for Commercial Development

   Cooperative research is aimed at understanding fundamentals of zeolite nucleation, growth
of CdTe single crystals and strain development during growth of GaAs.  G. G. Long, D. R.
Black, H. E. Burdette, and S. Krueger (Reactor Radiation Division) are working with E. Coker,
H. Wiedemeier and D. Larson of the consortium on this research.

National Institute of Statistical Sciences (NISS)

   A collaboration between NISS, the Ceramics Division, and the (NIST) Statistical Engineering
Division has explored cross-disciplinary applications of statistics and statistical concepts to
materials science and the formulation of a research agenda leading to high-impact advances.  An
outgrowth of this collaboration was a workshop, Statistics and Materials Science:  Microstructure
- Property - Performance Relations, which was held at NIST on July 26-28, 1993.
  
National Renewable Energy Laboratory

   Carbon films deposited by R. Pitts via solar methods at the National Renewable Energy
Laboratory were examined by L. H. Robins for diamond content by Raman spectroscopy.

National Research Institute for Metals (Japan)

   R. G. Munro and J. R. Rumble, Jr (NIST Office of Standard reference Data) are collaborating
with S. Nishijima, Y. Asada and K. Hoshimoto of NRIM on development of a comprehensive
materials property data base for high-Tc superconductors.

   J. A. Carpenter, Jr. participates with Y. Monma of NRIM and G. Dean of the National
Physical Laboratory (United Kingdom) in the  VAMAS Inventory of Data Reduction Models
Project. 

Naval Research Laboratory

   S. Lawrence and B. Bender of NRL are collaborating with J. S.  Wallace on the
thermochemical treatment of polymer-derived SiC fibers and the degradation mechanisms of these
fibers during high temperature heat treatments.
  
   M. D. Hill and G. S. White are is collaborating with Dr. Sadananda at NRL investigating
cyclic fatigue of piezoelectric material.  Mechanical properties are investigated at NIST and TEM
is done at NRL.  

   B. W. Steiner collaborates with M. Bell and R. Whitlock of NRL in a study of the role of
crystalline irregularities on the performance on quartz-crystal resonators.

   T. A. Vanderah collaborates with M. Osofsky and other physicists in the Materials Science
and Technology Division of NRL in the crystal growth and characterization of high-temperature
superconductors and microwave dielectric ceramics.

   D. L. Kaiser and T. A. Vanderah are collaborating with E. F. Skelton and S. B. Qadri of NRL
to study structural inhomogeneities in superconducting YBa2Cu3O7-x single crystals by means of
high spatial resolution x-ray diffraction.

Naval Surface Warfare Center

   Tom Russell of NSWC has been working with G. J. Piermarini on the study of energetic
materials and Buckminsterfullerenes at high pressure. 

   A joint research project with D. R. Black has been developed to supply and characterize
copper single crystal substrates for use as substrates for heteroepitaxial growth of diamond films. 
Northrop Grumman

   D. R. Black, H. E. Burdette and G. G. Long are collaborating with D. Larson of Northrop
Grumman on the characterization of earth-grown and space-grown CdZnTe crystals.

NZ Applied Technologies Corporation

   G. Fogarty and B. W. Steiner collaborate with J. Zhao of NZ and M. Cronin-Golomb of Tufts
University in the characterization of crystalline order of SBN layers grown on magnesium oxide.

   L. D. Rotter has performed electro-optic, poling and second harmonic generation studies on
BaTiO3 and SrxBa1-xNbO6 (SBN61) thin films grown by J. Zhao of NZ.

Oak Ridge National Laboratory

   A Collaborative Access Team (CAT) agreement has been established between MSEL (G. G.
Long), the University of Illinois at Urbana-Champaign (H. Chen) and the UOP Research
Corporation on the design and construction of a beamline at the Advanced Photon Source (APS)
at Argonne National Laboratory.

OPTEX Inc

   W. Wong-Ng collaborated with ATP-funded company OPTEX of Rockville, Maryland, on
x-ray diffraction studies of undoped and doped optical SrS thin films for optical data storage, to
characterize these films for correlations with processing parameters. 

   L. H. Robins uses CL spectroscopy to detect rare-earth ions in rare-earth doped SrS:(Eu,Sm)
thin films prepared by OPTEX.  The goal of this project is to better understand how the rare-
earth ions, as well as other impurities and defects, determine the optical emission properties of
the films, and to correlate the optical emission properties with film preparation conditions.

Polaroid Corporation

   P. K. Schenck is collaborating with K. S. Kim of Polaroid to study the mechanism of laser
ablation transfer being utilized in a state-of-the-art printer.

Research Triangle Institute

   A joint research project was developed with D. R. Black to study the microstructure of
diamond substrates to be used for homoepitaxial growth of diamond films by chemical vapor
deposition.

Rockwell International

   A. Feldman collaborated with S. Holly of Rockwell International to organize the Diamond
Optics IV conference sponsored by the Society of Photo-Optical Instrumentation Engineers
(SPIE).

   W. C. Carter assisted in development of computational models for woven composite behavior.

Russian Academy of Sciences Institute of Solid State Physics

   A collaborative program to elucidate the nature of disorder in oxide crystals has been initiated
by B. W. Steiner with V. Shekhtman of the Institute of Solid State Physics.

Russian Research Center for Standardization, Information and Certification of Materials

   R. G. Munro and J. R. Rumble, Jr. (NIST Office of Standard Reference Data) are
collaborating with A. D. Koslov to establish evaluated property data for selected oxide and
carbide structural ceramics worldwide.

Russian Academy of Science

   Cooperative activities under the NIST-Russian Academy of Science Agreement have
continued in the areas of tribology and materials science.  Current emphasis is on a joint US-
USSR book on tribology (A. W. Ruff and S. Jahanmir).  Future benefits to NIST and the
Division include exchange of tribology data, exchange of computer software for surface analysis,
and future exchange of technical staff.

   A collaborative program between the Russian Academy of Sciences and the NIST Ceramics
(D. L. Kaiser) and Metallurgy Divisions is underway to map flux distributions in high-
temperature superconductors by a magneto-optical technique.

SAC International Ceramics, Ltd.

   A. Solomah is collaborating with S. Jahanmir in the Ceramic Machining Consortium.  

Sanders Corporation

   B. W. Steiner and G. Fogarty collaborate on the crystal growth of barium titanate single
crystals with M. Cronin-Golomb of Tufts University and T. Pollack of Sanders.

Sandia National Laboratory

   A cooperative program has been established between Mark Smith at SNL and P. Pei, G. Long
and D. Smith of NIST to evaluate processing effects on the structure and properties of thermal
spraydepostied coatings.

Schmidt Instruments

   A collaborative research project was initiated with D. R. Black to grow heteroepitaxial
diamond films and characterize their crystal perfection.

Southwest Research Institute

   R. Page of SRI is collaborating with S. Kruger (Reactor Radiation Division) and G. G. Long
on the microstructure evolution of alumina during densification.

St. Gobain Norton

   V. Pujari of St. Gobain Norton and S. G. Malghan are studying the characteristics of agitation
milled silicon nitride powders in aqueous environment.  St. Gobain Norton has provided silicon
nitride powder samples for NIST to compare the performance of agitation ball milling to large-
scale processing by conventional methods. 

   V. Pujari is also cooperating with S. M. Hsu on the effects of machining on tensile strength
of silicon nitrides.  Tensile bars were received from St. Gobain Norton, subjected to chemically
assisted machining, and then tested for strength.

   K. Grey of St. Gobain Norton is learning to use the NIST (A. Feldman and H.P.R.
Frederikse) photothermal radiometry facility for the purpose of setting up such a facility at St.
Gobain Norton for thermal conductivity measurements on diamond films.  We plan to collaborate
in the analysis of the data generated at St. Gobain Norton.

   S. M. Hsu is working with B. McEntire of St. Gobain Norton to jointly evaluate ceramic
materials for valve seat insert application.  The program is a joint program with the Gas Research
Institute (GRI), Caterpillar, and Southwest Research Institute (SWRI) in which a full-scale engine
test is being conducted at SWRI to evaluate different materials for the valve seat inserts in a gas-
fueled Caterpillar 3500 series engine.

   The Cerbec Division of St. Gobain Norton has furnished silicon nitride bearing balls which
will be used by G. D. Quinn, R. Gettings, A. W. Ruff and L. K. Ives to make Knoop hardness
standard reference materials.

   S. Subramanian of the World Grinding Technology Center of St. Gobain Norton collaborates
with S. Jahanmir in the Ceramic Machining Consortium.

Smithsonian Institute

   W. Wong-Ng in collaboration with Y.S. Dai of the Smithsonian Institute has studied the twin
structure of Ba-Ti-Zn-(F,O) as well as the characterization of Na-doped Ba2YCu3O6+x
superconductors.

Tata Research Design and Development Center

   Under a Indo-US program, a collaborative project is in progress to study Al2O3-ZrO2
suspensions and their evaluation.

Torrington Company

   S. Redder of Torrington is collaborating with S. Jahanmir in the Ceramic Machining
Consortium.

Tower Oil and Technology Company

     E. Nachtman of Tower Oil collaborated with S. Jahanmir in the Ceramic Machining
Consortium.

Trans-Tech, Inc.

   T. A. Vanderah, R. S. Roth of the Viper group, and T. Negas of Trans-Tech, Inc. collaborate
on microwave dielectric materials processing, phase equilibria and crystal structure data for these
materials.  Measurement of electrical properties is a joint effort between NIST and Trans-Tech.

   J. J. Ritter collaborating with Trans-Tech under a CRADA to develop a simple, effective
process for making a variety of ferrite films.

U.O.P. Research Corporation

   A Collaborative Access Team (CAT) agreement has been established between MSEL (G. G.
Long), the University of Illinois at Urbana-Champaign (H. Chen) and the U.O.P. Research
Corporation on the design and construction of a beamline at the Advanced Photon Source (APS)
at Argonne National Laboratory.

U. S. Air Force

   J. J. Ritter provided B. Poindexter, a dentist at Bolling Air Force Base, information on the
efficacy of ceramic coatings for potable water condenser surfaces.

U. S. Army Research Laboratory

   G. D. Quinn is working closely with ARL in the preparation of a standard practice for the
characterization of fracture origin in ceramics.

U.S. Bureau of Mines at Albany

   The goal of this collaboration between N. Gokcen of the U.S. BoM and W. Wong-Ng is to
investigate the effect of high oxygen pressure on the structural and superconducting properties
of the superconductors, Ba2RCu3O6+x  (R=neodymium and yttrium), and of (Ca,Sr)CuO2 .  

W. R. Grace & Company

     J. Chakraverty of the Diamonite Plant collaborates with S. Jahanmir on the Ceramic
Machining Consortium.

West Advanced Ceramics, Inc.

     R. West collaborates with S. Jahanmir in the Ceramic Machining Consortium.

Xsirius, Inc.

   Collaboration in the characterization of sapphire substrates for high temperature
superconducting devices is ongoing between B. W. Steiner, U. Laor of the Nuclear Research
Center of the Negev (Israel), and W. Graham, President of Xsirius.

ACADEMIA

Alabama A&M University

   B. W. Steiner collaborates with R. Lal and A. Batra of Alabama A&M on the growth in
space and on the ground of triglycine sulfate crystals.  

Auburn University

   A. Feldman collaborated with Y. Tzeng of Auburn to organize the First International
Conference on the Applications of Diamond Films and Related Materials, ADC'91.

Boston University

   L. H. Robins has collaborated with J. Lin of Boston University to examine by
cathodoluminescence spectroscopy the defect content of thin boron-doped diamond films grown
by the electron cyclotron resonance microwave plasma assisted CVD method.  

Cleveland State University

   S. Duffy of Cleveland State is collaborating with T.-J. Chuang in the area of continuum
damage mechanics on continuous fiber reinforced ceramic composites for high-temperature
applications.

Columbia University 
   
   P. Somasundaran of Columbia has been collaborating with S. G. Malghan on a research
project to study basic parameters affecting the preparation of dense suspensions of silicon nitride
powder containing sintering aids.

Dartmouth College

   Real-time imaging of dislocation motion in pure and doped ice is currently underway between
D. R. Black and F. Liu of Dartmouth.

East China University of Chemical Technology 

   This is a joint effort to use finite-element techniques to analyze creep behavior of ceramic
c-rings at elevated temperatures.  D. Wu and Z.-D. Wang of ECUCT are developing the finite-
element model for C-rings and a computational algorithm for creep and T.-J. Chuang is providing
a theoretical framework and experimental data to support the program.

Free University of Brussels

   J. Hastie and D. Bonnell are collaborating with J. Drowart of Brussels on a survey of
ionization cross section usage in high-temperature mass spectrometry.

Florida State University

   A collaborative study between J. Schwartz of Florida State and D. L. Kaiser and F. W. Gayle
(Metallurgy Division) is underway to correlate microstructure with microscopic flux flow during
magnetization of Bi2Sr2CaCu2O8+x superconducting tapes by means of a magneto-optical imaging
technique.

Georgia Institute of Technology

   S. Danyluk of the School of Mechanical Engineering of Georgia Tech collaborates with S.
Jahanmir in the Ceramic Machining Consortium.
 
Harvard University

   G. Golovchenko of Harvard and J. C. Woicik are collaborating on standing-wave x ray and
scanning tunneling microscopy studies of Bi on Si(111).

Howard University
 
   G. Walrafen of the Chemistry Department of Howard University and G. J. Piermarini
continue a long-standing collaboration on study of materials at high pressures.  They are currently
studying liquid state of H2O in the superpressed state at elevated temperatures and pressures.

Indian Institute of Technology, Kanpur, India

   P. Ghosh of IIT-Kanpur and J. Hastie are collaborating on a study of ion-molecule reactions
in RF plasmas.

Indira Gandhi Institute (IGI) Kalpakkam, India

   A collaborative activity is underway between Dr. Mathews of IGI and J. Hastie for the mass
spectrometric investigation of materials at very high temperatures generated by laser heating.

Iowa State University
   
   Characterization of defects in icosahedral AlPdMn is being performed by D. R. Black and
A. Goldman and S. Kycia of Iowa State.

Johns Hopkins University

   J. Kruger and L. Krebs of JHU are collaborating with G. G. Long and C. Majkrazak (Reactor
Radiation Division) on in-situ polarized neutron reflectometry studies of the nature and structure
of passive films.

   D. Shechtman of JHU is collaborating with A. Feldman and E. Farabaugh in the high-
resolution TEM analysis of CVD diamond nucleation and growth.

Massachusetts Institute of Technology

   R. Hallock and W. Rhine of MIT interacted with W. Wong-Ng to characterize the BaTiO3
precursor material, BaTi(O)(C2O4)25H2O, by an x-ray diffraction method. 

National Tsing Hua University  

   S. Lee and J.-L. Chu Tsing Hua are collaborating with T.-J. Chuang on creep life prediction.

North Dakota State University

   G. J. McCarthy of the North Dakota State University is collaborating with W. Wong-Ng in
the preparation of standard reference for high-Tc superconductor and related materials.

Northwestern University

   S. M. Hsu is collaborating with M. Fine of Northwestern on optimization of ceramic wear
resistance by introducing compressive stress into the surface and interfaces.

   K. T. Faber and several of her students at Northwestern are collaborating with E. R. Fuller,
Jr. on a research project focused on the understanding and control of materials which undergo
process-zone phenomena around propagating cracks.  

   D.L. Johnson of Northwestern is collaborating with G. G. Long and A. Allen of the
University of Maryland on microwave-assisted reaction-bonded silicon nitride.

Pennsylvania State University

   S. M. Hsu is collaborating with Profs. Duda, Klaus, Philips, and Christen on a variety of
projects.  Duda and Klaus are working on lubrication, development of lubricants for alternative
fuels and ceramic lubrication.  Philips is working on synthesis of nano-sized particles of ceramic
materials using a microwave assisted plasma reactor.  Christen is working on computer simulation
of grain growth.

   S. G. Malghan and P. S. Wang are collaborating with R. German of PSU in their consortium
on powder injection molding.

   M. D. Hill is interacting with E. Cross of PSU in investigations of PZT.  NIST is providing
information on mechanical testing of PZT and is reviewing training on machining electrical
measurements.

   R. G. Munro (NIST) and J. Hellmann (PSU) are continuing their extended collaboration on
the indentification of important high-temperature ceramic materials and properties issues that may
be addressed in the development of the NIST Structural Ceramics Database.

Purdue University

   D. L. Kaiser is collaborating with M. McElfresh of Purdue University to study magnetization
and current transport in superconducting Yba2Cu3O7-x single crystals.

Rensselaer Polytechnic Institute
 
   Collaboration on the diffraction imaging of semiconducting multilayers in order to determine
the genesis and influence of disorder on photonic device performance is being carried out by B.
W. Steiner and H. Wiedemeier and K. Rajan of RPI.
Rice University

   D. Bonnell is collaborating with the High Temperature Group in the Chemistry Department
of Rice on levitation and thermophysical properties of liquid metals.
   
Rutgers University 
   
   S. C. Danforth of Rutgers has provided S. G. Malghan with nano-sized Si3N4 powder for
processing at NIST using cryogenic compaction.

   S. M. Hsu is collaborating with Profs. Niesz and Wachtman on microstructural design for
wear resistance on silicon nitrides.  Variation of grain size, shape and interface strength are being
examined.  The materials processed are evaluated both at NIST and at Rutgers.

   H. Han and G. Skandan of Rutgers are collaborating with G. G. Long and S. Krueger
(Radiation Reactor Division), and A. Allen of the University of Maryland in the study of
nanophase powders and processing.

Seoul National University

   J. E. Blendell is collaborating with D.-Y. Kim of Seoul National University on the wetting
of grain boundaries in Al2O3.

Stanford University

   W. Spicer of Stanford is collaborating with J. C. Woicik in the use of x-ray standing-wave
studies, surface-EXAFS, and ultraviolet photoemission of metal/semiconductor interfaces and
semiconductor surfaces.

State University of New York/Stony Brook

   Collaborative researh on the relationship of processing to microstructure of plasma sprayed
coatings has been under way between J. Ilavsky of SUNY and G. Long of NIST.

Stevens Institute of Technology

   T. Fischer of the Materials Science and Engineering Department is collaborating with S.
Jahanmir in the Ceramic Machining Consortium.

Texas A&M University

   J. Mayer of the Mechanical Engineering Department is collaborating with S. Jahanmir in the
Ceramic Machining Consortium. 
Tufts University

   B. W. Steiner and G. Fogarty collaborate with M. Cronin-Golomb of Tufts on the observation
of optical mixing and related optical phenomena in non-linear optical crystals.  Other
collaborators include R. Uhrin, M. Garrett, and J. Martin of Deltronic Crystal Industries and J.
Zhao of NZ Applied technologies.

University of California at Berkeley 

   A. M. Glaeser of UC Berkeley is collaborating with T.-J. Chuang on microdesign of
interfacial defects for creep crack growth experiments.

University of California at Santa Barbara 

   Joint experiments between J. N. Israelachvili and P. McGuiggan of UC Santa Barbara and
D. T. Smith) are being conducted to investigate frictional properties of silica surfaces under dry
conditions and with a variety of thin (< 10 nm) intervening liquid films.

University of Dayton Research Institute 

   Using UDRI's x-ray photoelectron spectrometer (XPS) and Auger electron spectrometer
(AES), T. Wittberg of UDRI is conducting studies on surface structures and reactivities with P.
S. Wang.   
 
University of Grenoble

   B. P. Burton has been working with A. Pasturel of the  University of Grenoble on first-
principles phase diagram calculations of BCC-based ordering in Ni-Al-Ti and Fe-Be alloys.

University of Illinois

   M. McNallan of UI is collaborating with S. M. Hsu on wear mechanisms of ceramic materials
and the definition of surface quality in terms of strength as a result of machining damage.

   A Collaborative Access Team (CAT) agreement has been established between MSEL (G.
Long), the University of Illinois at Urbana-Champaign (H. Chen) and U.O.P. Research
Corporation on the design and construction of a beamline at the Advanced Photon Source (APS)
at Argonne National Laboratory.

University of Maryland

   A collaborative study between A. Roytburd of the University of Maryland (UMD) and D. L.
Kaiser and F. W. Gayle (Metallurgy Division) involves theoretical aspects of the effect of twin
boundary and grain-boundary defects on flux flow during magnetization of high temperature
superconductors.

   L. Chang of UMd is collaborating with E. F. Begley and C. G. Lindsay on appropriate
instructional techniques for a computer-based tutorial in phase diagram interpretation.  UMd will
also provide a testbed of students for evaluation of the tutorial.

   B.-H. Chen and B. Eichgorn of UMd are collaborators with W. Wong-Ng in the structural
investigation of possible new superconductor related single-crystal materials.

   M. D. Hill, G. S. White, and S. W. Freiman are collaborating with I. Lloyd of UMd
investigating mechanical and electrical effects of cyclic loading of PZT.  Hill is using the
research as partial fulfillment of requirements for a PhD in materials science. 

   R. K. Khanna is collaborating with S. G. Malghan on spectroscopy of powders.

   S. Jahanmir, as Adjunct Professor in the Department of Mechanical Engineering at UMd, is
presently supervising three students (L. Job, K. Ritchie, and M. Nagarajan) who are working
toward their M.S. degrees.  These students work at NIST on ceramic machining as Guest
Researchers.

   G. Zhang of the Mechanical Engineering and the Systems Research Institute of UMd
collaborates with S. Jahanmir in the Ceramic Machining Consortium.
 
University of Michigan

   J. Gland of Michigan and D. A. Fischer are collaborating on the study of hydrogenolysis of
aniline on the Pt(111) surface.

   J. Schwank of Michigan is carrying out specialized characterization of conductive ceramic
powders by ESCA and Auger spectroscopy in collaboration with J. J. Ritter.  These powders are
synthesized at NIST for NASA.

University of Pennsylvania

   P. Davies of the University of Pennsylvania has been working with T. A. Vanderah and R.
S. Roth of the Viper Group on high-resolution transmission electron microscopic images of
microwave dielectric materials.

University of Rochester

   J. Chakraverty of the Diamonite Plant collaborates with S. Jahanmir in the Ceramic
Machining Consortium.

University of South Carolina

   R. G. Munro (NIST) and T. Datta (U. So. Car.) are collaborating on the evaluation of
materials properties for high-temperature superconductors.

University of Southampton

   D. Bonnell and J. Hastie have been working with I. R. Beattie of the University of
Southampton to adapt transpiration mass spectrometry to the quantitative determination of
volatiles from spent reactor fuel pins.  This association has developed into a detailed interaction
to refine details of system design and instrument selection for Project Osprey.

University of Toronto

   S. Jahanmir is collaborating with T. Coyl of the University of Toronto in machining of
ceramic composites.  C. Ryan, a graduate student from the Materials Science and Engineering
Department, is working on his thesis on machining at NIST with S. Jahanmir.

University of Virginia 

   D.T. Smith is collaborating with H.N.G. Wadley of UVa on nanoindentation studies of
Al/Al2O3 and Al/Cu nanoscale multilayer systems. 

University of Washington

   L. Sorenson of UW and J. C. Woicik are using diffraction anomalous fine structure
measurements to study strained semiconductor layers and 123 semiconductors.

   B. W. Steiner, J. C. Woicik, and J. G. Pellegrino (Thermophysics Division) also collaborate
with Professor Sorenson 
on strain relaxation in III-V photonic crystals.

   D. Castner and B. Ratner of the University of Washington and D. A. Fischer have used the
polarization dependence of carbon and fluorine NEXAFS to understand the orientation of
fluorocarbon groups and proteins on polymeric biomaterials used in medical implants.  

   G. D. Quinn is collaborating with M. Jenkins in the creation of a fracture toughness standard
test method for ceramics for ASTM Committee C28.

University of Western Ontario

   A collaboration was initiated this year between H. H. Schloessin and R. A. Secco of the
Geophysics Department of Western Ontario with R. D. Spal.  This work involves study of
geological samples by means of x-ray diffraction topography and the asymmetric Bragg
diffraction microscope.

University of Wisconsin

   A joint activity is underway between S. Babcock, X. Cai, and D. Larbalestier of the
University of Wisconsin and D. L. Kaiser to characterize the microstructural, magnetic and
electrical transport properties of single crystals and bicrystals of superconducting YBa2Cu3O6+x.

   M. D. Vaudin is collaborating with J.-L. Wang and S. Babcock of Wisconsin in the
determination of misorientations across twist bicrystals of ceramic superconductors.

Worcester Polytechnic Institute

   I. Bar-On of Worcester Poly is conducting a joint ASTM Committee C28-E08 project to write
a fracture toughness standard.

                                FACILITIES                                FACILITIES
 

POWDER CHARACTERIZATION AND PROCESSING

High Temperature X-ray Diffraction - J. P. Cline

The x-ray diffraction facility at NIST consists of a high-temperature machine of theta-two theta
geometry equipped with an incident beam monochrometer and a position sensitive proportional
counter.  The incident beam monochrometer removes the K2 radiation and results in diffraction
profiles that are more sensitive to effects of sample character.  The position sensitive detector
allows for data collection at a rate two orders of magnitude faster than conventional detectors. 
The furnace is an enclosed high vacuum chamber capable of reaching 3000 K, and is equipped
with a mass flow controller for atmospheric control.  This equipment is used for the study of
high-temperature phase equilibria, high-temperature reaction kinetics, sintering of monolithic
ceramics, and strain development during sintering of ceramic composites.  Additional equipment
consists of four automated and updated Philips diffractometers which are used for certification
of standard reference materials (SRMs), studies on the effects of microabsorption and extinction,
and the development of the Rietveld method for a conventional, sealed tube, x-ray diffraction
equipment.

Electrokinetic Measurements - V. A. Hackley and S. G. Malghan

The Matec ESA-8000 system has the unique capability for measuring colloidal properties in
dense slurries.  The analytical capabilities of the ESA system include performance in the
following modes: potentiometric titration, conductometric titration, time-series titration, and
concentration series titration.  In the selected mode, the equipment can monitor: electrokinetic
sonic amplitude, zeta-potential, electrophoretic mobility, electrical conductivity, isoelectric point,
surface charge density, and phase angle of the material with the specified experimental
conditions.  The latest addition to this laboratory is a Acousto-Sizer by Matec Applied Sciences.

Slurry Rheology - S. G. Malghan and V. A. Hackley

The RTI rheometer allows for viscosity as well as rheology characterization of ceramic slurries. 
Rheological measurements are more informative and flexible with respect to the various slurry
properties: Newtonian, pseudoplastic, plastic, dilatant, and thixotropic.  The modeling of these
rheological properties as a function of sample treatment and surface chemical properties is
paramount in developing and improving the slurry processing technology.

Physical Properties Characterization Laboratory - L. Lum, D. B. Minor, P. T. Pei and S. G.
Malghan

The physical properties characterization laboratory is equipped with state-of-the-art techniques
for the measurement of particle size distribution, specific surface area, specific gravity, tap
density, and porosity.  The particle size distribution is measured by three techniques -- gravity
sedimentation by Sedigraph, centrifugal sedimentation by Joyce-Loeble, and laser diffraction by
Horiba LA-900.  The range of particle size distribution covered by these techniques is (0.01 to
200) m.  The specific surface area determination is carried out by nitrogen adsorption and the
BET method.  The porosity of powders and ceramics is measured by mercury intrusion.

Colloidal Processing of Powders - S. G. Malghan, D. B. Minor and P. T. Pei

The focus of this laboratory is to develop data and understanding of non-oxide powders
processing in aqueous environment.  The laboratory is equipped with instruments and equipment
for studying deagglomeration, dispersion, suspension stability, slurry casting, and green body
microstructure evaluation.

Agitation Milling of Powders - D. B. Minor and S. G. Malghan

High energy agitation milling of silicon nitride powders is carried out with a minimum
contamination by the use of a specially designed milling system.  This milling device allows for
the size reduction of silicon nitride powder by milling at high slurry densities in approximately
1/6th to 1/10th of the time required by the conventional tumbling ball mill.  The mill is lined
with silicon nitride and the media are made of silicon nitride materials; hence, external sources
of contamination can be minimized.

Nuclear Magnetic Resonance (NMR) - P. S. Wang

The solid state NMR facility includes a Bruker MSL-400 NMR system capable of studying
almost all NMR-active nuclei in the periodic table in both solid and liquid states as well as
performing NMR imaging in proton and carbon-13 frequencies.  Currently, the operation
parameters for both states at proton, deuterium, carbon-13, and aluminum-27 have been defined
and proved by documented NMR spectra of organic and inorganic molecules.  The equipment
has been tuned to Si-29, Cu-63, and Y-89.

Scanning Electron Microscope/Image Analysis (SEM) Facility - J. F. Kelly

This laboratory is equipped with an Amray 1830 digital scanning electron microscope with LaB6
source and a Leitz optical microscope.  The SEM is equipped with a solid-state backscatter
detector and an ultrathin-window x-ray detector.  A Kevex Delta V EDS x-ray analysis and
image analysis system is interfaced to both the SEM and optical microscopes.  Automated
imaging capabilities enable rapid size and shape analysis of a variety of imaged features,
including ceramic powder particles and second phase regions in composite structures.  Fracture
stages have been developed for real time observation and measurement of in-situ crack
propagation in ceramic specimens.  The addition of an interior mounted phosphor screen with
video camera imaging provides the capability of imaging single-grain electron backscatter
diffraction patterns from bulk specimens.  This permits the measurement of crystallographic
orientation in ceramic specimens.

Thermal Analysis Facility - J. S. Wallace and J. E. Blendell

This facility includes equipment for measurement of behavior of ceramic materials in a wide
range of atmospheres and temperatures.  The equipment is comprised of a computer-controlled
differential pushrod dilatometer capable of measuring thermal expansion or sintering shrinkage
in vacuum, inert, oxidizing or reducing conditions from room temperature to 1600C.  The
atmosphere can be monitored using either a zirconia oxygen cell or an external mass spectrometer
using its own associated computerized data acquisition system.

The second major piece of equipment is a simultaneous thermal analysis (STA) system which
is capable of performing simultaneous thermogravimetric and differential thermal analysis from
room temperature to 1700C.  Atmospheres can be varied from vacuum to single and mixtures
of gases using a four-channel mass flow controller.  The STA is also connected to the mass
spectrometer system and it's associated data acquisition system.  The quadrapole mass
spectrometer system has a capability of analyzing to 512 AMU.

Chemical Laboratory Facilities - J. J. Ritter

Chemical synthesis of powders is carried out in a well equipped laboratory, which consists of
controlled atmosphere glove boxes, preparative chemical vacuum systems, and a chemical flow
reactor.  A range of powders can be synthesized for exploratory purposes.

Ceramics Powders Processing Laboratory - J. S. Wallace and J. E. Blendell

A processing laboratory for processing and sintering well controlled ceramic powders has been
assembled.  This facility consists of:  equipment for chemical powder synthesis routes, attrition
mills, ball mill, jet mill, pressure slip caster, uniaxial presses, cold isostatic press, spray dryers,
drying ovens, hot presses, air furnaces to 1700C, controlled atmosphere furnaces with associated
gas flow systems and oxygen sensors for temperatures to 1600C, graphite furnace for
temperatures to 2300C, and a hot-isostatic-press/gas-pressure sintering furnace capable of 2300C
and 200 MPa using graphite elements and insulation.

Nano-Size Powders Processing - E. Gonzalez, G. J. Piermarini and S. G. Malghan

This is a new facility which consists of equipment for powder handling in inert environment,
compaction of nano-size powders, and sintering under environment control.  The compaction
equipment was designed to facilitate the application of wide range of pressures (up to 5 GPa),
temperatures (cryogenic to 1000C), and environments.  The size of green ceramic produced in
this system is 3.0 mm diameter.

SURFACE PROPERTIES

Wear Tests - S. M. Hsu

A state-of-the-art friction and wear testing laboratory is available for the evaluation of materials
under different applications and conditions.  Contact geometries include pin-on-disk, cross
cylinders, ball-on-flat, ball-on-balls, flat-on-flat, and ring-on-block.  Various motions and
operating conditions are available to simulate many industrial applications.  Environmental
control includes temperature (room temperature to 1200C), vacuum, and humidity.

Surface Analysis - S. M. Hsu and R. S. Gates

Many modern specialized instrumentation are available for the analysis of surface properties of
materials.  Mechanical property measurement include hot hardness tester, Vicker's indenter, nano-
indentor, scratch test, and controlled-depth micro-scratch test.  Chemical property measurement
include time-resolved micro-Raman spectroscopy, FTIR microscopic spectroscopy, GC-MS, SEM
with EDX analysis, IR and UV spectroscopies with API compound identification files.  A
specially designed, organo-metallic specification facility is also available to detect surface
reaction products at ppm level.  Access to conventional surface analysis such as XPS, ESCA,
Auger, etc are also available through external contracts.

STM/AFM - S. M. Hsu

A digital commercial scanning tunnelling microscope (STM) and atomic force microscope (AFM)
is available to measure surface properties at atomic level.

Time-Resolved Micro-Raman - S. M. Hsu

This versatile facility consists of a pulsed Nd-YAG laser, a CW Ar-ion laser, a triple
monochromator, and a gated intensified diode array detector.  This facility, therefore, provides
a wide variety of Raman analysis techniques in both time-resolved and continuous operation
modes, using either visible or ultra-violet excitation sources for either operation mode.  In
addition, either bulk macro-Raman or 5-m-resolution micro-Raman analyses are available.

MECHANICAL PROPERTIES

Surface Forces Laboratory - D. T. Smith

The surface forces laboratory consists of a semi-clean-room preparation facility and a crossed-
cylinders surface force apparatus.  The crossed-cylinder apparatus permits measurements of
atomic-scale forces between surfaces.  It can be operated with a variety of liquid or gaseous
environments, thus allowing investigations of the effects of chemical changes on the forces
between two surfaces.  The apparatus includes several unique features that were developed and
built by the surface forces group.  First, sensitive custom electrometer circuits were built into the
apparatus to allow in-situ measurements of surface charges resulting from contact electrification. 
Second, the apparatus has been modified to permit the sliding of one surface over the other under
constant applied load.

Instrumented Microindenter - D. Smith

This apparatus is designed to bridge the gap between conventional hardness testers and the nano-
indentation facility.  It measures continuous load-displacement curves for indentations in the load
range 10 g to 2 kg, and is of particular use in studying the mechanical properties of thermal-spray
and other ceramic coatings with relatively coarse microstructures.

Analytical Electron Microscopy - B. J. Hockey

Several transmission and scanning electron microscopes are available for analysis of the changes
in microstructure as a result of creep. 

Glass Melting -  D. A. Kauffman

Extensive glass melting and annealing facilities for production of melts up to 1600C are
available.  Batch sizes up to about (2.5 to 3) kg can be produced using this equipment.  Special
facilities for melts containing heavy metals such as thallium and lead are also available.

Creep Apparatus - R. F. Krause, Jr. and S. M. Wiederhorn

The creep measurements laboratory possesses nineteen controlled-temperature furnaces (800 C
to 1700C), seven laser extensometers, ten optical long-distance microscopic extensometers, and
twenty loading frames (fourteen pneumatically driven, four screw driven, and two direct weight). 
Among these loading frames fourteen can be used in tension, three in tension or compression,
one in flexure, and one as a sintering forge.

Hot-Pressing Apparatus - R. F. Krause, Jr.

A graphite heating-element furnace (2300C maximum) which be can operated in vacuum or an
inert gas atmosphere is mounted in a hydraulic loading frame (0.5 MN maximum).  Ceramic
powders can be hot pressed in graphite dies, (50, 75, 100, and 125) mm diameter.

Nano-Indentation Facility - D.T. Smith

The Ceramics Division nano-indentation facility consists of a Nano Indenter II indentation
machine, manufactured by Nano Instruments, Inc., and related computer and optical components. 
The indenter, under computer control, is capable of measuring loading-unloading curves with
displacement resolution better than 0.1 nm and load resolution better than 200 nN.  Nomarski
interference contrast (NIC) optics and translation stages with placement precision better than
1 m permit the measurement of material properties such as hardness and Young's modulus in
selected volumes as small as 10-17 m3.

Optical Microscopy Laboratory - G. D. Quinn

The optical microscopy laboratory is equipped with conventional reflected light microscan
inspection of polished specimen as well as stero-binocular microscopes and camera stands for
fracture surface analysis.   A WILD M-10 stereo discussion microscope system with video
monitoring and instant photography capability is very well suited for fractography.

ELECTRONIC MATERIALS

Level 10 Clean Room - J. E. Blendell

A Level 10 Clean Room has been constructed for the processing of ceramics in a controlled
environment where the presence of air contaminants at low levels can seriously affect the final
product's properties.  The room is provided with separated work stations to allow simultaneous
conduct of experiments.

Thermal Wave Analysis Facility - A. Feldman and G. S. White

This facility is used for characterizations based on variations of thermal diffusivities.  Equipped
with both an Ar-ion and CO2 laser, the facility permits analyses by infrared and mirage methods. 
It is especially useful as a nondestructive method of detecting flaws in near-surface regions of
ceramics.

OPTICAL MATERIALS

Optical Characterization - L. H. Robins and A. Feldman

Facilities include a Cary spectrophotometer for measuring optical transmittance in the spectral
range 0.2 m to 2.5 m, optical spectrometers for measuring photoluminescence and Raman
spectra, and an argon ion laser.

Magneto-Optical Imaging of High Temperature Superconductors - D. L. Kaiser, F. W. Gayle
(Metallurgy) and A. Shapiro (Metallurgy).

The facility consists of a magneto-optical imaging system with attached video equipment.  It is
used to measure real-time flux distributions in high-temperature superconductors as a function
of temperature, (7 - 300) K, and applied magnetic field, (0 to  65) mT.

Electro-optic Thin-film Characterization - L. D. Rotter

The facility consists of a vibration-isolated optical table, argon-ion and helium-neon laser sources,
polarizing components, lenses, optical stages, optical detectors, and electronic signal processing
equipment for measuring the electro-optic coefficients and optical birefringence of thin ferro-
electric films.

Metalorganic Chemical Vapor Deposition (MOCVD) System - D. L. Kaiser

A specialized system was constructed for the deposition of oxide thin films from metalorganic
precursors.  It has been used to deposit BaTiO3 films on 1.5 cm x 1.5 cm substrates.

Diamond Film Deposition - E.N. Farabaugh and A. Feldman

Facilities consist of three hot-filament CVD reactors and a microwave-enhanced CVD reactor. 
The hot-filament reactors can accommodate substrates up to 2.5 cm X 2.5 cm square.  The
microwave reactor can accommodate substrates up to 10 cm in diameter.  The reactant gases are
hydrogen, methane, oxygen, argon, and ethyl alcohol which contains boron of doping.  Growth
rates typically range from (0.1 to 0.6) m/h.

MATERIALS MICROSTRUCTURE CHARACTERIZATION

Synchrotron Radiation Beamlines -  G. G. Long

The Materials Microstructure Characterization Group operates two beamstations on the X23A
port at the National Synchrotron Light Source at Brookhaven National Laboratory in New York. 
These two beamstations offer access to dedicated instrumentation for small-angle x-ray scattering,
x-ray diffraction imaging (topography) and EXAFS.

Small-angle x-ray scattering can be carried out in the energy range from (5 to 11) keV.  The
minimum wavevector is 4 x 10-3 nm-1 and the wavelength resolution is ^/^ = 10-4, allowing
anomalous small-angle scattering with excellent resolution.  Diffraction imaging of single crystals
and powders is carried out with monochromatic photons between (5 and 30) keV.  An energy-
tunable, x-ray image magnifier enables imaging of microstructure down to less than 1 m. 
EXAFS experiments are also performed over an energy range from (5 to 30) keV.
   
Small-angle scattering measurements on ceramic and metallurgical materials are being used to
characterize the microstructure in the 2 nm to 1 m size range as a function of starting chemistry
and processing parameters.  Diffraction imaging is being used to study imperfections and strains
in single crystals and powder compacts.  EXAFS is being used to study the structure of strained
semiconductor interfaces and metal multilayers.  A combination of EXAFS and diffraction will
provide a capability for site-specific local structure determination in crystals.

SANS - Ceramics Furnace - G. Long

The SANS-Ceramic furnace is a unique facility that has been recently commissioned.  This
system allows simultaneous in-situ densification studies of ceramic powders and SANS
measurements.  The experimental system has been designed to carry out densification studies of
oxide powders at temperatures up to 2000C.  In addition, the furnace will be equipped with a
dilatometer. 

PHASE EQUILIBRIA

Single Crystal X-ray Diffraction Facility- W. Wong-Ng

Currently, this research facility is primarily used to characterize single crystals in terms of crystal
symmetry, lattice parameters and detailed structure. 

Phase Equilibrium Facilities for High-Tc Superconductor Systems Bi(Pb)-Sr-Ca-Cu-O and Ba-R-
Cu-O - W. Wong-Ng and L.P. Cook.

This facility consists of two controlled-atmosphere, quenched furnaces and a Mettler thermal
analyzer for performing DTA/TGA experiments.  Both solid and melt can be quenched into
liquid nitrogen cooled helium atmosphere so that the high temperature structure can be captured
and analyzed. Liquid composition can also be estimated quantitatively with a wicking method
during the quenching experiments.

                                 APPENDIX