AN ASSESSMENT OF THE 

NATIONAL INSTITUTE OF STANDARDS 

AND TECHNOLOGY 

MATERIALS SCIENCE AND 

ENGINEERING LABORATORY 

FISCAL YEAR 2010 

Panel on Materials Science and Engineering 

Laboratory Assessments Board 

Division on Engineering and Physical Sciences 

THE NATIONAL ACADEMIES PRESS 

Washington, D.C. 

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Medicine. The members of the panel responsible for the report were chosen for their special 

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This study was supported by Contract No. SB134106Z011, TO#8, between the National 

Academy of Sciences and the National Institute of Standards and Technology, an agency of 

the U.S. Department of Commerce. Any opinions, findings, conclusions, or 

recommendations expressed in this publication are those of the authors and do not 

necessarily reflect the views of the agency that provided support for the project. 

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www.national-academies.org 
iv 

PANEL ON MATERIALS SCIENCE AND ENGINEERING 

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

JOHN ALLISON, University of Michigan 

DAVID B. BOGY, University of California, Berkeley 

PETER R. BRIDENBAUGH, Alcoa (retired) 

DUANE B. DIMOS, Sandia National Laboratories 

FRANCIS J. DISALVO, Cornell University 

MARK EBERHART, Colorado School of Mines 

KATHARINE M. FLORES, Ohio State University 

WILLIAM W. GERBERICH, University of Minnesota 

WILLIAM A. GODDARD III, California Institute of Technology 

BRIDGETTE L. GOMILLION-WILLIAMS, Saint-Gobain Performance Plastics 

RIGOBERTO HERNANDEZ, Georgia Institute of Technology 

FRANK P. INCROPERA, University of Notre Dame 

BERNARD H. KEAR, Rutgers, The State University of New Jersey 

CHRISTOPHER W. MACOSKO, University of Minnesota 

EDMUND H. MOORE, Air Force Research Laboratory 

OMKARAM NALAMASU, Applied Materials 

THOMAS P. RUSSELL, University of Massachusetts, Amherst 

JUDITH A. SCHNEIDER, Mississippi State University 

MARK L. WEAVER, University of Alabama 

Staff 

JAMES P. McGEE, Director 

CY BUTNER, Senior Program Officer 

LIZA HAMILTON, Administrative Coordinator 

EVA LABRE, Program Associate 
v 

Acknowledgment of Reviewers 

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

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

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

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

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

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

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

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

their review of this report: 

Ilhan Aksay, Princeton University, 

Morton Denn, City College of New York, City University of New York, and 

Gary Grest, Sandia National Laboratories. 

Although the reviewers listed above have provided many constructive comments 

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

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

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

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

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

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

rests entirely with the authoring panel and the institution.

vii 

Contents 

SUMMARY 1 

1 THE CHARGE TO THE PANEL AND THE ASSESSMENT PROCESS 5 

2 CERAMICS DIVISION 7 

3 MATERIALS RELIABILITY DIVISION 16 

4 METALLURGY DIVISION 26 

5 POLYMERS DIVISION 41 

6 OVERALL CONCLUSIONS 54 

1 

Summary 

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

Institute of Standards and Technology (NIST) works with industry, standards bodies, 

universities, and other government laboratories to improve the nation’s measurements 

and standards infrastructure for materials. Its work is aligned with the mission of NIST, 

which is to promote U.S. innovation and industrial competitiveness by advancing 

measurement science, standards, and technology in ways that enhance economic security 

and improve our quality of life. 

 At the end of fiscal year (FY) 2009, the MSEL consisted of 104 permanent 

technical staff, 34 National Research Council (NRC) postdoctoral researchers, 13 term 

appointees, 161.2 associates,1 and 21 administrative support staff, with total funding of 

$52.6 million. The MSEL is organized into four divisions: Ceramics, Materials 

Reliability, Metallurgy, and Polymers. 

 A panel of experts appointed by the NRC assessed the four divisions, attending 

interactive presentations, touring laboratories, and engaging in small-group discussions 

with postdoctoral researchers and early-career staff. As requested by the Director of 

NIST, the scope of the assessment included the following criteria: (1) the technical merit 

of the current laboratory programs relative to current state-of-the-art programs 

worldwide; (2) the adequacy of the laboratory’s budget, facilities, equipment, and human 

resources, as they affect the quality of the laboratory’s technical programs; and (3) the 

degree to which laboratory programs in measurement science, standards, and services 

achieve their stated objectives and desired impact. 

TECHNICAL MERIT 

 On the basis of its assessment of the MSEL conducted in March 2010, the NRC’s 

Panel on Materials Science and Engineering concluded that, overall, with a few 

exceptions as noted in the report, for the selected portion of the MSEL programs 

reviewed, the projects are outstanding. They are clearly focused on the mission of the 

MSEL and have produced results that have garnered recognition through awards and 

frequent citations in the literature as well as from strong support by industry and the 

worldwide research community for standard reference materials (SRMs) and standard 

reference data. 

FACILITIES, EQUIPMENT, AND HUMAN RESOURCES 

 The facilities and equipment of the MSEL are being upgraded within budget 

constraints. Notably, the new Hydrogen Test Facility is now operational, and the 

Precision Measurement Laboratory, which will provide some laboratory space to the 

Materials Reliability Division, will open this year. However, the building that houses 

most of the Materials Reliability Division laboratories is subject to flooding and has poor 

 1

 NIST associates, comprising contractors and guest researchers, are reported in terms of workyears. Other staff numbers represent numbers of individuals. 
2 

electrical power. Both issues reduce the productivity of the staff. Other MSEL facilities 

and laboratories are among the best in the world, and in several cases they are unique. 

 Since 2008, the MSEL has hired several full-time staff to replace retirees and 

transferred staff. It increased the postdoctoral temporary staff through the highly 

competitive NRC-administered National Academies Research Associateship Program. 

The morale of the staff and leadership is high. The postdoctoral appointees and earlycareer staff interviewed by the panel during the current assessment are impressive. 

MEETING OBJECTIVES AND IMPACT 

 The MSEL technical staff is highly productive as measured by its publication in 

refereed journals, output of products (such as SRMs and standard reference databases 

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

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

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

enhances the reputation and stature of NIST. The relatively new SRMs for 

nanotechnology are popular with researchers worldwide, as are the Charpy test specimens 

and supporting analyses that have been a signature contribution of NIST for decades. 

 The findings and recommendations of the panel are cited in the division 

chapters—Chapters 2 through 5—for each group, and at the division level for those 

issues that are common to several groups. Findings and recommendations that are at the 

MSEL level are summarized below. Chapter 1 describes the charge to the panel and the 

assessment process, and Chapter 6 contains the panel’s overall conclusions. 

POSTDOCTORAL PROGRAMS 

 The MSEL has embraced the NRC-administered National Academies Research 

Associateship Program to attract outstanding researchers. Not only do these individuals 

do noteworthy research during their appointments, but they also provide a pool of 

talented individuals for consideration for permanent positions. Approximately 20 

postdoctoral associates and recent hires from the Research Associateship Program who 

were interviewed evidenced impressive capabilities and enthusiasm; all but one of them 

wanted to have a full-time appointment to the MSEL (the one exception was targeting an 

academic appointment). 

Finding: Even though all of the interviewed postdoctoral researchers stated that 

they are favorably impressed by the MSEL, their individual experiences there vary 

widely, from being essentially technicians to being fully and quickly integrated into 

research programs. A few of the postdoctoral researchers interviewed commented on the 

uneven nature of the assignments (not always their own experience). In a few cases, the 

postdoctoral associates were encouraged to write research proposals with internal or 

external collaborators and developed skills that will be useful at NIST or elsewhere. 

Recommendation: The experience of the postdoctoral appointees should be 

enhanced through the establishment of clearly defined expectations for the staff and 

managers fortunate enough to have postdoctoral associates. The minimum requirements 
3 

should include a meaningful role in an ongoing research program and strong 

encouragement to develop research proposals submitted to secure appointments or an 

alternate that would enhance the capabilities of the postdoctoral associates. An 

independent review process should be established to assess postdoctoral experiences as a 

basis for continuous improvement. 

PATENT POLICY AND IMPLEMENTATION

 Improving intellectual property management, notably, applying for more patents, 

could enhance MSEL’s mission to promote U.S. innovation and industrial 

competiveness. 

Finding: There are several examples of technology developed to advance 

measurement science and standards that could have significant commercial value, but 

there was little discernible interest in filing patent disclosures. The current MSEL and 

NIST leadership encourages staff to file disclosures; however, the history of little support 

for such efforts and the experience of senior staff that these efforts are not appreciated or 

rewarded tend to discourage action by senior new staff. 

Recommendation: The relatively recent decision to develop actively the 

intellectual property generated in MSEL and NIST should be vigorously pursued. The 

fundamentals of the process appear to be in place. Developing technology from a 

laboratory demonstration to commercial production requires significant investment, 

typically millions of dollars and several years. That level of investment requires patent 

protection and an exclusive license to a commercial entity. The processes to ensure 

fairness are somewhat cumbersome, but they should not be allowed to diminish the 

effectiveness of the MSEL in fulfilling its mission.

WEB-BASED INFORMATION DISSEMINATION 

 Improving the ability to disseminate information in the form of data and models 

would greatly improve the effectiveness and visibility of NIST. 

Finding: Some groups within the MSEL effectively use the World Wide Web to 

disseminate high-quality data and models; however, the MSEL has an opportunity to do 

much more. The use of this relatively new dissemination venue is non-uniform, and 

some groups appear to have no such tools. This opportunity was identified during the 

2008 NRC review of the laboratory; however, only one new project was reported 

(Atomistic Potentials Repository, in the Metallurgy Division), and little additional 

progress was evident. In a recent National Materials Advisory Board report on Integrated 

Computational Materials Engineering (ICME), NIST was identified as having an 

important role to play in the development of such dissemination mechanisms.2

 2

 National Research Council, Integrated Computational Materials Engineering: A 

Transformational Discipline for Improved Competitiveness and National Security. Washington, D.C.: The 

National Academies Press, 2008, pp. 31-32, 125. 
4 

Recommendation: The MSEL should develop a comprehensive approach to data 

and model dissemination and collaboration on the Web. As part of such an assessment, 

the MSEL should also follow the recommendations of the National Research Council’s 

2008 Integrated Computational Materials Engineering report. Efforts in the 

Thermodynamics and Kinetics Group (Metallurgy Division) should be viewed as a role 

model for this activity. Some specific opportunities have been identified within the 

Metallurgy Division for disseminating high-strain-rate and sheet-forming mechanical 

behavior data and models. A comprehensive approach to this problem would provide 

industry and academic researchers with ready access to information developed at NIST. 

A comprehensive assessment should also consider the issues and opportunities for 

providing repositories for high-quality information developed by researchers external to 

NIST. 

PERFORMANCE METRICS 

 Consistent metrics for assessing the productivity of staff would help ensure a high 

level of professionalism across the MSEL organization. 

Finding: Metrics of productivity are not always evident or uniformly articulated. 

Recommendation: MSEL management should evaluate the utility of uniform 

metrics for such things as publications (e.g., h factor analysis), external support, patents 

and disclosures, and other factors, and apply them to various subunits and compare the 

results to selected benchmark groups. 
5 

1 

The Charge to the Panel and the Assessment Process 

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

Research Council has, since 1959, annually assembled panels of experts from academia, 

industry, medicine, and other scientific and engineering environments to assess the 

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

there are now nine,3

 as well as the adequacy of the laboratories’ resources. In 2010, 

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

Laboratory, the Manufacturing Engineering Laboratory, the Materials Science and 

Engineering Laboratory, the NIST Center for Neutron Research, and the Physics 

Laboratory. Each of these was assessed by a separate panel of experts; the findings of the 

respective panels are summarized in separate reports. This report summarizes the 

findings of the Panel on Materials Science and Engineering. 

 For the FY 2010 assessment, NIST requested that the panel consider the 

following criteria as part of its assessment: 

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

 state-of-the-art programs worldwide; 

2. The adequacy of the laboratory budget, facilities, equipment, and human 

resources, as they affect the quality of the laboratory’s technical programs; 

and 

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

and services achieve their stated objectives and desired impact. 

The context of this technical assessment is the mission of NIST, which is to 

promote U.S. innovation and industrial competitiveness by advancing measurement 

science, standards, and technology in ways that enhance economic security and improve 

the quality of life. The NIST laboratories conduct research to anticipate future metrology 

and standards needs, to enable new scientific and technological advances, and to improve 

and refine existing measurement methods and services. 

In order to accomplish the assessment, the NRC assembled a panel of 20 

volunteers, whose expertise matches that of the work performed by the MSEL staff.4

 The 

panel members were also assigned to four subgroups (division review teams), whose 

expertise matched that of the work performed in the four divisions in the MSEL: 

(1) Ceramics, (2) Materials Reliability, (3) Metallurgy, and (4) Polymers. These division 

review teams individually visited MSEL facilities in Gaithersburg, Maryland, and 

 3

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

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

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

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

the Physics Laboratory. 4

 See http://www.nist.gov/msel/ for more information on Materials Science and Engineering 

Laboratory programs. Accessed May 1, 2010. 
6 

Boulder, Colorado, for a day to a day and a half, during which time they attended 

presentations, tours, demonstrations, and interactive sessions with MSEL staff. 

Subsequently, the entire panel assembled for a day and a half at the NIST facilities in 

Gaithersburg, Maryland (on March 1-3, 2010), during which it received welcoming 

remarks from the NIST Director’s representative, an overview presentation by MSEL 

management, and an interactive session with MSEL management. The panel also met in 

a closed session to deliberate on its findings and to define the contents of this assessment 

report. 

 The approach of the panel to the assessment relied on the experience, technical 

knowledge, and expertise of its members, whose backgrounds were carefully matched to 

the technical areas of MSEL activities. The panel reviewed selected examples of the 

technological research covered by the MSEL; because of time constraints, it was not 

possible to review the MSEL programs and projects exhaustively. The examples 

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

report salient examples of accomplishments and opportunities for further improvement 

with respect to the following: the technical merit of the MSEL work, its perceived 

relevance to NIST’s own definition of its mission in support of national priorities, and 

specific elements of the MSEL’s resource infrastructure that are intended to support the 

technical work. These examples are intended collectively to portray an overall 

impression of the laboratory, while preserving useful suggestions specific to projects and 

programs that the panel examined. The assessment is currently scheduled to be repeated 

biennially, which will allow, over time, exposure to the broad spectrum of MSEL 

activity. The panel applied a largely qualitative rather than a quantitative approach to the 

assessment, although it is possible that future assessments will be informed by further 

consideration of various analytical methods that can be applied. 

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

MSEL exhaustively. Instead, the report identifies key issues. Given the necessarily 

nonexhaustive nature of the review process, the omission of any particular MSEL 

program or project should not be interpreted as a negative reflection on the omitted 

program or project. 
7 

2 

Ceramics Division 

SUMMARY

 The mission of the Ceramics Division is to promote U.S. innovation and industrial 

competitiveness in the development and use of materials by advancing measurement 

science, standards, and technology in ways that enhance economic security and improve 

our quality of life. The Ceramics Division has 22 NIST permanent technical staff, 3 NRC 

postdoctoral researchers, 4 term employees/students, 31.3 research associates (see 

footnote 1), and 6 administrative and support staff. Approximately 50 percent of the staff 

is physicists. The total budget in FY 2009 was $14.5 million, with $271,000 coming from 

other agencies. The division is organized into four groups: Nanomechanical Properties; 

Functional Properties; Synchrotron Methods; and Structure Determination Methods. 

 The chief of the Ceramics Division presented for the division review team a 

comprehensive overview, including as topics the mission, organization, staffing, budget, 

facilities, equipment, and core competencies. The overview was followed by 

presentations from the group leaders and tours of three laboratories. 

 The format of the review worked well. The presentations were nicely focused, 

and the laboratory tours provided a good impression of the excellent facilities. The staff 

discussions helped the panel members understand the work environment. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

 The staff of the Ceramics Division are knowledgeable and recognized as leaders 

in their respective fields. Their output was 147 refereed journal publications over the 

past 2 years, not counting open-software and reference materials. There also has been a 

concerted effort in the division to publish in high-impact journals, which was effectively 

demonstrated in the breakdown of publications relative to journal impact factor. There 

were 3 NIST publications or reports, 24 referred conference proceedings, and 13 review 

articles or book chapters. Several division scientists received important awards, career 

and early-career awards, and competitive NIST awards. The staff is also well engaged in 

professional society activities, which demonstrates good technical leadership. 

 The division’s programs continue to address critical scientific and technical issues 

in their respective fields, guided by the well-defined mission of NIST to advance 

measurement science, standards, and technology. There is no organization with a 

comparable focus in the United States, so a direct comparison with the performance of 

other government laboratories is not feasible. Nevertheless, judged by the standards of 

the scientific community, the quality of research performed in this division ranks with the 

best in the world. 
8 

ADEQUACY OF BUDGETS, FACILITIES, AND HUMAN RESOURCES 

 Other than the occurrence of a budget spike in FY 2007, the budgets have been 

stable over the past 5 years. 

 State-of-the-art facilities for measurement science have long been a feature of the 

NIST organization. The division’s facilities are top-notch, and all of the laboratories 

examined are in good shape. In particular, the Nanomechanics Cleanroom Facility in the 

Advanced Measurement Laboratory represents an outstanding capability. Group leaders 

and staff are generally satisfied with the breadth and quality of the equipment, which 

includes equipment that is among the best in the world and some that is unique. There 

was also heavy infrastructure investment in FY 2009. Highlights include the American 

Recovery and Reinvestment Act of 2009 (ARRA; Public Law 111-5) funding of an 

equipment investment of $1.9 million to the Synchrotron Methods Group for the near 

edge x-ray absorption fine structure (NEXAFS) Microscope Endstation at the National 

Synchrotron Light Source (NSLS)-I and -II and $1 million for the Nanomechanical 

Properties Group for the Imaging X-ray Photoelectron Spectroscopy System (for the 

nanomaterial environmental, health, and safety [EHS], Nano-EHS Program). 

 Since the 2008 review, several excellent new staff hires have occurred to backfill 

for recent retirements. The division has demonstrated that it can hire new staff 

expeditiously. Newly hired staff are thriving in this laboratory environment through a 

combination of mentorship, freedom to pursue their work, and good leadership. Active 

leadership development is helping to reinvigorate the workforce. In addition, two NRC 

postdoctoral researchers are expected in the summer of 2010. Bringing in additional 

NRC postdoctoral researchers is an opportunity for this division, which has the fewest of 

them in the MSEL. 

 The technical staff of NIST is well known worldwide for their collective expertise 

in all aspects of measurement science and standards. In addition, the Ceramics Division 

chief is the designated lead of the NIST Nano-EHS Program and has demonstrated strong 

institutional leadership on this topic. The division is now shifting emphasis into vitally 

important areas, such as health and safety, structural and functional nanomaterials, 

advanced synchrotron technologies, and sustainable and renewable energy materials. 

 As a part of these new technical thrusts, the division is making strategic 

investments in human resources. As a prestigious institution with a well-recognized track 

record, NIST is attracting high-caliber new staff. In particular, the impressive earlycareer staff and postdoctoral researchers are receiving excellent mentoring, they are 

excited by the projects on which they are working, and they are already formulating a 

vision of what needs to be done to maintain a leadership position in their research areas. 

Box 2.1 illustrates how professional leadership has produced an important new research 

project. 

ACHIEVEMENT OF OBJECTIVES AND DESIRED IMPACT 

 The Ceramics Division has met its objective of developing and disseminating 

measurement science, standards, and technology relevant to mechanical properties, 

functional properties, structure determination, and synchrotron methods for the 

development and use of advanced materials. Personal interaction and organized 
9 

BOX 2.1 

Professional Leadership Produces Important New Research Project 

 The Materials Science and Engineering Laboratory encourages the participation 

of its staff and managers in professional organizations to help disseminate its 

accomplishments, attract staff and postdoctoral candidates, and promote professional 

growth, and to help define research projects. The latter is well illustrated by a growing 

project that resulted from a group leader’s having the honor of being elected to chair a 

Gordon Conference in 2006. This MSEL staff member chose a topical area that excited 

participants who were facing a common technical problem of determining “local 

structure” from x-ray diffraction analyses. The results include the distinction of having 

an invited article by MSEL authors in Science magazine (an honor), a new project (Local 

Structure Determination), a workshop hosted by NIST, and 14 publications, the most 

recent being selected as an Editor’s Choice in Physical Review B. 

workshops account for good customer engagement. For example, six major workshops 

have been hosted since October 2008—all of which have contributed to a sharpening of 

the focus of existing and potentially new programs. The production of SRMs, 

documentary standards, SRDs, and data analysis software continues to provide an 

invaluable service to the entire materials community worldwide. 

TECHNICAL PROGRAM REVIEW 

Nanomechanical Properties Group 

 The Nanomechanical Properties Group consists of 5 NIST permanent technical 

staff, 2 NRC postdoctoral associates, 3 term employees or students, 18.1 NIST associates 

(see footnote 1), and 1 administrative staff member. The stated objectives of the group 

are to develop mechanical measurement science, standards, and technology needed by 

U.S. industry to apply materials and components in nanomechanical applications. This 

group continues to perform high-quality research in scanning probe microscopy, 

nanoparticle metrology, and nanoscale stress and strength measurements. Its budget in 

FY 2009 was $4.3 million. 

 This group is mature, understands the unique mission of the laboratory, and has 

acted accordingly. Looking beyond that, it has recognized the importance of having 

control of the materials that it is measuring. In a few cases, notably theta-section 

fabrication and laser ablation of films, the group has already taken a step in this direction. 

 Improvements in scanning probe microscopy measurement techniques are needed 

by the broad materials community, and researchers in this group are providing leadership 

on this topic. The achievements to date are impressive. In particular, the progress in the 

development of an electromechanical coupling measurement method for extremely thin 

films and elastic modulus measurements of nanowires and nanotubes are noteworthy. 

The nanoparticle metrology project team has assembled excellent capabilities to 

investigate laser light scattering, optical spectroscopy, and field-flow fractionation. 

Advances in confocal Raman microscopy, strain measurement by electron diffraction, 
10 

and related areas are significant and continue to make an impact in the scientific 

literature. 

 Nanoscale stress and strength measurements show significant progress on all 

fronts. A highlight of this research is the optimization of a photolithographically formed 

“theta” device for micro-tensile strength measurements. The device is robust, reliable, 

and versatile. 

 Nanoindentation-based elastic, plastic, viscous, and fracture measurements 

continue to be a productive area of research, with numerous publications to the group’s 

credit in archival journals. 

 The Nanomechanics Cleanroom Facility is impressive. It surely will provide 

unmatched capabilities for conducting atomic force microscopy, scanning tunneling 

microscopy, and nanoindentation measurements without being compromised by concerns 

with respect to sample contamination. This facility will likely assume even greater 

importance as device technology advances progressively into the nanoscale domain. 

Working closely with nanodevice manufacturers should be a rewarding activity. 

 Opportunity areas for further research include the design, fabrication, and testing 

of nanoscale sensors and electromechanical devices to monitor and assess the reliability 

of large-scale engineered structures. Another opportunity area is that of self-healing 

nanostructured coatings to replace chromate-based protective coatings for diverse 

applications. 

 The panel’s findings and recommendations with respect to the Ceramics 

Division’s Nanomechanical Properties Group are as follows: 

 Finding: The electromechanical measurement method for thin films has potential 

for broader use. 

Recommendation: As a new initiative, this technology should be applied to 

nanocrystalline (one phase) and nanocomposite (two or more phases) ceramics where 

there is a need to determine changes in hardness, stiffness, and wear properties across 

nanograin and nanophase boundaries. In addition, precise measurements on high-density 

ceramics to determine unequivocally the dependence of hardness on grain size extending 

from micro- to nanoscale dimensions would be beneficial. 

 Finding: The theta test device is a powerful tool for exploring mechanical 

properties of materials. 

 Recommendation: The “gapped-theta” design for determining the strength and 

stiffness of micro- and nanofibers of materials should be evaluated. Beyond that, there 

are opportunities to modify the device further to perform microscale and nanoscale 

measurements of (1) temperature dependence of tensile strength and fracture behavior, 

(2) low- and high-cycle fatigue properties, and (3) susceptibility to stress-corrosion 

cracking. The ability to carry out these tests on carbon fibers would also be invaluable, 

now that carbon-fiber-reinforced composites are being used in commercial and military 

aircraft. 
11 

 Finding: Knowing the details of a material synthesis process is often essential to 

understanding its properties, but existing capabilities are limited. 

 Recommendation: The “nanofabrication” capabilities should be upgraded to 

provide high-quality materials for property and performance measurements, as well as for 

in-depth materials characterization. 

 Finding: The nanoindentation work merits expansion. 

 Recommendation: The nanoindentation effort should be expanded to include 

nanowear, nanoscratch, and nanoimpact tests. For example, scratching experiments 

performed at ramped loads could enable the measurement of the critical load at which 

failure occurs in bulk materials, or at which decohesion occurs for coatings. High-cycle 

fatigue tests could be performed by oscillating the sample, causing the diamond probe to 

impact the surface repetitively at high frequency until failure occurred. These are 

significant challenges, but well within the capabilities of the Nanomechanical Properties 

Group’s personnel. 

Functional Properties Group 

 The Functional Properties Group consists of four NIST permanent technical staff, 

one NRC postdoctoral researcher, and 4.2 NIST associates (see footnote 1). The stated 

mission of the Functional Properties Group is to (1) develop and disseminate 

measurement science, standards, and technology pertaining to functional properties of 

advanced materials and devices; and (2) determine and disseminate key data needed to 

establish the relationships between structure, properties, and performance of functional 

materials for advanced applications in energy, sustainability, and microelectronics. The 

stated mission is broad, but the group is focused on four technical areas: (1) energy 

conversion materials, (2) carbon mitigation, (3) nanocalorimetry, and (4) combinatorial 

measurement methods. This group is relatively new and, from the perspective of its 

$2.6 million budget, is the smallest of the four groups in the Ceramics Division. 

 This group is in the process of getting fully established, which is consistent with 

the number of early-career group members. The group has some excellent external 

collaboration with industry and academia, including good international collaborations 

with top institutions (e.g., the Interuniversity Microelectronics Center [IMEC] in Belgium 

and the National Institute for Materials Science [NIMS] in Japan). 

 In the area of energy conversion materials, this group has and is developing a 

comprehensive suite of characterization capabilities for thermoelectric materials. The 

intent is to develop standard reference materials and determine the best measurement 

techniques and protocols for characterizing thermoelectric performance. Standard test 

methods and unique test systems developed by NIST are being effectively used to 

address the stated goals of the group, which has also developed a range of good partners 

(industrial and academic) on this topic. NIST has also established a combinatorial 

materials effort focused on characterization methods, which has been effectively applied 

to determining work function in gate electrode systems. Interactions with Micron 

Corporation, SEMATECH, IMEC, and NIMS on this topic are noteworthy. The group is 
12 

now appropriately looking for ways to take further advantage of this combinatorial 

materials effort by applying it to thermoelectric materials in combination with their other 

technique development on thermoelectrics. 

 In terms of establishing new, leading-edge capabilities, the effort to develop a 

chip-based nanocalorimetry capability seems quite novel. This relatively new work has 

some good, early accomplishments and, if successful, should provide a new capability 

that can be applied broadly. Noteworthy here is that Micron Corporation is supporting a 

student intern at NIST to increase its engagement with this effort. Also valuable are 

additional collaborations on this topic with the NIST Nanofab facility in the NIST Center 

for Nanoscale Science and Technology, with the University of Illinois at UrbanaChampaign, and with the Johns Hopkins University. A new effort on measurement needs 

related to carbon mitigation has been initiated. Measurement challenges have been 

identified, but it is too early to evaluate the focus or progress of this project. 

 Two noteworthy accomplishments were achieved by the group this year. The first 

was the development and certification of a Bi2Te3 Seebeck coefficient SRM for the 

calibration of measurement apparatus. In addition, a NIST Bronze Medal was awarded to 

one of the staff for exceptional programmatic leadership over an extended period. 

 The panel’s finding and recommendation with respect to the Functional Properties 

Group are as follows: 

 Finding: There is substantial room for the Functional Properties Group to expand 

technically, especially in the area of energy conversion materials, where batteries and 

capacitors were identified as an appropriate growth area. 

 Recommendation: The Functional Properties Group should continue to hold 

workshops, such as the upcoming workshop on carbon mitigation planned for 2011, to 

determine how NIST can best contribute to broad and fast-moving fields from the 

perspective of measurement science and technology. 

Synchrotron Methods Group 

 The Synchrotron Methods Group consists of three NIST permanent technical staff 

members and four associates. The mission of the Synchrotron Methods Group is 

measurement science and technology that pertains to chemical and electronic structure of 

advanced materials and devices by synchrotron methods. The group is meeting its 

objectives by developing state-of-the-art methods and making them available to NIST 

users and other collaborators. The suite of spectroscopy beam lines at the National 

Synchrotron Light Source impressively spans the entire Periodic Table and served 110 

users with 90 experiments over the past year. Funding for the Synchrotron Methods 

Group has increased appropriately, from $2.5 million to $3.0 million over the past 

2 years. Capability upgrades have been realized through ARRA and Small Business 

Innovative Research (SBIR) III funding. 

 The group is also appropriately focused on working with the Brookhaven 

National Laboratory on the NSLS-II project, which is a billion-dollar facility that will 

have x-ray beams with improved coherence and tunability and increased brightness (by 

10,000 times) in comparison with the current NSLS facility. The NIST group at 
13 

Brookhaven appears to be an important stakeholder in the planning of this new national 

facility, which is expected to start construction in 2010, with start of operations in 2015. 

 The x-ray absorption fine structure spectroscopy (XAFS) at beam line X23A2 

demonstrated a major accomplishment of revealing ferroelectric functionality of SrTiO3

thin films on Si by means of piezo-force microscopy.5

 A cryostat sample holder will be 

added to this capability next year. In addition, the group works well with the Polymers 

Division, which led to determining the molecular structure-function relationship of a 

mixture of polymer-fullerenes using NEXAFS beam line U7A at NSLS. 

 The hard x-ray photoelectron spectroscopy (HAXPES) beam line X24A has been 

an important part of a SEMATECH collaboration on semiconductor gate stacks. The 

x-ray photoelectron spectroscopy (XPS) three-dimensional chemical microscope, which 

is under development at beam line U4A at NSLS, appears to be an excellent capability 

that ranks among the best in the world. In addition, excellent work continues with the 

Ultra-Small Angle X-ray Scattering (USAXS) facility at the Advanced Photon Source, 

Argonne National Laboratory. One good example was the certification of gold 

nanoparticle size for NIST reference materials: 8011, 8012, and 8013. 

 The Synchrotron Methods Group has many good outreach activities to meet 

customer needs, including partnerships, Cooperative Research and Development 

Agreements (CRADAs), board service, Memorandums of Understanding (MOUs), 

industry coalitions, and international workshops. The group leader of the Synchrotron 

Methods Group was recognized with a Bronze Medal (a NIST award) for significantly 

advancing NEXAFS spectroscopy methods to quantify the interfacial molecular 

orientation of organic semiconductor materials that are being developed for flexible lowcost electronics. The group is at the state of the art in the development and application of 

synchrotron methods, has established a very mature capability that continues to produce 

significant accomplishments, and has clearly met its stated mission objectives. 

 The panel’s findings and recommendations with respect to the Synchrotron 

Methods Group are as follows: 

 Finding: The group is at the state-of-the-art level in the development and 

application of synchrotron methods. The group has established a very mature capability 

that clearly meets stated mission objectives through significant accomplishments. 

 Recommendation: The upcoming transition to the National Synchrotron Light 

Source-II project should be used to build and upgrade facilities and equipment. 

Finding: No patents were awarded during the past 2 years. 

Recommendation: Appropriate developments should be patented. 

 5

 M.P. Warusawithana, C. Cen, C.R. Sleasman, J. Woicik, Y. Li, J. Kluga, L.F. Kourkoutis, H. Li, 

L.P. Wang, M. Bedzyk, D.A. Muller, L.Q. Chen, J. Levy, D.G. Schlom, “A Ferroelectric Oxide Directly on 

Silicon,” Science 324:367, 2009. 
14 

Structure Determination Methods Group 

 The Structure Determination Methods Group consists of nine permanent technical 

staff members, one term employee/student, nine associates, and one administrative staff 

member, with a budget of $4.2 million. The stated mission of the group is to develop and 

disseminate measurement science, standards, and technology for the determination of the 

structure of advanced materials by improving: x-ray, electron, and neutron diffraction; 

and computational tools and providing SRMs and SRDs. The x-ray metrology and 

USAXS facilities have demonstrated outstanding performance. In particular, their newly 

commissioned divergent beam diffractometer achieves ±20 femtometers precision in 

lattice parameter measurements. This group is the premier source for crystallographic 

data for non-organic compounds; its SRDs are packaged with instruments marketed by 

several major vendors, and its SRMs comprise 4 to 5 percent of NIST’s total sales 

volume. 

 The group highlighted three projects: X-ray Metrology and Standards, 

Measurement and Prediction of Local Structure, and Crystallographic and Phase 

Equilibrium Data. The X-ray Metrology and Standards project develops SRMs and 

quantitative, reproducible measurement methods and protocols for powder diffraction, 

high-resolution diffraction, and x-ray reflectometry to enable the accurate and precise 

determination of material structure at the x-ray wavelength scale. Among other notable 

accomplishments, this project has achieved order-of-magnitude improvements in 

accuracy and precision in lattice parameter determination with its new divergent beam 

diffractometer. 

 The Measurement and Prediction of Local Structure project develops theoretical 

predictions and data-analysis methods for the quantitative determination of local atomic 

structure, based on inputs from multiple experimental techniques and first-principle 

calculations. The project lists several recent publications on a variety of materials 

systems, including the determination of the local structure origin of dielectric properties 

in AgNbO3-based ceramics, which received an Editor’s Choice award. 

 The Crystallographic and Phase Equilibrium Data project provides critically 

evaluated, comprehensive crystal-structure SRDs in formats that are readily incorporated 

into x-ray, neutron, and electron diffraction instrumentation. Its Inorganic Crystal 

Structure Database has been expanded to include calculated (non-experimental) atomic 

coordinate information, in addition to experimentally derived information. This project 

has achieved excellent results in determining, compiling, evaluating, and disseminating 

phase-equilibrium data, which are now published electronically and cover the literature. 

 This group is meeting the needs of its customer base, particularly in the 

production of SRDs and SRMs, which are in heavy demand. The development of 

software capable of combining multiple types of experimental data for the determination 

of local structure will be a valuable tool, particularly for the nanomaterials community. 

 With respect to the Structure Determination Methods Group, the panel makes the 

following recommendation: 

Recommendation: The Structure Determination Methods Group should continue 

to look for new, high-impact structure determination work and novel methods for the 

dissemination of information to build on its excellent current performance. 
15 

OVERALL FINDINGS AND RECOMMENDATION 

 Finding: There has been a strong leadership commitment to bringing in new staff 

to reinvigorate the Ceramics Division. 

 Finding: The Ceramics Division has a small amount of external funding relative 

to other divisions in MSEL. 

 Finding: The name “Ceramics” Division may no longer be appropriate as a 

description of the primary work being done by this division.

 Recommendation: Opportunities for bringing in additional funding should be 

explored. Other-agency funding can be used to expand staffing and capabilities and helps 

to sharpen people’s focus, as developing external funding is a very competitive process. 
16 

3 

Materials Reliability Division 

SUMMARY 

 The mission of the Materials Reliability Division is to develop and apply new 

measurement science to determine how, when, and why a material fails to perform as 

expected and to conduct research to help determine its operational limits during use. The 

division has seen slow but steady growth over the past 5 years, from 31 staff members in 

2005 to 43 in 2010, including 17 permanent technical staff, 6 NRC postdoctoral 

researchers, 1 term employee/student, 17.4 associates, and 2 administrative positions (see 

footnote 1). At the same time, the division’s budget has grown from approximately 

$5.25 million to $8.6 million, with $370,000 coming from other agencies. 

 Three groups—Structural Materials, Nanoscale Reliability, and Cell and Tissue 

Mechanics—conduct the activities of the Materials Reliability Division. The programs of 

the Structural Materials Group are concerned with test methods to ensure materials 

reliability for structural applications. The programs of the Nanoscale Reliability Group 

are concerned with developing measurement methods to assess changes in the behavior 

of materials when dimensions approach the nanoscale. Finally, the Cell and Tissue 

Mechanics Group is developing measurement techniques targeted at the reliability of the 

interface between biological systems and biomaterials. Each group is engaged in three to 

four major projects. 

 The review, which extended over a day and a half, consisted of an overview of 

each group and then a more detailed presentation of at least two programs of the group. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

 The programs reviewed are of high technical quality. The relatively recent efforts 

related to cell biology are exciting and attracting external collaborators, and the classic 

Charpy test specimen program continues to enjoy strong industrial support. 

ADEQUACY OF BUDGETS, FACILITIES, AND HUMAN RESOURCES 

 The Materials Reliability Division is located at NIST’s Boulder, Colorado, site. 

Although the division’s principal building is old and marginally functional, the 

laboratories within are well equipped. The High Pressure Hydrogen Test Facility, 

completed in January 2010, and the Precision Measurements Laboratory, scheduled for 

completion in 2011, will facilitate the expansion of both structural materials and biorelated activities as well as provide unique precision imaging capabilities that will benefit 

all of the division’s programs. Most of the laboratories will remain in the main building, 

which suffers from periodic flooding and poor-quality electrical power. 

 As its budget had grown, the division has added staff. These include impressive 

early-career staff and outstanding NRC postdoctoral associates (see Box 3.1). 
17 

BOX 3.1 

Outstanding New Staff Produce Results Fast 

 The panel observed several examples of new staff who have had a fast start. One 

of these provides an exceptional example of outstanding capability coupled to excellent 

support by the MSEL and NIST. This individual, in slightly less than a year after joining 

the Materials Reliability Division, applied her modeling capability to develop software 

for an integrated analysis of several x-ray analytical techniques. The work is scheduled 

for publication, and the software released for public use. 

 In addition, the same staff member was invited to serve on the program committee 

of an international meeting that she is hosting at NIST. She pointed out that her 

management and the NIST policies to facilitate hosting conferences were critical 

elements of her success. 

ACHIEVEMENT OF OBJECTIVES AND DESIRED IMPACT 

 During the past 2 years (2008 and 2009), the staff of the Materials Reliability 

Division were responsible for 39 publications in peer-reviewed journals, 11 articles in 

refereed proceedings, 6 contributions to books, and 2 NIST Recommended Practice 

Guides. This is an appropriate publication record for this division. A single patent 

application was filed. Six staff have been honored by NIST Bronze Medal awards (3 in 

2008 and 3 in 2009), and several Distinguished Associates Awards were presented each 

year. 

 The objectives of the division’s research projects are clearly defined, and the 

work reviewed is consistent with the project plans. 

TECHNICAL PROGRAM REVIEW 

Structural Materials Group 

 The Structural Materials Group has core competencies in macroscale mechanical 

testing and in developing standard testing procedures and reference materials that are 

important to the reliability of the nation’s infrastructure. The group has responsibility for 

four projects and is composed of six permanent technical staff, two NRC postdoctoral 

researchers, and 8.7 associates (see footnote 1), who exhibit a high level of competence 

and dedication to meeting critical infrastructure needs. Investments made since 2008 have 

enhanced the group’s testing and measurement resources, thereby maintaining 

capabilities that are among the best in the world, and in some cases, unique. The 

programs and project reviewed for this assessment are the Charpy Verification Program, 

the Pipeline Safety Program, and the Physical Infrastructure Project. 

 Since the previous review, numerous upgrades to the test capabilities of the 

Structural Materials Group have been made. High-bay tensile and fatigue in addition to 

Charpy testing capabilities have been upgraded with new hydraulic flow systems, load 

frames and controllers that expand the load range from 20 kN to 4.5 MN, increase 

temperature capabilities from -269°C to 1,000°C, and increase crack growth rates up to 
18 

5 m/s. For large-scale tensile testing, temperatures can be maintained from -60°C to 

250°C. Although not installed, a new 55 kip load frame has been purchased. The 

group’s testing capabilities were also enhanced by the recent commissioning of the 

world’s most advanced high-pressure hydrogen test facility, capable of operating at 

pressures approaching 140 MPa. 

Charpy Standard Reference Materials and Verification Program 

 The Charpy Standard Reference Materials (SRMs 2092, 2096, and 2098) continue 

to play a vital role in validating Charpy impact machines used to qualify steels employed 

in construction. Annually, the program evaluates specimens from testing on more than 

1,000 machines to ensure that national and international standards are maintained for 

high-impact energy tests and supplies more than 10,000 certified SRMs for verification 

of acceptance tests. The Charpy Verification Program has been a traditional pillar of the 

Materials Reliability Division, and it continues to serve vital national needs while 

remaining innovative in seeking ways to improve its capabilities. In response to the 

higher-strength steels being developed, an ultrahigh-load-capacity (700 J) Charpy test 

machine has recently been commissioned. To serve the program’s customers better, a 

laser scanning system is now used to document notch characteristics more precisely, 

increasing the sensitivity to detecting roughness at the notch. Better environmental 

control (temperature and humidity) has been achieved in the Charpy test laboratory with 

the installation of a dedicated heating, ventilating, and air-conditioning system. 

Pipeline Safety Program 

 The Pipeline Safety Program has developed unique capabilities for testing large 

pipeline sections that are more than 2 m long, while creating a uniform strain field over 

more than 1 m. Current testing of 2-m-long by 0.3-m-wide curved plates at up to 4.5 N 

and temperatures as low as -60°C is producing unique fracture resistance data. A highspeed camera system has been integrated into the Crack Tip Opening Angle test system 

for stop-frame imaging of cracks approaching actual pipeline rupture conditions. This 

work involves external collaborators, who are developing three-dimensional crackpropagation models in order to validate test methods and establish design criteria. 

Activities also include the development of a facility to test fracture behavior in pipelines 

that transfer corrosive biofuels and fuel blends. The extensive in-house testing conducted 

by the Pipeline Safety Program is meeting the needs of numerous industrial customers 

and partners. 

 With the completion of the hydrogen test facility, the Hydrogen Storage and 

Transport project is beginning work on standardizing methods for high-pressure testing, 

acquiring critical materials data, and establishing codes for material behavior and 

selection. 

Physical Infrastructure Project 

 The Physical Infrastructure Project is motivated by the growing cost of 

infrastructure rehabilitation. There is a pressing national need to assess aging 
19 

infrastructure for its reliability quickly and reliably. These assessments will benefit from 

new measurement tools and methods. This project is directed toward the development of 

measuring techniques that will reduce the error and uncertainty associated with the 

inspection of existing bridges. To this end, the project is qualifying new sensors, some of 

which may be embedded in a bridge’s structure. A necessary step in the development of 

these sensors has been taken with a new acoustic emission calibration block facility, 

which is used to calibrate new acoustic emission sensors. 

Findings and Recommendations 

 The panel’s finding and recommendation regarding the Structural Materials 

Group are as follows: 

 Finding: Overall, the personnel of the Structural Materials Group are productive 

and meeting important national needs. 

 Recommendation: Productivity and impact would be enhanced by the addition of 

two new staff members—one a materials scientist to delve more deeply into fundamental 

aspects of the test results, and the other a technician dedicated to large-scale testing 

activities in the high-bay facility. 

Nanoscale Reliability Group 

 The mission of the Nanoscale Reliability Group is to address physical 

mechanisms that dictate reliability when material and device dimensions are constrained 

in the nanoscale regime and to develop test methods, instrumentation, and models to 

measure material performance directly in complex device geometries and under in-use 

conditions in order to interpret size effects fully. The group has responsibility for three 

major projects. It is composed of seven permanent technical staff, two NRC postdoctoral 

researchers, and four NIST associates (see footnote 1). Postdoctoral research in the 

Nanoscale Reliability Group involves the innovative assessment of viscoelastic properties 

using contact resonance force microscopy and failure processes of carbon nanotubes 

under fatigue. The projects reviewed are these: Interconnect Reliability, Atomic Force 

Microscopy (AFM)-Based Nanomechanics, and Microsystems for Harsh Environments. 

Interconnect Reliability Project 

 The incorporation of a theorist is helping with the design of testing methods based 

on the modeling of electrical and thermal stress distributions. Cyclic thermal lifetime by 

resistance heating is a clever simulation of industrial significance to the semiconductor 

industry. Potentially, this could become an industry standard for the quality control of 

next-generation conduction pathways on a chip, as the test being developed does not 

require specialized test specimens. The electrical resistance fatigue instrument has been 

developed specifically for testing at the nanometer scale and could be available as a 

commercial interconnect screening technology. The instrument is beyond the state of the 

art and meets an important commercial need, as demonstrated by interest from Novellus 
20 

Systems, Inc., which is collaborating with NIST on utilizing this method to detect failures 

in copper interconnect lines. 

Atomic Force Microscopy-Based Nanomechanics Project 

 An effort using contact resonance measurements to make measurements on buried 

interfaces has both linear and nonlinear potential for measuring extremely small scale 

responses of importance to the architectural design of microelectromechanical systems 

(MEMS) and nanoelectromechanical systems (NEMS) devices, nanocomposites, 

microelectronic devices, and other thin films and nanostructures. 

 The development of the contact-resistance force microscopy (CR-FM) imaging 

technique under the Atomic Force Microscopy-Based Nanomechanics project is 

relatively mature, but the detection of buried interfaces was initiated as a new direction 

for this work in late 2009. CR-FM couples an acoustic AFM method with NISTdeveloped electronics for high-speed imaging, enabling measurements of the relative 

stiffness and moduli of buried interfaces—an advance in the state-of-the-art technology. 

The method and associated electronics for this project are finding a variety of 

applications, including the characterization of interphases, buried defects, nanostructures, 

polymer blends, and thin-film adhesion. 

 The Nanoscale Reliability Group is collaborating with other MSEL projects 

(Exploratory Research Grant, and Innovation in Measurement Science). A commercial 

AFM company has already invested in the electronics as a potential upgrade to its 

devices. 

Microsystems for Harsh Environments Project 

 As nuclear reactors are relicensed, test methods are needed to ensure their 

reliability near the end of their design lifetimes. Since the volume of potential test 

material exposed to these harsh environments for 40 years is dwindling, the need to better 

utilize the remaining test specimens is critical. NIST is evaluating the use of small-scale 

test structures to provide rapid testing of statistically relevant samples stored in harsh 

environments. If focused ion beam and micro-electro-discharge-machining techniques 

for the sectioning of specimens can be developed, a statistical database can be developed 

in a short time with minimal material. 

Findings and Recommendations 

 The panel’s findings and recommendations for the Nanoscale Reliability Group 

are as follows: 

 Finding: The Nanoscale Reliability Program is poised to launch several 

innovative and consequential techniques that would benefit both its basic and applied 

goals. Both science-based and commercial opportunities were quite apparent and to some 

degree have already formed. The research base exists but is subcritical in size to exercise 

its potential sufficiently. 
21 

 Recommendation: Greater collaboration should be pursued with universitybased modeling efforts in order to reach full potential. A particularly appropriate avenue 

for collaboration would be to involve a recognized authority on Green’s functions and 

thereby to coordinate efforts between the Nanoscale Reliability Group’s experimentalists 

and university-based multiscale-modeling efforts. 

 Finding: The recent hire for the Nanoscale Reliability Group addresses one of the 

findings by the NRC panel that reviewed the laboratory in 2008: that finding stated that 

new hires were essential. 

 Recommendation: The incremental productivity increase provided through 

another hire or two to this group should catalyze substantial program growth. Emphasis 

should be given to proposal writing. Successful proposals would be beneficial in 

improving the program. 

Cell and Tissue Mechanics Group 

 The Cell and Tissue Mechanics Group is composed of three permanent technical 

staff, two postdoctoral researchers, and 4.7 associates (see footnote 1). The group’s 

mission is the development of measurement techniques to assess the reliability of 

biomaterials. Here reliability is seen to occur at the interface between biological systems 

and synthetic (bio) materials where the interaction between the biological system and the 

biomaterial can cause failure of one or both. Hence, developing measurement 

techniques to determine properties at the interface between tissues and biomaterials is a 

key component of this group’s focus. 

 The group has responsibility for four projects: Medical Device Reliability, 

Instrumented Bioreactor, Cell Platforms for Quantifying Nano/Bio Interactions, and 

Resonating Platforms for Nanomaterial Analysis. This fourth project also includes 

efforts to characterize carbon nanotubes in collaboration with researchers in MSEL and 

the Physics Laboratory. The projects reviewed are these: Medical Device Reliability, 

Instrumented Bioreactors, Cell Platforms for Quantifying Nano/Bio Interactions, and 

Resonating Platforms for Nanomaterial Analysis. 

Instrumented Bioreactor Project 

 The Instrumented Bioreactor project is aimed at improving the mechanical 

durability for cartilage replacement and other load-bearing applications. Thus for 

optimizing hydrogel-based engineered tissues, the project has developed ultrasonic 

sensors to be incorporated for monitoring extracellular matrix content, and 

electrochemical sensors have been developed to measure metabolic activity. This 

technology is being used to advance hydrogel-based cartilage replacement. 

 This project involves novel instrumentation for measurements important to 

industrial biochemistry. 
22 

Cell Platforms for Quantifying Nano/Bio Interactions, and Resonating Platforms for 

Nanomaterial Analysis 

 The Cell Platforms for Quantifying Nano/Bio Interactions and the Resonating 

Platforms for Nanomaterial Analysis projects of the Cell and Tissue Mechanics Group 

are intended to create methods useful in the evaluation of biocompatibility and toxicity of 

nanoparticles. The increasing use of nanomaterials and their potential proliferation in the 

environment motivate these projects. The environmental, health, and safety effects that 

arise from the unique dimensional characteristics (e.g., size, shape, aspect ratio) and 

properties (e.g., composition, surface chemistry, charge, reactivity) of these materials are 

not well understood, in part because of a lack of standardized methods for evaluating 

their toxicological consequences. 

 These projects are outgrowths from prior work on three-dimensional tissue 

scaffolds, which is now being developed as a testbed to evaluate nanotoxicity in a threedimensional tissue engineering hydrogel scaffold in the presence of neural cells. This 

scaffold provides an environment in which cell response to nanoparticles can be 

measured for weeks, without the expense associated with in vivo assays or the short-term 

limitations of biochemical assays. A systematic approach is focused on evaluating the 

nanoparticle distribution and concentration within the hydrogel, which will then form a 

framework for the evaluation of the dose effects and potential for changes in evaluating 

the long-term stability of the nanomaterials. 

Resonating Platforms for Nanomaterial Analysis 

 A new technique using resonating platforms for nanomaterial analysis has been 

developed to evaluate properties of a few carbon nanotubes. This technique, developed 

in-house, appears to be a very good addition to their capabilities. Once the carbon 

nanotubes can be characterized and sorted according to critical dimensions, their 

interaction/reaction can be rapidly screened using a new instrument based on the quartz 

crystal microbalance. 

 To be able to develop certified reference materials, a separate project at the 

Gaithersburg, Maryland, facility is developing methods to produce well-characterized 

carbon nanotube suspensions. The careful control of parameters (length, type, charge, 

concentration, and impurities) will rely on the development of techniques to characterize 

these properties using small amounts of suspensions. Methods are being evaluated to 

ensure consistency among the carbon nanotubes used in the toxicity screening. 

Finding and Recommendation 

 The panel’s finding and recommendation for the Cell and Tissue Mechanics 

Group are as follows: 

 Finding: The Cell and Tissue Mechanics Group is young but poised to respond to 

an important and growing national need. 

 The equipment seems adequate for the project, although cramped in the current 

space. It is noted that the group has allocated a larger laboratory and will be relocating 
23 

shortly. Laboratory access on upper floors is a concern as there is currently no elevator to 

transport supplies, including cryogenic fluids and gases. 

 Recommendation: The design and installation of an elevator to service the 

group’s laboratory should be expedited. 

CONCLUSIONS 

 In general, the Materials Reliability Division is in excellent shape and has 

addressed the issues identified by the 2008 NRC review panel. The projects reviewed in 

the present assessment are focused on the mission of the MSEL and build effectively on 

the historic strength of the division in mechanical testing for reliability. The research 

distribution among the three division groups is close to ideal. There is an excellent mix 

of established (Structural Materials Group), maturing (Nanoscale Reliability Group), and 

nascent (Cell and Tissue Mechanics Group) research projects, which is indicative of the 

attempt to anticipate national needs. Such a mix also helps to ensure division vitality 

well into the future. 

 The division has developed several noteworthy measurement tools and devices 

that have the potential to enhance greatly the competitive position of different segments 

of the U.S. industry. However, as indicated in the panel’s findings and recommendations, 

there are areas that could use improvement. 

 Finding: The Materials Reliability Division’s staff member publication rate is 

low. A division of this size should target 35 to 50 publications per year in reputable 

journals. 

 Recommendation: Publications should be encouraged not simply for the sake of 

numbers, but because the work merits publication. A higher publication rate has the 

added advantage of lowering the barrier to proposal submission—an absolute necessity if 

the division is to grow. 

 Finding: Several technologies appear to be eligible for patent protection and 

licensing. The level of interest and awareness of patenting within the division was 

relatively low. 

 Recommendation: A strong and consistent policy regarding intellectual property 

should be developed. 

 Finding: Extensive collaborations of division staff on the Boulder, Colorado, 

campus with MSEL in Gaithersburg, Maryland, were not apparent. 

 Recommendation: To the extent that the panel’s perception of the level of 

collaboration between the MSEL components in Boulder and Gaithersburg is accurate, 

steps should be taken to leverage the expertise of the NIST laboratories as a whole. 
24 

 Finding: Several of the staff members and division leadership expressed the need 

for outreach to other national laboratories or universities to partner joint proposals. This 

observation underlined the self-recognized weaknesses in generating peer-reviewed 

publications. In this respect the strengths of the Nanoscale Reliability Program are 

highlighted. 

 Recommendation: Sufficient resources should be added to facilitate this 

outreach. The resources could be in the form of additional staff or technical support 

personnel who would free up time for the necessary outreach. Attracting more 

postdoctoral associates might also facilitate outreach. Either way, this effort could pay 

dividends in terms of publications (recognition) and greater success at generating soft 

funding (proposal success). 

 Finding: Failing of the infrastructure and physical plant is leading to frustration 

and lower productivity. Flooding, in particular, has repeatedly led to experimental 

downtime. However, the construction underway to improve the nanofabrication facility is 

a very positive event. This facility will house various Raman, atomic force microscopy, 

and transmission electron microscopy improvements in instrumental capabilities. 

 Recommendation: Laboratory access (the elevator noted in the earlier 

recommendation for the Cell and Tissue Mechanics Group) and necessary maintenance, 

including the refurbishing of the older physical plant, need be provided as soon as 

possible. 

 Finding: NRC postdoctoral associates were knowledgeable and excited about 

their projects, with unique proposal ideas that continue to evolve. However, there were 

inconsistencies in the mentoring of the postdoctoral associates. In addition, there was a 

general desire among these postdoctoral associates for a more stimulating and scholarly 

environment of the type that most experienced during their postgraduate education. 

 Recommendation: The division, and perhaps the entire Boulder facility, should 

undertake a review of the postdoctoral experience and support efforts to build a 

postdoctoral community, establish mentoring guidelines, and establish programs to 

“market” NIST postdoctoral associates to the broader scientific community. (See Box 

3.2 below.) 
25 

BOX 3.2 

Well-Mentored Postdoctoral Appointee Quickly Produces Science and Proposals 

 Opportunities for research and skill development for capable, ambitious 

postdoctoral appointees who are mentored effectively are illustrated by the experience of 

one of the postdoctoral appointees whom the Panel on Materials Science and Engineering 

interviewed. She is engaged in ongoing research and, in addition, has co-authored two 

external research proposals that build on the unique NIST technology. One proposal is 

with a faculty member of Colorado State University, the other with her former adviser at 

the University of Texas. The proposals had not been funded at the time of the review. 

However, merely writing them is a beneficial experience for the appointee, and the 

collaborations support the mission of NIST to disseminate its technology. 

 
26 

4 

Metallurgy Division

SUMMARY 

 The mission of the Metallurgy Division is to promote U.S. innovation and 

industrial competitiveness in the development and use of materials by advancing 

measurement science, standards, and technology of metals-based systems, in ways that 

enhance economic security and improve our quality of life. The division is organized 

into four groups: Thin Film and Nanostructure Processing, Magnetic Materials, Materials 

Performance, and Thermodynamics and Kinetics. 

 As of the end of FY 2009 (September 2009), the division technical staff included 

31 permanent technical staff (includes 2 NIST fellows), 6 NRC postdoctoral associates, 

and 4 term employees/students. In addition, there were 5 administrative support staff and 

44.4 associates. The associates category includes contractors, foreign guest researchers, 

and guest workers from universities and industry (see footnote 1). The total budget for 

the division in FY 2009 was $13.5 million, with $630,000 coming from other agencies.

 There are 17 active projects in this division. The panel reviewed 9 projects in 

detail through presentations by research staff and 8 more projects generally, through 

overviews by the group leaders. All of the projects appeared to be very thoughtful, well 

executed, and targeted to further the MSEL and NIST missions. 

 This is a division with high morale and enthusiasm for the work, supported by 

effective technical leadership. The division’s technical capability is outstanding. The 

division is well equipped and has good facilities as a result of recent capital investments 

using ARRA and internal NIST funding. The division consistently develops clever, 

unique measurement science through equipment design and modeling. 

 The division has strong cross-division, cross-MSEL, and external collaborations. 

The technical staff is internally and externally recognized for its capabilities and excellent 

output. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

 The quality of research in the Metallurgy Division is comparable to the best in 

this field worldwide. This is evidenced through the number of citations for its 

publications, the recognition of its staff, and requests for involvement by outside 

organizations such as the Defense Advanced Research Projects Agency (DARPA; see 

details in the group reports below). 

 In the period since March 2008, the division has published 123 archival journal 

articles, 22 conference proceedings, and 10 book chapters. In addition to numerous 

contributed presentations, division staff gave a total of 132 invited talks at conferences, 

universities, other agencies, and industrial sites. In 2008-2009, eight invention 

disclosures were filed, and one patent was awarded. 
27 

 The staff have received numerous awards for technical excellence and recognition 

of leadership over the past 2 years. Three members were elected fellows of the 

Electrochemical Society, one a fellow of ASTM International (formerly known as the 

American Society for Testing and Materials), and one a fellow of the American 

Association for the Advancement of Science. Staff also won Department of Commerce 

Silver and Bronze Awards, and one recent division retiree was selected for the very 

prestigious NIST Portrait Gallery. There were two Best Paper awards and the SPIE 

Nanoengineering Pioneer Award. Finally, one staff member was made an honorary 

member of the Indian Institute of Metals—an honor limited to 60 members worldwide at 

any given time—and elected president of the International Organization of Materials, 

Metals, and Minerals Societies. 

ADEQUACY OF BUDGETS, FACILITIES, AND HUMAN RESOURCES 

 Staffing in the Metallurgy Division has been quite stable over the past several 

years, with some retirements or other departures from the division and a few hires in 

high-priority areas. This stability has been enabled by a significant (approximately 24 

percent) increase in overall funding over the past 5 years, which kept pace with rising 

costs. 

 Over the past 2 years, the division has made significant investments in capital 

equipment that have brought it to standards that are among the best in the world. (See 

details in the group reports below.) The past 2 years have seen substantial increases in 

investment in capital equipment. In FY 2008, the division invested heavily in a 

$2.5 million state-of-the-art transmission electron microscope (TEM), with unique 

features allowing three-dimensional compositional imaging at the nanoscale; Lorentz 

microscopy; and electron holography. In FY 2009, the division used $2 million in ARRA 

funds, plus another $0.5 million in laboratory funds, to augment the mechanical test 

facility, providing unique capabilities to the division in high-strain-rate metrology and 

measurements targeting the automotive and other industries reliant on metal forming. 

Other strong facilities in the division include nanomaterials fabrication (semiconductor 

nanowires, magnetic and other thin films, and electrodeposition), a superb magnetic 

characterization facility, and the Hardness Laboratory, among others. 

 Data on division budgets for the individual projects reviewed within each group 

are given below. In all cases, there are substantial collaborations with other divisions (or 

operating units) at NIST; thus the entire NIST effort may be significantly larger. 

 The division leads in the development and application of computational materials 

science at NIST and the use of the World Wide Web for information dissemination and 

collaboration. 

ACHIEVEMENT OF OBJECTIVES AND DESIRED IMPACT 

 The Metallurgy Division is a very high quality research organization in 

measurement science. It has several unique equipment capabilities and a technical staff 

that is among the best in the world and that is fully aligned with NIST’s mission. Major 

contributions are being made to issues involving national security and competitiveness in 

the automotive, magnetics, and aerospace industries. 
28 

TECHNICAL PROGRAM REVIEW 

Thin Film and Nanostructure Processing Group 

 The mission of the Thin Film and Nanostructure Processing Group is to develop 

metrology needed for processing and characterization of materials at dimensions where 

internal and external interfaces substantially impact their properties. 

 At the end of FY 2009, this group included 10 permanent technical staff, 2 NRC 

postdoctoral researchers, and 2 administrative support staff. Fourteen associates provided 

significant contributions to the research program. The group budget was approximately 

$3.8 million. 

Special Facilities and Capabilities 

 Specialized capabilities and facilities of the group include the following: 

 A suite of semiconductor nanowire test structures, fabrication, and 

measurement capabilities (including structural, compositional, electrical, 

 and optical) for electronic, photonic, and sensor applications; 

 A suite of measurement capabilities for the high-throughput and highaccuracy evaluation of the capacity, charging/discharging kinetics, and 

structural characteristics of hydrogen storage materials. These methods, 

developed in Metallurgy, are calibrated with prompt gamma activation 

analysis (the only direct measurement of hydrogen content) at the reactor; 

 A wafer-curvature system enabling in situ measurement of stress evolution 

associated with adsorption of additives and growth and reaction of thin films 

in electrolytes with sub-monolayer resolution during electrochemical 

processing; 

 Scanning tunneling microscope (STM) imaging of the surfactant phases 

responsible for superconformal film growth with measurements performed at 

additive concentrations and potentials directly relevant to industrial copper 

metallization processes used in the microelectronics industry; and 

 Multispectral, integrated instrumentation to measure and characterize 

structure, composition, and properties bridging the microscopic down to the 

atomic length scales (microscopy). 

Technical Program Review, Findings, and Recommendations 

 There is strong evidence of focus and excitement in the Thin Film and 

Nanostructure Processing Group, encouraged through very dynamic technical leadership. 

Regarding the impact being made in the country and indeed worldwide, there is ample 

evidence through the number of the publications and some hints through one measure of 

their citation history that they may be having impact. Numbers of publications of the 

senior members, as found in the ISI Web of Knowledge, were largely between 50 and 

100 authored or coauthored papers in quality peer-reviewed journals (though the time 

frame for these accumulations was not analyzed). One measure of impact is the 
29 

h-index—the number of papers that have been cited at least that many times. This 

criterion for the senior staff was comparable to what is typically found in top-ranked 

universities—about 20 to 30. A few of the papers were cited several hundred times, 

suggesting possibly broad utilization by other researchers. This indicator should be 

considered alongside other metrics to help determine its validity. 

 This group has activities in the following areas: 

 Electrochemical processes; 

 Mechanics and thermodynamics of nanoscale systems; 

 Electrical, optical, and sensing properties of nanowires and nanowire devices; 

and 

 Electron microscopy and crystallography. 

 

 While interesting and important work is being done in all of these areas, two 

relatively new projects, begun since the previous MSEL review, are described here. 

Characterization of 3D Photovoltaics Project 

 The Characterization of 3D Photovoltaics project is a new program with an 

expected duration of 5 years and a budget of about $1.2 million per year. The goal is to 

develop measurements and platforms for evaluating the impact of three-dimensional 

nanoscale patterning in third-generation photovoltaic materials and devices. 

 All capabilities in fabrication, measurement, and modeling are new. Key facilities 

include three-dimensional device fabrication capabilities with lithographic patterning and 

electrodeposition, solgel, sputtering, and other deposition techniques. Also available are 

microstructural characterization capabilities including x-ray diffraction, scanning electron 

microscope (SEM) and TEM imaging of materials microstructures and device 

geometries, as well as standard optical properties characterization tools. 

Some of the accomplishments from this new project include the establishment of 

microscale electrode patterning capability and the development of the required materials 

processing capabilities. Good progress has been made in the development of modeling 

programs for drift-diffusion models for three-dimensional geometries using the FiPy 

program (an object-oriented, partial differential equation solver, written in Python) 

developed in the group. A major accomplishment is the fabrication of cadmium telluride 

(CdTe) homojunction and CdTe-based heterojunction devices together with the modeling 

of these devices. 

Hydrogen Storage Project 

 The objective of the 6-year, $6.1 million Hydrogen Storage project is to develop 

the metrologies necessary for the rapid, high-throughput measurement of the hydrogen 

content of novel materials proposed for hydrogen storage and for electrodes in nickelmetal hydride (Ni-MH) batteries. 

 The facilities for this work include state-of-the-art thin-film fabrication and 

infrared, Raman, and pressure-composition-termperature measurement capabilities; and 

measurement capabilities for the evaluation of the thermodynamics, kinetics, and 
30 

structural characteristics of hydrogen storage materials. These methods, developed in the 

Metallurgy Division, are calibrated with gamma activation analysis at the reactor. 

Combining spectroscopic and hydrogen content measurements provides insight into the 

mechanisms of hydrogenation processes. To date, the project has developed a new 

method to measure the kinetics of hydride growth, which utilizes infrared imaging and 

wedge-shaped configuration of films. Also, it has produced an energy-dispersive x-ray 

spectroscopy/scanning electron microscope (EDS/SEM), TEM phase diagram study of 

multiphase, multicomponent alloys for a new generation of negative electrodes for 

Ni-MH batteries. 

Findings and Recommendations 

 The panel’s findings and recommendations for the Thin Film and Nanostructure 

Processing Group are as follows: 

Finding: The Characterization of 3D Photovoltaics project to support nextgeneration photovolatics is off to a good start with capable management and research 

personnel. 

Finding: The Hydrogen Storage project is well organized, led by very capable 

professionals, and shows excellent promise for major success in the future. 

Recommendations: For both projects—the Characterization of 3D Photovoltaics 

project and the Hydrogen Storage project—no changes are recommended. They should 

continue along the same trajectory. 

Magnetic Materials Group 

 The mission of the Magnetic Materials Group is to develop magnetic 

measurement science, standards, and technology needed by U.S. industry to apply 

materials and components in the magnetic applications of magnetic storage, magnetic 

sensors, transformer and automotive magnets, and health applications. 

 At the end of FY 2009, this group included 5 permanent technical staff, 2 NRC 

postdoctoral researchers, and 10.9 associates (see footnote 1). The budget was 

approximately $2.2 million. 

Special Facilities and Capabilities 

 The Magnetic Engineering Research Facility has the most diagnostic tools 

attached to the thin-film deposition system of any in the world, which allows the in situ 

determination of what is happening during the growth of the films. Such measurement 

enables the manufacture of high-quality layered structures (including tunnel junctions) 

and the understanding of how their structure, chemistry, and morphology changes. 

 The Magneto-optic Indicator Film equipment is unique, being capable of imaging 

magnetic domains in a ferromagnet (FM) in real time, while in the middle of an 

electromagnet. Most methods of domain imaging do not allow real-time measurement. 
31 

It is useful even when the material of interest does not have a large magneto-optic Kerr 

effect (the only other method available for real-time observations). This tool has enabled 

the group to be the first to prove the predictions that a soft FM is forced to reverse by 

rotating its spins when next to a hard FM (the so-called exchange-spring FM, which is the 

basis for the Magnetic Materials Group’s DARPA project) and also to be the first to show 

that in a bi-layer couple of an antiferromagnet and a ferromagnet, the magnetization 

reversal of the FM does not occur by the same process when reversing back to its original 

configuration. This latter effect was quite a revelation, which has changed the thinking of 

people in magnetics community. 

 A special TEM holder to enable electrical transport measurements while also 

enabling electron microscopy allows the measurement of electrical characteristics of the 

exact spot being imaged. Most electron microscopes cannot do this. 

Technical Program Review, Findings, and Recommendations 

 Two projects were selected for review. Their descriptions follow. 

Magnetic Nanoparticle Metrology 

 The 4-year, $2.2 million Magnetic Nanoparticle Metrology project is showing that 

nanoparticles need to be interacting with each other in order to heat effectively for 

hyperthermia treatments, and recent work has shown that magnetic torque measurements 

can provide the information that small angle neutron scattering (SANS) measurements do 

in distinguishing between different suspensions of magnetic nanoparticles. 

 Biomedical applications of magnetic nanoparticles are expanding rapidly, with 

developments in academia and industry. The physical origin of these applications is not 

understood, and assumptions about them are often wrong (e.g., interparticle interactions). 

 Measurement methods to characterize the basic properties of magnetic 

nanoparticle systems are still developing, as the conventional methods are often either 

wrong or incorrectly applied (e.g., blocking temperature). 

 There is significant interest in this work from industry, academia, and government 

(Food and Drug Administration, National Institutes of Health, and others). 

Magnetic Tunnel Junctions for New Computer Memories 

 This 4-year, $4 million Magnetic Tunnel Junctions for New Computer Memories 

project investigates metrology for the technology that may replace complementary metaloxide-semiconductor (CMOS) technology after it can no longer maintain Moore’s law. 

Magnetic memory elements can be much smaller than CMOS, and they require 90 

percent less power and heat. IBM and Intel, among other companies, have active 

programs in Spin Torque Transfer Magnetoresistive Random Access Memory (STTMRAM). 

 DARPA is funding this group to perform and interpret critical measurements. 
32 

Finding and Recommendations 

 The panel’s finding and recommendations for the Magnetic Materials Group are 

as follows: 

Finding: The Magnetic Materials Group has established world leadership in 

magnetic tunnel junction fabrication and characterization and is conducting forefront 

work on medical uses of magnetic nanoparticles. 

Recommendation: Planning should be started now for leadership change in the 

Magnetic Tunnel Junctions for New Computer Memories project, as retirements are 

anticipated. 

Recommendation: Consideration should be given to leveraging current 

competitive advantage by seeking additional external funds for the Magnetic Materials 

Group. 

Materials Performance Group 

 The mission of the Materials Performance Group is the mechanical 

characterization at length scales from nanometers to tens of meters. At the end of FY 

2009, this group was made up of 10 permanent technical staff, 1 NRC postdoctoral 

researcher, and 1 term employee/student; and 6.2 associates (see footnote 1) provided 

significant contributions to the research program. The group budget was approximately 

$4.1 million. 

Special Facilities and Capabilities 

 Special facilities of the Materials Performance Group include the following: 

 The pulse-heated compression Kolsky bar (existing) and high-strain-rate, 

high-heating-rate conventional tensile Kolsky bar (purchased with ARRA 

funds, with delivery in early 2011) provide a well-equipped high-strain-rate 

test facility. 

 A Marciniak forming machine with full-field strain and x-ray stress 

measurement for sheet metal forming. 

Technical Program Review, Findings, and Recommendations 

 The following subsections describe four activities selected for review. 

NIST Hardness Program 

 The expected duration of the NIST Hardness Program is FY 2011–FY 2020, and 

the budget is approximately $400,000 per year. 
33 

 The objectives of this 9-year, $3.6 million program are to standardize and 

improve hardness measurement both domestically and abroad. This group continues to 

function in the forefront of hardness testing and measurement. It serves as the U.S. 

National Metrology Institute (NMI) for hardness, and as such is responsible for 

traceability in hardness measurements. This entity continues to produce SRMs, to revise 

calibration and test methods, and to serve as a technical point of contact for hardness testrelated issues. Major accomplishments over the past 10 years have included a revision of 

the Rockwell C hardness scale in the United States to match international scales, and the 

development of a hardness standardizing laboratory. This group continues to do 

excellent work, even with reduced staffing. The staff member leading this project 

became a fellow of ASTM International. 

 In the future, this group will lead revisions of International Organization for 

Standardization (ISO) standards on Rockwell hardness testing and ASTM standards for 

portable testers, and rapid indentation testing. It will also contribute to revising Rockwell 

and Brinell hardness test methods and, at the request of Instron, to updating calibration 

methods in accordance with test method standards (develop calibration laboratory 

accreditation). The objective of the nanoindentation study is to develop standard test 

methods and materials. 

Fundamentals of Deformation Project 

 The new Innovation in Measurement Science award (through the NIST Director’s 

Innovation in Measurement Science Program) with the Ceramics Division to develop 

nanoindentation standards is timely and desperately needed in the science and 

engineering community. Under the umbrella of the Fundamentals of Deformation 

project, efforts were undertaken to quantify the stress fields beneath nanoindents at the 

Advanced Photon Source. These efforts ultimately led to the development of an x-ray 

measurement technique capable of probing the stresses inside individual dislocation cells. 

Mechanical Performance Under Extreme Conditions Project 

 The objectives of this 9-year, $6 million project are to provide property data, 

metrology, and standard test methods for materials systems under extreme conditions for 

areas critical to manufacturing, homeland security, and energy infrastructure within the 

United States. The goals of the presented project are to develop new high-strain-rate 

measurement techniques and to provide more accurate and robust data for modeling 

material behavior under extreme conditions (e.g., manufacturing, transportation safety, 

law enforcement, fire, etc.). 

 Research to develop National Institute of Justice (NIJ) standards for lead-jacketed 

bullets continued in FY 2009. This work was not presented in the project overview but is 

slated for presentation at two conferences in FY 2010. One project detailed during the 

division review team’s visit was a collaborative effort with the Naval Research 

Laboratory (NRL). The NRL goals called for the development of a biomimetic gel 

capable of simulating the human body under compressive loading caused by nearby blast 

waves. In support of this project, NIST researchers conducted a series of high-strain-rate 

tests to assess the viability of the material selected by the NRL. The distinctive physical 
34 

characteristics of the biomimetic gels required the development of unique hardware and 

new three-dimensional digital image correlation techniques to allow good results to be 

collected and ultimately assessed by means of standard finite-element methods. Results 

collected by this group ultimately led to the conclusion that the material initially selected 

by the NRL did not accurately mimic the response of real tissues and was unsuitable for 

its purposes, prompting the NRL to consider a different material. 

 Plans are in place to develop and acquire new capabilities to meet the needs of 

some of NIST’s core constituents (i.e., NIJ, NRL, the automotive industry). Currently, a 

new pulse-heated tension Kolsky bar is under development for high-strain-rate ductility 

and fracture studies. This effort was motivated directly by the U.S. automotive sector to 

evaluate the crashworthiness of prospective light alloys (e.g., magnesium alloys, 

transformation-induced plasticity [TRIP] steels, etc.). An important feature of this 

instrument is that it will allow data to be collected on sheet specimens. The current 

Kolsky bar setup is limited to compressive loading, which precludes the investigation of 

thin sheet material. The development of this instrumentation, which was made possible 

through MSEL funds, will be of immediate value to all end users of sheet materials. An 

intermediate-strain-rate servo-hydraulic test frame has been purchased using ARRA 

funds to allow for testing at intermediate strain rates. This acquisition will allow NIST 

scientists and engineers to collect high-quality data over all strain rates from quasi-static 

to very high Kolsky bar rates. 

 This research group has continued to develop data that could not be generated 

elsewhere. As noted above, the level of technical merit is very high for this project. The 

test methods developed will be of significant importance to any sector, scientific or 

industrial, in which an understanding of high-strain-rate properties is needed. Thus the 

broader impacts of this work are great. This program is funded adequately in terms of 

infrastructure. 

Center for Metal Forming 

 The expected duration of the Center for Metal Forming project is FY 1999–FY 

2016, with a budget of approximately $850,000 per year. 

 The objectives of this $12.7 million project are to develop measurement 

methodology, standards, and analysis necessary for the U.S. auto industry and base-metal 

suppliers to transition from a strain-based to stress-based design system for auto-body 

components, and to successfully transfer this technology to NIST customers in industry. 

 This group has done an outstanding job in partnering with industries and 

universities to develop new measurements and data to assist the U.S. automotive industry 

and suppliers in developing and implementing advanced and lightweight materials. 

These data will ultimately lead to improved die designs, which will reduce die tryouts 

and new-model development costs. The center has initiated these efforts through its own 

diligent efforts, resulting in the formation of a strong, vital center with representation 

from industry, standards agencies, and universities. 

 One exciting product of this effort is the development of a Marciniak geometry 

forming station with full-field strain and x-ray stress measurement during sheet-metal 

forming. This instrumentation, which is the only instrumentation of its kind, allowed 

NIST researchers to map the evolution of the tensile yield surface in advanced aluminum 
35 

and steel. This instrumentation was noted by the panel that reviewed the laboratory in 

2008. Since that time, the experimental techniques have been refined, and the 

experimental results have been complemented with crystal plasticity modeling using 

crystallographic textures, in association with researchers in the Department of Materials 

Science and Engineering at Carnegie Mellon University. 

 An additional exciting observation was the first prediction of transformation 

potentials in TRIP steels, which showed that initial crystallographic textures play a 

significant role in the TRIP effect. This work, which was not highlighted in the 

presentation to the division review team but was discussed in some detail during the 

facility tour, represents a major advancement that will help propel TRIP steels into more 

widespread application areas. The work is truly crosscutting and has the potential to 

positively impact many technical areas beyond the automotive sector. 

 Over the next 2 years, further extensions of this program are planned, including 

the development of a new crystal plasticity based constitutive law incorporating complex 

slip (with Carnegie Mellon University). Capital equipment acquisitions will include the 

development of an advanced multiaxial forming machine with x-ray in situ stress 

measurement and differential interference contrast strain measurement capabilities. This 

instrumentation, which was made possible through ARRA funds, will allow studies to be 

conducted on specimens with industrially relevant sizes. 

 The Metallurgy Division is also noteworthy in that it has committed $600,000 in 

MSEL base funds to establish a new research project on Physical Infrastructure. 

Personnel committed to this project include 1 full-time permanent staff member, 2 parttime permanent staff members, and 1 guest researcher (2.5 full-time equivalent, FTE). 

This project will address experimentally and computationally critical issues related to the 

nation’s deteriorating highway infrastructure. Initial efforts, in collaboration with the 

Federal Highway Administration (FHWA), include the determination of limit states for 

steel gusset plates and to examine the performance of such components under extreme 

conditions (e.g., fire, corrosion, etc.). These studies have shown the FHWA safety 

guidelines to be appropriate for gusset plates and have suggested safety factors for steel 

gusset plates. 

Findings and Recommendations 

 The panel’s findings and recommendations for the Materials Performance Group 

are as follows: 

Finding: In its work on steel and aluminum sheet, the Materials Performance 

Group has developed many, if not all, of the necessary components to provide Integrated 

Computational Materials Engineering capabilities for these systems. Such capabilities 

would be of significant interest to the automotive industry. The models developed for 

sheet forming also include predictions of postformed texture. The group envisions 

extending its expertise in sheet-metal forming to understanding the performance of sheet 

metal at high rate, appropriate to crashworthiness. 

Recommendation: These models for sheet forming should be linked with 

thermodynamic/kinetic-based microstructural evolution models developed by the 
36 

Metallurgy Division’s Thermodynamics and Kinetics Group into models that can 

holistically integrate manufacturing effects (e.g., stamping) on microstructure and 

properties (e.g., high-strain-rate properties) and ultimately performance (e.g., crash). 

Finding: The NIST Hardness Program continues to serve as the National 

Metrology Institute for hardness in the United States. Through the Innovation in 

Measurement Science Program, a new initiative was begun to develop nanoindentation 

standards. 

Recommendation: The NIST Hardness Program should continue, with 

appropriate resources to allow for an expansion of the nanoindentation effort. 

Finding: The Mechanical Performance Under Extreme Conditions research group 

has continued to develop high-strain-rate data that could not be generated elsewhere. The 

test methods developed and the data are of significant importance to any scientific or 

industrial sector in which an understanding of high-strain-rate properties is needed. 

Finding: The Mechanical Performance Group has additional opportunities in two 

key areas: (1) the development of Web-based knowledge information dissemination 

mechanisms for its high-quality data and models, and (2) the combining of its models and 

data into ICME tools for steels and aluminum. 

Recommendation: Both of these efforts would be significantly aided by 

increased collaboration with the Thermodynamics and Kinetics Group. 

Recommendation: Additional staffing should be allocated to the mechanical 

performance project, including technician support to maintain the complex equipment 

being developed. 

Finding: The Center for Metal Forming has evolved well over the past 24 months 

to address the needs of its core constituents better. Its decision to focus on physical 

infrastructure is timely and forward-thinking. 

Recommendation: The support for the Center for Metal Forming should be 

continued, and additional funding should be provided for the expansion of the Physical 

Infrastructure Program. It produces high-quality data using complex forming apparatus 

and high-strain-rate testing devices. These data should be provided in a digital form to 

the external community by means of an improved and modern Web site. The design of 

the Web site should be forward-looking, with the perspective of ultimately being able to 

be used by others to download externally produced data and to provide it to the wider 

materials community for assessment and use. This recommendation is consistent with 

the recent National Materials Advisory Board report on Integrated Computational 

Materials Engineering.6

 6 National Research Council, Integrated Computational Materials Engineering: A 

Transformational Discipline for Improved Competitiveness and National Security. Washington, D.C.: The 

National Academies Press, 2008, pp. 31-32, 125. 
37 

Thermodynamics and Kinetics Group 

 The mission of the Thermodynamics and Kinetics Group is the development of 

fundamental-based, quantitative models of microstructural changes in materials, new 

measurement paradigms for complex materials systems, and the dissemination of 

methods, tools, data, and models. 

 At the end of FY 2009, this group included 4 permanent technical staff, 1 NRC 

postdoctoral researcher, 3 term employees/students, 12.5 associates (see footnote 1), and 

1 administrative support staff member. The group budget was approximately $2.9 

million. This group has a well-developed portfolio that is appropriate to its size and 

budget. 

 This group makes use of and leads the Theoretical and Computational Materials 

Science facility, which has experienced a major growth in computational capability in the 

past 2 years. This facility is an MSEL-wide facility and, given the importance of 

modeling and simulation for materials, this is an important and encouraging 

development. This group has also demonstrated an ability to optimize its resources by 

proactively stopping a project (reactive wetting in complex systems) to enable starting a 

new project (nanosilver in vivo). The reactive wetting project had reached a logical 

conclusion and developed models, which are available to industry and other researchers 

to be used to solve more focused problems. 

 In addition to the detailed project reviews of two projects (see below), the panel 

was provided an overview of the entire group portfolio, which includes projects on 

reactive wetting of complex systems, nanosilver in vivo and the environment, 

thermodynamic and kinetic data for energy systems, and characterization of threedimensional photovoltaics. 

Technical Program Review, Findings, and Recommendations 

 Two projects were reviewed in detail. Their descriptions follow. 

NIST Atomistic Potentials Repository 

 The expected duration for this project is FY 2008–FY 2013, with a budget of 

approximately $300,000 per year. 

 This 5-year, $1.5 million NIST Atomistic Potentials Repository project is 

developing a public repository for interatomic potentials for use in atomistic simulations. 

Atomistic simulations are becoming more common within industry and academia; 

however, there is no single source of information on interatomic potentials. This 

important endeavor will lead to improvements in the accuracy and consistency of 

simulation results. The goal is to provide a Web-based, publicly accessible repository of 

interatomic potentials from known sources with reference data and tools to facilitate 

comparisons of potentials from different sources. The inputs are downloaded by the 

NIST team and audited by the potential developers. At this time more than 50 distinct 

potentials for elements and alloys are available for downloading. An important part of 

this project is outreach to researchers through annual workshops on Atomistic 

Simulations for Industrial Needs, which have been held since 2008. Future directions 
38 

include continuing to add other elements, alloys, and forms of interatomic interactions, 

standardization (through the user forums) and the extension of these potentials to predict 

elastic properties. 

 This project can be viewed as a “role model” for the division and the MSEL for 

the dissemination of data and models on the Web. 

Lead-free Solders: Tin Whiskers 

 The expected duration of the Lead-free Solders: Tin Whiskers project is 

FY 2006–FY 2011, with a budget of approximately $850,000 per year. The objective of 

this 5-year, $4.2 million project is to develop measurements and models to establish the 

underlying mechanism causing whisker growth in tin (Sn) electronic interconnects. As 

the electronic industry moves to lead-free interconnects, Sn whisker growth is an 

increasingly important and frequently vexing problem, which can lead to poor reliability 

of electronic devices. In this project the NIST team has used a tour-de-force of careful 

and complex experiments and leading-edge modeling techniques to elucidate the causal 

factors leading to these whiskers and to identify the means for their mitigation by means 

of increases in the electroplating current densities. 

 The Thermodynamics and Kinetics Group demonstrated an ability to meet its 

stated objectives and achieve its desired impacts in measurement science and standards. 

To ensure that its objectives are designed for maximum impact, this group makes 

excellent use of workshops with industry and academics to help define important 

materials systems and materials problems, which are important to its target customers. 

Findings and Recommendations 

 The panel’s findings and recommendations for the Thermodynamics and Kinetics 

Group are as follows: 

Finding: The technical merit of the programs that the Thermodynamics and 

Kinetics Group is conducting is at the leading edge of the state-of-the-art worldwide. Its 

researchers are highly regarded within the global technical community. The core 

competencies of this group are in solid-state phase transformations, multicomponent 

alloy thermodynamics, diffusion, solidification, microstructural and atomistic modeling, 

and surface energies. It has an exceptionally strong theoretical backbone, which is 

reinforced by the presence of experienced, competent technical leadership. 

Recommendation: The Thermodynamics and Kinetics Group should continue 

on the same path and should continue to engage other groups to emphasize the 

importance of theory and modeling. It should serve as a role model for the delivery of 

knowledge by way of the Web and should advance Web 2.0 concepts within the MSEL. 

In particular, it has opportunities to work with other groups in the Metallurgy Division 

(Mechanical Performance and Magnetics) to develop similar data and model 

dissemination techniques for mechanical and magnetic properties. 
39 

Recommendation: The Thermodynamics and Kinetics Group also has a specific 

opportunity to work with the Mechanical Performance Group for the development of 

ICME tools for sheet aluminum and steel. Such tools would be of significant value to the 

automotive industry. These groups should hold a joint workshop with automotive and 

academic experts to define goals and assess the resources required to accomplish this 

goal. 

Finding: The deep expertise in thermodynamics and kinetics enables this group 

to provide high-quality, rapid response to shifting national priorities. There is a strong 

emphasis on the inherent linkage between thermodynamics and kinetics and the use of 

these tools in the development of models that enable the prediction of microstructure—a 

key enabler for the prediction of complex properties, failure modes, and the discovery of 

new metrics for materials properties and performance. 

Recommendation: The Thermodynamics and Kinetics Group should work 

closely with other groups within the Metallurgy Division, especially the Mechanical 

Performance Group, to develop ICME tools. 

Finding: Web-based knowledge repositories and collaboration spaces are an 

increasingly important dissemination and collaboration mechanisms for all of the 

sciences. This group is playing an important role in exploring and developing 21stcentury Web-based (Web 2.0) means of deploying information to the materials 

community. In addition to the interatomic potential repository described above, the 

group has well-developed databases for thermodynamics and diffusion data, which it 

frequently updates. In addition, it has developed an open-source code for the solution of 

partial differential equations, called FiPy, and made it available through the NIST Web 

site. Differential equations form the core of most material science problems; however, 

because the detailed mechanisms are quite varied across material systems and problems, 

providing a comprehensive code for model development is a difficult challenge. The 

NIST FiPy code appears to be making an impact and has been downloaded by 2,400 

individuals to date. The second version of FiPy was released in February 2009. 

Recommendation: The Thermodynamics and Kinetics Group should work 

broadly with others within the MSEL to develop comprehensive and robust tools for 

knowledge dissemination and collaboration. 

METALLURGY DIVISION AND MSEL CROSSCUTTING ISSUES 

 Finding: Data and model dissemination and collaboration by way of the Web are 

not uniformly or fully developed in the Metallurgy Division (or the MSEL). 

Recommendation: The Metallurgy Division and the MSEL should consider 

developing a comprehensive approach to data and model dissemination and collaboration 

by way of the Web. Efforts in the Thermodynamics and Kinetics Group could be viewed 

as a role model for this activity. 
40 

Finding: Metrics of productivity are not always evident or uniformly articulated. 

Recommendation: Management should evaluate the utility of uniform metrics 

for such things as publications (e.g., h factor analysis), external support, patents and 

disclosures, and other factors, and apply them to various subunits and compare the results 

to selected benchmark groups. 

Finding: Technician support appears lower than optimal. 

Recommendation: The balance between scientists, technical support, 

administration, and Web support (information technology) should be evaluated and 

optimized for internal and external support. 
41 

5 

Polymers Division 

SUMMARY 

 The stated mission of the Polymers Division is based on NIST’s overall mission. 

Namely, 

To enable U.S. innovation and industrial competitiveness in the development and 

use of materials by advancing measurement science, standards, and technology—

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

 Within the general framework of polymers, the work of the division encompasses 

a broad range of activities that include advanced imaging measurements of the interaction 

of biological systems with polymer materials, organic photovoltaics and electronics, 

small-angle neutron and x-ray scattering measurements of nanostructured materials, the 

separation and purification of single-wall carbon nanotubes, and the enabling of new tests 

of the reliability of soft body armor. It would perhaps be best to articulate the mission in 

the following terms: “The mission of the Polymers Division ties into NIST’s overall 

mission as restricted to measurement sciences involving polymeric materials and 

complex fluids.” 

 The Polymers Division consists of 31 permanent technical staff (includes 2 NIST 

fellows), 19 NRC postdoctoral researchers, 2 term employees/students, and 67.6 NIST 

associates (see footnote 1), plus 5 administrative support staff. The total budget in FY 

2009 was $15.1 million, with $2.3 million coming from other agencies. Of the technical 

staff members, 5 are involved with significant amounts of administrative and supervisory 

duties, and roughly 15 members are associated with the externally funded American 

Dental Association Foundation portfolio. Hence, the number of the active permanent 

staff members in the core portfolio unsaddled with supervisory and administrative duties 

is 26. In response to suggestions offered by the panel that reviewed the laboratory in 

2008, the division has consolidated six groups into four groups and has consolidated the 

number of programs from 22 to 13. Each group has anywhere from 20 to 30 scientists, 

with roughly a 1:2 ratio of NIST permanent staff and postdoctoral researchers and NIST 

associates, a more leveraged organization than other areas of the MSEL or other 

Department of Energy national laboratories. 

 The Polymers Division continues to do outstanding research, to collaborate 

worldwide with academia and industry, and to have a great impact on the industry 

through CRADAs, Materials Transfer Agreements (MTAs), and various other technology 

transfer mechanisms. The Polymers Division displayed a high degree of coordination 

among staff members within the four core groups. This was particularly evident in the 

selection of equipment that was chosen for ARRA stimulus funding. This equipment 

expands the core capabilities of the Polymers Division in energy and materials 

characterization in ways that cut across the division and work also with staff in the NIST 
42 

Chemical Science and Technology Laboratory (CSTL) and the NIST Electronics and 

Electrical Engineering Laboratory. 

TECHNICAL MERIT RELATIVE TO STATE OF THE ART 

 The projects described in all four of the Polymers Division’s groups demonstrate 

outstanding technical performance in most areas, with accomplishments that are 

competitive with those of external academic, industrial, and government laboratories. 

There is a balance between research that is on the frontier of fundamental polymer 

science and metric science and technology, with outstanding accomplishments in each 

category. The Polymers Division continues to transfer technological developments into 

the industrial sector to have an economic impact and contribute to U.S. competitiveness 

on the international level. 

 In the period since March 2008, the division has published 137 refereed journal 

articles and 3 book chapters. The division is disseminating its results and findings 

through the literature at a rate commensurate with its size. It is hitting its internal targets 

for 4+ papers per year by senior principal investigators, with publications spread out over 

specialty journals and high-impact journals—for example, Science and Nature. The 

awards in the past 2 years—including the 2009 Presidential Early Career Award for 

Scientists and Engineers, the 2008 and 2010 Sigma Xi Young Investigator Award 

(NIST), the 2008 Spicer Award (Stanford Synchrotron Radiation Lightsource), the 2010 

Outstanding Young Scientist (Adhesion Society), and the 2008 Distinguished Committee 

Service Awards—speak to the quality of the young scientists who have been recruited 

into the division. Two of the division scientists hold the rare honor of being NIST 

fellows, with one of them having been so named in 2009. Recent recognition of the 

senior staff members includes the 2009 Patrick Laing Award (ASTM) and induction as a 

fellow in the American Physical Society. 

 The division’s programs are very highly leveraged with CRADAs, MTAs, 

interagency agreements, international research collaborations, an extremely active NRC 

postdoctoral program, and a highly successful national and international visiting scientist 

program. 

 In project after project, examples of measurement methods that are on the leading 

edge and that are also being applied and/or transitioned to the business sector are evident. 

NIST-developed measurement methods are continuing to have far-reaching consequences 

in transforming U.S. industries and promoting U.S. competitiveness. 

ADEQUACY OF FACILITIES, EQUIPMENT, AND HUMAN RESOURCES 

 Although the overall size of the Polymers Division staff has remained stable over 

the past 5 years, there has been a significant amount of turnover in the division. It lost 

several key administrators and scientists. With the realignment and in response to 

recommendations offered by the NCR panel that reviewed the laboratory in 2008, the 

Polymers Division has consolidated six groups into four groups and made changes in 

group leadership. One of the groups, however, is led temporarily by the division chief. 

These extraordinary changes in leadership over the past 2 years seem to be a concern to 
43 

the division staff. The current and proposed names for the groups in the Polymers 

Division are these: 

 Current: Characterization and Measurement Group; proposed: Sustainable 

Polymers Group; 

 Current: Electronic Materials Group; proposed: Energy and Electronic 

Materials Group; 

 Current: Processing Characterization Group; proposed: Complex Fluids 

Group; and 

 Current: Biomaterials Group; proposed: remain unchanged. 

 Division activities that engage substantial numbers of staff members were 

presented as “Supporting Activities.” At present, the division has identified four 

supporting activities: Safety, Standards, Theory and Modeling, and Industry Consortium: 

Soft Matter with Neutrons. Some of these have been grouped under the auspices of a 

named director, and others are loose confederacies (called working groups) with no clear 

reporting structure. As these and other supporting activities are critical in establishing the 

core competencies of the division, it would be advisable to make this structure more 

formal, with clear leads for each such crosscutting capability. Adding a reporting 

structure based on capabilities to the existing structure based on programmatic themes 

would lead to a matrix structure which would ensure that both problems and 

competencies persist as individual staff members enter or leave the division. 

 The Polymers Division has a large number of facilities and capabilities that are 

consistent with the breadth of its mission. The use of the facilities is generally managed 

on an ad hoc basis, with primary care performed by the users of the given equipment. The 

division has core competencies in areas as diverse as controlled biopolymer interfaces, 

combinatorial methods and fabrication, scaffold fabrication, optimal imaging and 

characterization, nonlinear optical spectroscopy, mechanical and adhesion property 

testing, polymer synthesis, microfluidics, mass spectroscopy, chromatography, x-ray and 

neutron characterization and reflectivity, electron microscopy, quantitative calorimetry, 

solid-state nuclear magnetic resonance (NMR), Brownian dynamics, fluid mechanics 

simulations, and phase-field simulations. Two notable mismatches between the capability 

suite and the existing facilities are the lack of significant computing resources (balancing 

the computational capabilities) and a wide-bore NMR (balancing the emerging solid-state 

NMR capabilities). Two ARRA-funded acquisitions are also coming online in 2010–

2011: an organic photovoltaic test facility ($1.2 million) and sum frequency generation 

and thin-film nonlinear optical spectroscopy ($750,000). The latter is notable because it 

involved collaboration (and an MOU) with the CSTL where it will be housed, although 

the asset is owned by the MSEL. The quality and number of facilities are impressive, but 

more acquisitions or MOUs with other NIST units will be needed in the future to 

maintain the needs of the programs. 

ACHIEVEMENT OF OBJECTIVES AND IMPACT 

 The panel reviewed selected examples of the technological research covered by 

the Polymers Division. Because of time constraints, it was not possible to review the 
44 

Polymers Division programs and projects exhaustively. The examples reviewed by the 

panel were selected by the Polymers Division. 

Biomaterials Group (Bioimaging and Biomaterials Measurements and Standards) 

 The four main projects in the Biomaterials Group within the Polymers Division of 

the MSEL are Quantitative Bioimaging, 3D Tissue Scaffolds, Protein Preservation, and 

Dental Materials. The group is composed of 7 permanent technical staff, 6 postdoctoral 

researchers, 38.2 research associates (see footnote 1), and 1 administrative support staff 

member. 

 Three major advances were described: broadband three-dimensional chemical 

imaging of biological tissue, deoxyribonucleic acid (DNA)-derivatized water-soluble 

quantum dots for functional bioimaging, and standards for dental materials and tissue 

engineering scaffolds. 

 The technical merit of the programs described was outstanding, leveraging the 

unique measurement capabilities of NIST with innovation in both standardization and in 

preparing unique and interesting materials. 

 As described below, the research programs in the areas of Bioimaging and Protein 

Preservation are outstanding. This is illustrated in terms of the relatively large amount of 

extramural funding, recognition, and dissemination. The work also contains significant 

collaboration outside NIST. Although this is generally positive, the downside is that the 

number of NIST staff members involved in the two projects is somewhat small. Due to 

the injection of ARRA funds, the budgets were adequate to acquire two major 

instrumental facilities important to the continued development of new standards and for 

advancing the research objectives, while also hiring an additional 10 postdoctoral 

fellows, doubling the number. 

 Every program showed significant advances in measurement science. 

Novel Spectroscopies

 The Novel Spectroscopies work was the first to demonstrate broadband Coherent 

Anti-Stokes Raman Scattering (CARS) microscopy, and it continues to develop this 

powerful microscopy. The method uses two broad input light pulses and one narrow one 

to read out the vibrational susceptibility of a sample. This possesses the inherent chemical 

sensitivity required to spatially map cell phenotype noninvasively. 

 This achievement is a major scientific breakthrough that was pursued by a number 

of groups. NIST succeeded by developing signal background reduction and analysis 

methods and improved signal generation methods to obtain sufficient sensitivity and 

specificity that CARS microscopy can be applied successfully to biological systems. 

Quantitative Bioimaging Project

 The Quantitative Bioimaging project is developing noninvasive optical methods 

and high-affinity probes for the quantitative imaging-based characterization of the 

structures inside the cell. This allows the researchers to gain information about cellbiomaterial interactions, including molecular signatures of cellular proliferation and 
45 

differentiation. These methods are promising for increased accuracy in evaluating 

biomaterials. These methods use aptamer-derivatized quantum dots as imaging probes for 

disease signatures. 

 Here they apply surface plasmon resonance imaging to measure the adsorption 

potential of engineered quantum dots on surfaces and interfaces and to measure the 

binding constants of their biomarker probes to specific targets. This may facilitate the 

accelerated development of materials and expanded progenitor cells for use in 

regenerative medicine. The researchers on this project are working closely with the 

National Institutes of Health and other agencies. 

The 3D Tissue Scaffold Project 

 The 3D Tissue Scaffold project is aimed at providing a reproducible 

combinatorial platform for screening cell response to three-dimensional tissue scaffold 

properties. The other stated goal of the project is to develop reference materials for tissue 

engineering. The platform combines noninvasive imaging with controlled scaffolds of 

multiple types (salt-leached scaffolds, hydrogels, electrospun nanofiber scaffolds). The 

arrays can provide gradients or discrete steps. 

 This systematization of standardized arrays combines innovative science with 

unique imaging. This capability has been extended to provide Reference Materials 

Scaffolds, a unique service to academic and industrial research laboratories, very much in 

line with the NIST mission. 

Protein Preservation Project

 Stability of proteins is critical in biopharmaceutical and drug delivery 

applications. The Protein Preservation project is developing analytical tools for rapid 

formulation assessment to avoid the 6-month testing cycle times for current technology. 

Also the researchers are aiming these studies to obtain an understanding of the 

preservation mechanisms. They are developing measurements to characterize sugar-based 

glasses with respect to their ability to serve as preservation media for therapeutic proteins 

and cytokines, and are working to develop theoretical bases for those measurements. 

 These methods are aimed at addressing critical needs of biopharmaceutical 

formulators, to allow sequestration of cytokines into and delivery from tissue scaffolds 

with minimal aggregation or chemical degradation. The project results indicate that the 

beta relaxation times correlated with the stability. 

The Dental Materials Project 

 The Dental Materials project has developed unique tools for the characterization 

of dental composite materials. It uses x-ray microcomputed tomography (μCT) to 

quantify and map (1) polymerization shrinkage and (2) the resultant gaps that appear 

between the material and tooth structure and often produce leakage. These defects are 

likely to be responsible for the secondary tooth decay now becoming an increasing health 

problem. 
46 

 The researchers find that slight variations in polymer fabrication protocol can 

alter the surface hydrophobicity and surface chemistry, which in turn can dramatically 

affect the initial bacterial colonization on films prepared from the same dental polymer. 

 To enable the use of these new NIST tools in an industrial laboratory 

environment, the project team has explained its method to instrument suppliers, industrial 

customers, other government agencies, and academia. Moreover, they are involved in the 

American Dental Association-Standards Committee for Dental Products to ensure the 

adoption of standardized tools. 

Findings and Recommendations 

 The panel’s finding and recommendation for the Biomaterials Group are as 

follows: 

Finding: The Bioimaging and Protein Preservation core areas are understaffed for 

the scope and importance of the work. 

Recommendation: The outstanding technical progress in the Bioimaging and 

Protein Preservation areas should be leveraged to grow these programs with additional 

staff and resources. 

Characterization and Measurement Group

 The Characterization and Measurement Group (composed of 7 permanent 

technical staff, 4 postdoctoral researchers, and 6.8 NIST associates [see footnote 1]) has 

completed a significant reorganization, with the merger of the Combinatorial Methods 

Group with the Characterization and Measurement Group, with a focus on sustainable 

materials. This transition is quite significant, and it was apparent in that there was not 

really a clear vision of this group, or at least a vision that reflected the ongoing research 

in the group. 

 This mismatch in research and vision is not unusual at such an early stage in a 

reorganization. Topics in the presentations included some beginning efforts on renewable 

materials, a complex interfaces (or a buckling and wrinkling) effort on thin polymer 

films, and a ballistic resistance effort. The quality of the research being presented was 

adequate, but the overall effort seemed a catchall, with a group of nonrelated topics being 

put together under one heading. It was not made clear how these different research 

efforts meshed toward a common goal, nor was it really clearly stated what the potential 

impact of the research would be in the short term and in the long term. This is important 

in the framework of a public presentation of the research and for establishing a coherent 

effort that will have significant impact from the combined expertise of the investigators 

on sustainable materials. The advances made in the ballistic-resistant materials were 

significant, and the identification of extractable phosphorus-containing materials as one 

route by which a chemical degradation of the soft body armor could occur was important. 

The expected route of wear by a continued mechanical working of the material was also 

uncovered. Test protocols were established in both cases, which is in line with the overall 

mission of NIST and, as a research topic, was quite appropriate for research at NIST. 
47 

However, there is no apparent reason why this should have been placed under the 

heading of sustainable materials. There are clearly some initial efforts being made on the 

enzymatic synthesis of some polycaprolactone materials and, along with notable external 

researchers, advances have been made in the adsorption/desorption of enzymes from 

polylactic acid (PLA) polymers (biodegradable polymers), by use of microfluidic devices 

pushing the synthesis to higher molecular weights was demonstrable but, in the long 

term, it is not clear how this will have a great impact. 

 Another area of research under this theme was on instabilities in thin polymer 

films. This effort was really focused on the advances made in the area of wrinkling in a 

composite film architecture where moduli, relaxation behavior, and dynamics in thin 

polymer films can be assessed. Some very tenuous coupling to sustainable materials was 

made, and some indications on the measurement of the mechanical properties of 

sustainable materials were made. However, it was very clear that this is an ongoing, 

successful research effort that has had a track record of accomplishments and that is not 

being integrated into an effort that really does fit with the other topics. There is no 

question that the surface is quite important in the degradation of materials and that the 

surface is the first part of a material that will fail and that the measurements can clearly 

provide information on the surface behavior of a material. What was not done in the 

presentation was to draw the results of the studies into a clear framework under the 

heading of sustainable materials. 

Findings and Recommendations 

 The panel’s findings and recommendations for the Characterization and 

Measurement Group are as follows: 

Finding: Sustainable materials are an important topic in which NIST should have 

a presence and be developing measurement standards or generating novel materials that 

will set their own standards; however, the Characterization and Measurement Group is 

not in a position at present to do this. 

Recommendation: To have a significant impact in this area, some effort on the 

synthesis of new materials is critical. 

. 

Finding: While this research is topical and the group could have significant 

impact, the effort is certainly not complete yet. 

Recommendation: A rescoping of the effort is needed; a redefinition of the 

vision is in order; a set of objectives, goals, and milestones needs to be established; and 

the researchers in this effort must work in a quasi-unified manner toward this common 

goal. 

Electronic Materials Group 

 The Electronic Materials Group is composed of 7 permanent technical staff, 5 

postdoctoral researchers, 11 NIST associates (see footnote 1), and 1 administrative 
48 

support staff member. The group’s vision is to transform itself to have an impact on both 

electronics and energy industries. The group’s efforts have been expanded to include 

significant work in organic electronics and photovoltaics, and some effort in energy 

storage and delivery materials toward accomplishing that vision. Some of the CRADAs 

in semiconductor electronics have been successfully completed, and several new 

CRADAs and MTAs have been initiated in organic photovoltaics. 

 Key facilities and instrumentation to which the group has access and developed 

include x-ray measurement capabilities, materials measurements, and a newly developed 

organic electronics processing laboratory. The group has been successful in obtaining 

close to $2 million for setting up an organic photovoltaic test facility and femtosecond 

laser-based nonlinear optical spectroscopy for thin-films analysis. 

 A strategic planning process has streamlined and integrated the group’s multiple 

programs into three broad umbrellas of dimensional metrology for nanofabrication, a new 

focus on materials for energy storage and delivery, and a focus on organic electronics and 

photovoltaics. 

 The dimensional metrology for nanofabrication activity is continuing to focus on 

addressing dimensional metrology needs as well as other critical issues of importance to 

lithography, such as line edge roughness, linewidth roughness, and the International 

Technology Roadmap for Semiconductors through a variety of techniques that include 

x-ray scattering, critical-dimension small-angle x-ray scattering (CD-SAXS), grazing 

incidence small-angle x-ray scattering (GISAXS), and quantitative rotational SANS. The 

group has validated and propagated the methods to industry through CRADAs, 

workshops at conferences, participation in industrial consortia meetings (e.g., 

SEMATECH), and participation in round-robin critical-dimension scanning electron 

microscopy (CD-SEM) and optical scatterometry measurement comparisons. 

 The Energy Storage and Delivery Materials project is focused on understanding 

the charge transport and device performance of fuel cells and batteries through an 

elucidation of the structure and dynamics in transport media of membranes. The 

researchers have demonstrated that ineleastic neutron scattering is sensitive to both 

nanosecond and picosecond dynamics, which dictate ion transport in Nafion in the case 

of fuel cells and polyethylene oxide (PEO) in the case of batteries. The effort unraveled 

an interface defined structure in Nafion that is subject to strong deviations in water 

diffusivity, solubility, and permeability in thin films. Polarization-modulation infrared 

reflectance spectroscopy measurements have demonstrated how interfacial regions of 

Nafion can impede water diffusion because of lamellar-like ion transport channels in 

Nafion. The study also established a strong correlation between the nanosecond and 

picosecond dynamics data obtained for hyperbranched PEO with neutron scattering to 

lithium-ion mobility in batteries. The effort is conducted through collaborations with both 

industry and global academia. 

 The Organic Electronics and Photovoltaics project has established several 

collaborations with academic institutions, the National Renewable Energy Laboratory, 

and many industrial institutions through CRADAs and MTAs, with a vision to develop a 

fundamental understanding of polymer semiconductors and polymer bulk heterojunction 

(BHJ) devices. Materials’ electrical parameters and device performance have been 

correlated to both molecular properties of constituent layers and the microstructure and 

interfacial properties of thin films. The microstructure and interfaces in turn are defined 
49 

by the process parameters. This insight is extremely important for taking the important 

fields of organic electronics and organic photovoltaics from an empirical state to a 

science-based understanding that will help develop reproducible devices from robust 

manufacturing processes. Some of the key accomplishments of the effort include the 

following: 

 An integrated suite of measurement techniques that determined the 

importance of conjugated plane tilt and side chain interdigitation in pBTTT 

polymers and its importance to their semiconducting properties. 

 Dark field TEM to quantify the size and orientation of the grains and correlate 

the domain size changes to semiconducting properties on the one hand and the 

process parameters on the other. 

 Interfacial segregation in BHJ films by a combination of NEXAFS, variableangle spectroscopic ellipsometry, and neutron reflectivity both to obtain 

composition information as a function of depth and to ascertain the role of 

substrate or superstrate. 

 Solid-state NMR to obtain phase and interface information and model bilayers 

to measure the exciton diffusion lengths and decouple the role of BHJ 

interfaces from morphology. Despite this success, it suggests an emerging 

need for a wide-bore solid-state NMR instrument capable of assessing 

heterogeneous materials and devices whose size exceeds that of the solid-state 

NMR equipment available at present in the laboratory. 

 The effort is well recognized, with 55 peer-reviewed publications; more than 

75 invited talks at conferences, industry, and academia; 15 industrial 

collaborations; 18 academic collaborations; 4 CRADAs; 2 MTAs; and 

conversion of MSEL funding to scientific and technical research services 

(STRS) base ($263,000) and 6 academic interns. 

The Processing Characterization Group 

 The Processing Characterization Group comprises 7 permanent technical staff, 4 

NRC postdoctoral researchers, 10.2 NIST associates (see footnote 1), and 1 

administrative support member. The mission of this group is to develop measurement 

methods that quantify the mesoscopic structures, the interactions, and the ultimate 

product performance of complex fluids. The proposed name change to “Complex Fluids 

Group” is logical. The technical leaders are very visible in the complex fluids 

community. Their publications and presentations are at a high technical level. Project 

areas of each group member were listed, but indications of quality such as publications 

and impact factor were not provided. The group lost one very visible staff member in the 

past year to academia and one to retirement, while one senior hire and one internal 

transfer were made. There appear to be many connections to industry, but these were not 

clearly documented or summarized. 

 The panel reviewed selected examples of the technological research covered by 

the Processing Characterization Group; however, the examples chosen did not tell a 

cohesive story that related how the changes implemented since the previous assessment 

improved the effectiveness of the group. 
50 

Carbon Nanotube Metrology 

The objective of this group is to develop and augment measurement technologies 

for identifying and predicting the properties of carbon nanotubes (CNTs). The Nanotube 

Metrology Program has made noteworthy progress since the assessment 2 years ago. It 

has developed a CNT SRM, which will be introduced this year. An indication of the need 

for this CNT SRM and who the customers will be were not presented. The addition of 

expertise in DNA that has been made allows CNT separation by chirality in addition to 

the group’s scalable centrifugation technique and has accelerated the Nanotube 

Metrology Program. 

 Although the size of the group appears sufficient to achieve the stated objectives 

and meet the challenges articulated, the long-term vision, impact, and future plans were 

not clear. The fact that no mention was made that this work was an improvement upon 

the state of the art seems an indication that there was no real excitement about the 

magnitude of the group’s accomplishments. 

Nanoparticle Assembly in Complex Fluids 

The objective of this group is to develop in situ measurements that quantify the 

dynamic structure, transport properties, and stability of nanoparticle assemblies in 

multicomponent fluids. The motivation statement is vague, and it does not capture that 

complex fluids can comprise a rich variety of systems including colloidal suspensions, 

surfactant mixtures, polymeric liquids, and biomolecular assemblies. This rich variety 

should make an interesting pathway for industry and academic collaboration. For 

example, the research efforts of the University of Illinois in soft materials, interfaces, and 

complex fluids can tie their theoretical/simulation efforts with the measurement paradigm 

at NIST. The pH jump experiments are impressive but need to show a tie to NIST 

missions, perhaps to environmental health and safety. The objectives of this program are 

unclear, as there was no clear statement of need from an external customer or partner. 

Micro-rheometry

 The objective of the Micro-rheometry Program is to develop micro- and 

nanofluidic tools that measure rheological properties of complex fluids. Over the past 

several years, the group has developed a clever, very small volume capillary rheometer 

for polymer melts. The microfluidic-based technology that it has developed to measure 

drop deformation and velocity tracking inside droplets is cutting-edge work. Although the 

ability to obtain interfacial tension, adsorption kinetics, as well as interfacial viscosity 

and especially dilation simultaneously was impressive, technical aspects were hard to 

understand, and the impact and importance to the field were not clearly articulated. 

Further, the step change advancement in rheological measurement was not framed within 

the overall space of the current state of the art. This provides another opportunity for 

broad dissemination of this work within the context of measurement science. This work 

seems to fit into the NIST mission of new measurement methods. 
51 

 Although commercialization is being pursued under an SBIR by a respectable 

small company, Cambridge Polymer Group, the group should also contact RheoSense to 

see if there is interest in its MEMS-based dynamic rheome. 

FINDINGS AND RECOMMENDATIONS 

Finding: The vision for the Polymers Division needs to be more clearly defined 

and presented in a more compelling manner. 

Recommendation: A crisper vision should be developed for the Polymers 

Division, portraying where the orgainization will be in a 5-year time period. The 

aspiration should be specified away from the simple aim of being a “great research 

laboratory.” Instead a clear vision should be articulated of which areas will be grown, the 

resources required (staff and equipment), and how this plan will lead to maintaining and 

enhancing the Polymers Division’s national and global prominence. 

Finding: The successful semiconductor electronics project appears to be 

terminating while substantial industrial interest in it remains. 

Recommendation: The Polymers Division should look for ways to maintain the 

size and scope of the semiconductor electronics effort to continue to have an impact on 

this important industry. 

Finding: The current division structure does not clearly align staff with core 

capabilities. 

Recommendation: A divisional structure should be considered that is more 

clearly matrixed to classify staff both along the lines of groups and of core capabilities. A 

capability leader should be identified for each core capability in order to ensure that the 

capabilities are appropriately managed and maintained through staff turnovers. 

Finding: There is a certain amount of anxiety and uncertainty owing to the loss of 

key personnel and an unfilled group leader position. 

Recommendation: The position of group leader for the Biomaterials Group 

should be filled as soon as possible. 

Finding: In some groups, particularly the Biomaterials Group, the substantial 

strength of the research area is strongly reliant on the competencies of non-NIST 

collaborators. 

Recommendation: These programs should be grown to increase the NIST 

competency, and this could be done through the leveraging of existing strengths. 

Finding: Theoretical and computational groups are not adequately integrated and 

would also benefit from increased ties to other groups outside NIST. At present they 
52 

meet through an ad hoc consortium and do not appear to have any unifying mechanisms, 

such as a seminar series, that focuses on theoretical and computational tools, or a 

common computing facility. Their computing needs are currently addressed through the 

use of desktop computing or off-site high-performance computing (HPC) facilities. A 

mid-sized HPC facility somewhere between these two extremes, located within the 

division, is notably absent. 

Recommendation: The theoretical and computational groups, in particular, 

should be unified within a core capability, and a capability leader should be identified. 

Through this leadership, collaboration between theoretical groups and through programs 

to experimentalists should be built. While this area would likely benefit from additional 

staff—temporary or permanent—the core capability and collaboration could also benefit 

from increased ties to theoretical and computational laboratories throughout the nation. 

(That is not to say that ties do not exist at present as, for example, existing collaborators 

include Juan de Pablo at the University of Wisconsin-Madison and Glenn Fredrickson at 

the University of California, Santa Barbara.) The acquisition of a mid-sized HPC facility 

managed by division scientists would permit local users to explore larger systems than 

those accessible on their personal computers without the overhead of requesting time on 

off-site HPC facilities or the need to ensure that they satisfy the parallelization 

requirements for said off-site resources. If managed properly, it would also enable the 

development of codes that scale across a larger number of processors within an 

environment that is more conducive for fast coding than that which can be found in 

typical off-site HPC facilities. An additional benefit of a mid-sized HPC facility is the 

social networks that it would create between the current set of broadly distributed 

computational scientists across the division. 

Finding: The quality and number of Polymers Division facilities are impressive, 

but more acquisitions or MOUs with other NIST units will be needed in the future to 

maintain the needs of the programs. 

Recommendation: A prioritized list of acquisition needs and how they dovetail 

into the division’s strategic plan should be prepared. Examples of future need are (1) a 

high-field, wide-bore NMR to advance solid-state characterization; and (2) increased 

high-performance computing assets to simulate the large, multiscale and heterogeneous 

materials being designed and measured within the programs. The motivation for these 

two target acquisitions was detailed earlier in the chapter. 

Finding: Close ties to instrument companies have been beneficial to transferring 

technology from NIST to U.S. industry. 

Recommendation: Relationships with analytical equipment companies, both as 

customers and collaborators, should continue to be aggressively cultivated so as to define 

simple pathways to transfer Polymers Division technological developments to the 

marketplace. In addition, with the continued drive toward new areas of polymer and 

measurement science, the inroads that have been made to existing technologies, like the 
53 

microelectronics industry, must be maintained for the impact of prior accomplishments to 

be fully realized. 

Finding: Mentoring of postdoctoral associates is uneven across the Polymers 

Division. 

Recommendation: A mentoring program and a set of guidelines for mentoring 

postdoctoral associates as well as junior staff should be established, and an expectation 

should be set that mentoring is necessary to be promoted to positions of leadership. 

Finding: Division scientists are well qualified to receive more national awards. 

Recommendation: The Polymers Division should focus on conducting evenhigher-impact research as well as on the marketing of the accomplishments and on 

obtaining due recognition for the work. 

Finding: The obvious strength of this very successful division needs to be 

enhanced by a bolder vision for expansion and growth. 

Recommendation: The Polymers Division should focus more on systematically 

pushing the boundaries of its budgets and its core competencies and less on addressing 

short-term administrative turnover and other exigencies. 
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6 

Overall Conclusions 

 The projects reviewed by the Panel on Materials Science and Engineering fulfill 

the mission of the Materials Science and Engineering Laboratory. They are formulated 

well and conducted in generally excellent facilities by an outstanding technical staff. 

Associates (visiting scientists) and postdoctoral researchers are usually well integrated 

into the projects. The results are appropriately disseminated and have received 

recognition by awards and through broad use by the technical community. Opportunities 

for improving the MSEL are related to operations—for example, integrating postdoctoral 

researchers, improving patent processes, and more effectively using the World Wide 

Web. The technical programs and staff of the MSEL are strong.