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Materials Science and Engineering Laboratory



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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 6 Materials Science and Engineering Laboratory

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 PANEL MEMBERS James Economy, University of Illinois at Urbana-Champaign, Chair David W. Johnson, Jr., Agere Systems (retired), Vice Chair Dawn A. Bonnell, University of Pennsylvania Karla Y. Carichner, Conexant Systems, Inc. Michael J. Cima, Massachusetts Institute of Technology F.W. Gordon Fearon, Dow Corning Corporation Katharine G. Frase, IBM Microelectronics Division Elizabeth G. Jacobs, Texas Instruments Sylvia M. Johnson, NASA-Ames Research Center Elsa Reichmanis, Bell Laboratories/Lucent Technologies Lloyd Robeson, Air Products and Chemicals, Inc. Iwona Turlik, Motorola Advanced Technology Center Robert L. White, Stanford University James C. Williams, Ohio State University Submitted for the panel by its Chair, James Economy, and its Vice Chair, David W. Johnson, Jr., this assessment of the fiscal year 2002 activities of the Materials Science and Engineering Laboratory is based on site visits by individual panel members, a formal meeting of the panel on March 14-15, 2002, in Gaithersburg, Md., and documents provided by the laboratory.1 1   Department of Commerce, Technology Administration, National Institute of Standards and Technology, Ceramics Division: FY2001 Programs and Accomplishments, NISTIR 6780, National Institute of Standards and Technology, Gaithersburg, Md., September 2001. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Materials Reliability Division: FY2001 Programs and Accomplishments, NISTIR 6795, National Institute of Standards and Technology, Gaithersburg, Md., September 2001. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Polymers Division: FY2001 Programs and Accomplishments, NISTIR 6796, National Institute of Standards and Technology, Gaithersburg, Md., September 2001. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Metallurgy Division: FY2001 Programs and Accomplishments, NISTIR 6797, National Institute of Standards and Technology, Gaithersburg, Md., September 2001.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 LABORATORY-LEVEL REVIEW Technical Merit The Materials Science and Engineering Laboratory (MSEL) states that its mission is to work with industry, standards bodies, universities, and other government laboratories to improve the nation’s measurements and standards infrastructure for materials. The MSEL is organized in four divisions: the Ceramics Division, the Materials Reliability Division, the Polymers Division, and the Metallurgy Division. These four divisions are assessed in the report that follows. MSEL also houses the NIST Center for Neutron Research, which is reviewed in a separate subpanel report at the end of this chapter. The MSEL organization is presented in Figure 6.1. The MSEL continues to perform work of strong technical merit. In general, the technical competence of staff members is very high, and their projects often push the state of the art and its applications. This strong technical merit is evidenced in part by the awards garnered by MSEL researchers and by the strong publication record that the laboratory has amassed. The level of accomplishment in the laboratory is quite high relative to similar organizations. The laboratory’s output is generally excellent in terms of both quality and quantity. The panel was particularly impressed with the accomplishments achieved relative to the resources available to laboratory researchers. The panel noted in particular that the laboratory is making better use of collaborations both within and outside of NIST. This change has had a positive impact on programs, increasing the depth of FIGURE 6.1 Organizational structure of the Materials Science and Engineering Laboratory. Listed under each division are the division’s groups. Listed for the NIST Center for Neutron Research are the center’s three groups.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 expertise brought to technical problems and thus increasing the sophistication of experiment and theory applied to their solutions. Specific examples of programs with particularly strong technical merit are presented in the divisional reports below. Program Relevance and Effectiveness Overall, the panel was pleased with the relevance and effectiveness of MSEL’s programs. Many examples of programs that have relevance and effectiveness exist, such as these: Phase equilibria studies. This area of basic research may be quite traditional, but the program goes beyond traditional methods to provide data on properties of materials and systems, which enables industrial researchers to solve important problems relevant to materials processing and product development. Combinatorial methods. Many researchers and organizations are involved in this “hot” field, which is already used to decrease discovery time in the pharmaceutical industry and is being adapted for many other development uses. However, MSEL has identified an important and appropriate niche in this crowded field, focusing on developing standardized methodologies and measurements so that researchers will ultimately be able to compare results obtained in different laboratories using different protocols. Standard Reference Materials. Although the production and characterization of SRMs may seem mundane, these artifacts underpin tens of thousands or more measurements in industry each year. They allow researchers throughout the country to assure the precision and accuracy of the measurements that underlie their guarantee of products’ performance and safety. The SRMs produced in MSEL are recognized as crucial to technology. NIST-Recommended Practice Guides. This recently instituted series of instructional booklets provides practical, easy-to-understand advice and guidance on performing standard materials measurements. The booklets are a means of disseminating the experience of NIST scientists, who practice measurement science every day, to researchers throughout the country, who may have recourse to these measurement methods only infrequently. MSEL has been a leader within NIST in publishing these Recommended Practice Guides. WebBooks. MSEL has initiated the publication of data through these instruments on the World Wide Web. These resources have been quickly utilized by the broad technical community and praised for their utility and impact. The divisional reports below contain more examples of programs with strong relevance and effectiveness. Although many strong examples of relevant and effective programs exist within the MSEL, there is still room for improvement. Although the laboratory has a strategic plan, it is not clear that all levels of staff understand the laboratory’s strategic priorities. Through its discussion with various levels of staff, the panel concluded that more effective communication of laboratory priorities, goals, and objectives is called for throughout the organization. There was a perception among some staff members that the laboratory’s stated priorities and goals were simply “buzzwords of the day” and not long-term strategic directions. All levels of laboratory management need to reinforce the importance of laboratory priorities through their actions as well as their words.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 Laboratory Resources Funding sources for the Materials Science and Engineering Laboratory are shown in Table 6.1. As of January 2002, staffing for the laboratory included 162 full-time permanent positions, of which 136 were for technical professionals. There were also 38 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers. NIST is finalizing its institutewide strategic plan and has identified several Strategic Focus Areas that can provide important opportunities for MSEL to contribute to national goals. In particular, MSEL has expertise that could contribute strongly to NIST work in the areas of homeland security (nondestructive evaluation of infrastructure) and health care (tissue engineering). However, the panel is concerned that the steady decline in the number of MSEL staff may make the laboratory unable to step up to these challenges and opportunities. TABLE 6.1 Sources of Funding for the Materials Science and Engineering Laboratory (in millions of dollars), FY 1999 to FY 2002 Source of Funding Fiscal Year 1999 (actual) Fiscal Year 2000 (actual) Fiscal Year 2001 (actual) Fiscal Year 2002 (estimated) NIST-STRS, excluding Competence 30.6 30.1 31.3 32.0 Competence 0.3 0.1 0.4 0.9 ATP 2.5 2.7 2.6 0.9 Measurement Services (SRM production) 0.9 0.7 1.0 1.0 OA/NFG/CRADA 3.8 3.9 2.8 3.1 Other Reimbursable 0.2 0.6 0.7 0.1 Totala 38.3 38.1 38.7 38.0 Full-time permanent staff (total)b,c 199 178 163 162 NOTE: Funding for the NIST Measurement and Standards Laboratories comes from a variety of sources. The laboratories receive appropriations from Congress, known as Scientific and Technical Research and Services (STRS) funding. Competence funding also comes from NIST’s congressional appropriations but is allocated by the NIST director’s office in multiyear grants for projects that advance NIST’s capabilities in new and emerging areas of measurement science. Advanced Technology Program (ATP) funding reflects support from NIST’s ATP for work done at the NIST laboratories in collaboration with or in support of ATP projects. Funding to support production of Standard Reference Materials (SRMs) is tied to the use of such products and is classified as “Measurement Services.” NIST laboratories also receive funding through grants or contracts from other [government] agencies (OA), from nonfederal government (NFG) agencies, and from industry in the form of cooperative research and development agreements (CRADAs). All other laboratory funding, including that for Calibration Services, is grouped under “Other Reimbursable.” aThe funding for the NIST Center for Neutron Research (NCNR) is excluded from these totals. Information about the center’s funding is available in the section of this chapter titled “Review of the NIST Center for Neutron Research,” which contains the subpanel review of that facility. bNCNR personnel are excluded from these totals. Information about the center’s personnel is available in the section of this chapter titled “Review of the NIST Center for Neutron Research.” cThe number of full-time permanent staff is as of January of that fiscal year.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 As the number of permanent staff continues to decline, the panel is concerned that core competencies of the laboratory are increasingly at risk. Important skills and knowledge often reside with only one staff member. Many important staff members are approaching retirement eligibility; mentoring and training of new staff in their skills must occur before these individuals leave. Declining numbers of personnel put the capability to transfer this knowledge at risk. Junior staff at the laboratory report that the presence of a strong cohort of colleagues is a major reason why they have chosen to work at NIST. If staffing levels continue to decline, this sense of being surrounded by the best colleagues will diminish, and the laboratory may find it difficult to attract and retain researchers with the skills needed to address important emerging areas of science relevant to NIST’s overall priorities. MSEL has some very good examples of leveraging its human resources through collaborations. Its program in tissue engineering is a particularly good example. This program involves collaborations with other laboratories at NIST, and with external researchers at other government agencies and in industry. The program consequently has the potential for far greater accomplishment and impact than if MSEL had attempted to enter this area on its own. The panel encourages MSEL to continue the efforts it has made thus far to use collaborations judiciously to extend the impact of its programs, and it urges MSEL to look for additional areas in which its resources might be so leveraged. MSEL has embarked on an important path of providing various means of linking and disseminating data through the Internet. The panel encourages this effort and urges the laboratory to consider strengthening its skill level in information technology (IT) to support these programs. MSEL has a particular management challenge because its staff is located in both Gaithersburg, Maryland, and Boulder, Colorado. The laboratory has greatly improved coordination between these two sites in the past year through a special budget to encourage staff to travel between the two sites to interact with their colleagues. Not only has this greatly improved collaboration between the Boulder and Gaithersburg staff, but it allows the laboratory to make much better use of the skills resident in Boulder. The panel hopes that resources for such travel will continue to be made available. It also notes that most of the travel in the past year was on the part of Boulder researchers; visits between Boulder and Gaithersburg should be more reciprocal. In particular, Gaithersburg laboratory management could reinforce the importance of staff at Boulder through more frequent visits there. Facilities for the Boulder researchers have improved somewhat but are still problematic and below standard for laboratory space of this sort. The panel understands that NIST is moving to correct facilities inadequacies at Boulder and will look for progress on this topic. Responsiveness to Previous Report The panel found excellent MSEL responsiveness to its previous report.2 In fact, last year the panel’s report also mentioned the excellent responsiveness of laboratory managers to the panel’s recommendations and suggestions. In almost all cases where specific program focus and direction had been questioned by the panel, the laboratory reexamined its programs and either adjusted the focus or terminated the program. The panel applauds the laboratory on this responsiveness. Continued attention is needed to more general concerns such as communication of goals and objectives to staff and to the potential for subcritical staffing of programs. 2   National Research Council, An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001, National Academy Press, Washington, D.C., 2001.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 MAJOR OBSERVATIONS The panel presents the following major observations: The Materials Science and Engineering Laboratory continues to field programs of high technical merit and strong relevance and effectiveness. Laboratory managers at all levels must reinforce laboratory goals and objectives in both words and action in order to increase understanding of these priorities throughout the laboratory and to improve program focus. The panel is concerned that decreasing staff levels put core MSEL competencies at risk and hamper the laboratory’s ability to step up to new challenges and priorities. MSEL should seek further opportunities to leverage its human resources through appropriate collaborations. The Tissue Engineering Program is an excellent example of such leveraging. Increased staff travel between Boulder and Gaithersburg has paid off in better collaborations between the two sites. Funding for such travel should be continued. DIVISIONAL REVIEWS Ceramics Division Technical Merit The Ceramics Division states its mission as working with industry, standards bodies, academia, and other government agencies in providing leadership for the nation’s measurements and standards infrastructure for ceramics materials. The division is now organized in six groups: Ceramic Manufacturing, Phase Equilibria, Film Characterization and Properties, Materials Microstructural Characterization, Surface Properties, and Data Technologies. The panel was presented with detailed updates on six divisional programs: Advanced Engine Materials, Powder Measurements, Advanced Manufacturing Methods, Nanotribology, Phase Equilibria, and X-ray Characterization. In the past year, the Ceramics Division has made several notable changes to its programs. It successfully completed the realignment of the ceramics machining and ceramics manufacturing activities and the coatings activities into the Powder Measurements Program and the Advanced Engine Materials Program. This change entailed directing resources to select, narrow problems such as specific nanoparticle characterization and reliability of thermal barrier coatings. A new industrial advisory panel on ceramic wear components was constituted for the Advanced Engine Materials Program. This advisory panel includes component suppliers, engine suppliers, and test instrument firms. Other changes include the expansion of efforts in nanotribology, wideband gap materials, and combinatorial chemistry. In addition, a new research effort on low-temperature co-fired ceramics (LTCC) was initiated as the Advanced Manufacturing Methods Program. A number of these changes implemented previous panel recommendations. Finally, owing to a promotion, the division is now planning a nationwide search for a new chief. The Powder Measurements Program focuses on three topics: measurement and dispersion of nanosize powders, measurements in concentrated systems, and detection and characterization of larger particles or agglomerates. These areas are extremely important for a rather broad cross-section of industry. For example, nanosized-particle media are used for chemical mechanical polishing of wafers at intermediate processing steps in microelectronic manufacturing, and nanosized particulates of phar-

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 maceuticals are increasingly important for the formulation of new drug products. Within the broad research arena, there is a severe lack of metrological rigor and an absence of standards for the characterization of nanoparticulate systems, despite their increasing importance. The division is pursuing three strategic research initiatives to mitigate this technological deficiency. The first is an effort to develop a sub-500-nm-particle-size Standard Reference Material. This material must have well-characterized physical and optical properties, and dispersion protocols must be provided. The second initiative is in situ measurements on slurries of nanoparticles and the detection of defect-causing particles. This research initiative could provide important new process control measurements as well as opening up important new basic science. Regarding the third initiative, a new project to determine the optical constants for nanoparticulates is under study. These constants are required to improve the accuracy of laser-based metrology methods for nanoparticles. Property measurements on nanometer-scale volumes of materials are increasingly important, and the panel believes that NIST should play an important role in developing these techniques. The Advanced Manufacturing Methods Program consists almost entirely of a process modeling effort for the manufacture of low-temperature co-fired ceramics. LTCC products are primarily used in hybrid packages for electronics. They are assuming an increasingly important role in modules for radio-frequency (RF) technology. Early generations of these packages were simple co-fired structures with Ag/Pd thick-film conductor traces. More recently, LTCC products incorporate co-fired resistors and capacitors. Active devices are added during postfiring assembly operations. In addition to electronics, several experimental approaches to preparing fluidic devices by this method exist, so that complex internal cavities can be produced. Key to all of the existing and potential applications is the ability to predict with precision any dimensional distortion that will occur during sintering. The current industrial practice involves empirical trial tests and repeated retooling. The NIST program seeks to develop predictive tools for these processes and is trying to leverage efforts at other laboratories that use different approaches to predicting the distortion that occurs during the manufacture of these products. The panel had some concern that this particular problem is rather narrowly focused to a small technical need. The microstructure-based modeling approach that is being employed is sound if applied to gross distortions that occur on the hundreds-of-microns scale. Unfortunately, the approach is unlikely to help with the very subtle distortions that occur on a macroscale, such as camber (bending). Many factors other than the local ceramic microstructure contribute to these small distortions on a large scale. It is possible this approach will lead to microstructure-based constitutive parameters and relationships that could be useful for conventional continuum modeling of the sintering process. Nanotribology is a critical area that directly impacts information storage industries. The division’s Nanotribology Program is in a leadership position in the area of magnetic hard disk technology. Recent technical advances achieved by the division include new measurement tools and new understanding of issues involved in molecular interactions in organic lubricating films. These studies have led to a strategy of molecular assembly of more effective organic lubricating films. The panel strongly endorses the division’s expansion of this program to include tribology in microelectromechanical devices (MEMs), since wear is a significant impediment to their broader adaptation. This expansion is possible because of an external grant program involving Ohio State University; the University of California, Davis; and the University of California, Berkeley. The panel further encourages strategic hiring to extend the division’s internal capabilities in MEMs, an area in which NIST has the potential to make substantial contributions. The X-ray Characterization Program continues to make outstanding contributions to many NIST research projects. The research carried out at the NIST beam lines at Brookhaven, the Advanced Photon Source, and NIST is of the highest quality. Some recent highlights that directly influence the Ceramics

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 Division include dopant identification in alumina, the structure of oxide films on GaAs, creep cavitation, and the formation of Stober silica. This program also includes research relevant to programs outside of the Ceramics Division, in areas such as protein crystallography. This research is exploring exciting new directions that extend the NIST competence in x-ray characterization to a broader community. The Advanced Engine Materials Program combines elements of the former Ceramic Manufacturing and Coatings Programs. “Advanced engine materials” is a very broad area, encompassing monolithic and composite materials and coatings for diesel and gas turbine engines. The program is focusing on two areas: rolling contact fatigue of silicon nitride and thermal and mechanical properties of thermal barrier coatings. The rolling contact fatigue work is aimed at diesel applications, while the thermal barrier coatings work is for gas turbine applications. The program has an Industrial Advisory Panel, consisting of both industrial and academic representatives. The first meeting of this advisory panel in December 2001 resulted in very positive comments on the program, together with the suggestion that a future measurement direction might be thin, wear-resistant films, especially for light alloys. Two NIST fellows are involved in this program, both in the area of rolling contact fatigue and in that of failure mechanisms at intermediate temperatures (700 to 800 °C). The division’s work on rolling contact fatigue is being guided by an assembly of companies, national laboratories, and universities through a Contact Damage Working Group. This group developed a project plan for studying the standard test methods for rolling contact fatigue, developing models, and developing a practice guide. A series of round-robin tests on the three-ball and cylinder test, a cam follower simulation test, and characterization of diesel engine parts after use are planned. The leader of the working group is also involved with the International Energy Agency in an effort to compare test methods used in Europe, Japan, and the United States. The division faces many practical considerations when designing test methodologies, and it must balance the ease of testing with the usefulness of the data derived from the test. This is particularly true for the three-ball test, which may require better instrumentation to understand the range of applicability of the test. The panel advocates a balanced approach to understanding current rolling contact fatigue testing methodologies and a broadening of the scope of testing approaches. The thermal barrier coatings work, a continuation of previous work, involves object-oriented finite-element (OOF) simulations, finite element modeling of residual stresses, and the development of a fracture mechanics model. The application of OOF is interesting, as are the variations in microstructure appearing as a result of changing the imaging analysis protocol. Modeling has been done on ideal microstructures and is being extended to real microstructures. The initial results of this effort are promising. This work is performed in collaboration with GE, and, in general, the panel finds this work to be scientifically sound and of interest to the community. The Phase Equilibria Program has continued its excellent work during the past year. A current focus on dielectric ceramics seeks to measure and predict phase equilibria and electronic behavior in dielectric oxide ceramics, with applications to relaxor ferroelectrics, dielectrics for cellular base stations, and dielectrics for LTCC applications. First-principles computational studies are included in this effort. The particular merit of this program is that it enables the use of phase diagrams to determine material compositions that have specific properties needed for industrially important applications. An example is the need to have materials with high permittivities as well as temperature stability. Development and exploration of a potential phase diagram (MgO-LaO1.5-TiO2-CaTiO3) steered industry away from one research direction and indicated more likely compositional areas. In the study of the Bi-Zn-Nb-O system, the use of phase diagrams and structure refinement contributed significantly to the understanding of the properties of a particular compound. The first-principles effort has made progress, as in the development of an approach to enable 40 × 40 × 40 molecular dynamic calculations. The long-term goal

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 of this effort is to guide experimental work, and the work described by the division is consistent with that goal. Program Relevance and Effectiveness The Nanotribology Program is well connected with industry through active involvement in the National Storage Industry Consortium. The relevance of this program to industry is demonstrated by the active participation of industry leaders in the NIST research. The X-ray Characterization Program has a number of impacts. SRMs for line position and quantitative analysis developed in the program are being utilized at an increased rate, with 50 to 100 percent more sales this year than last. The breadth of impact is also demonstrated in the prolific publications that NIST has had in this area in journals as diverse as Nature, Physical Review, and Macromolecules. An extensive community that involves more than 100 direct users from more than 50 academic and industrial sites utilizes x-ray beam lines that are supported by NIST. The impact in materials research is much broader than even these numbers indicate. The existence of these facilities and the excellence of the associated staff are a critical asset to the country. The Advanced Engine Materials Program is exploring areas of industrial relevance and, as mentioned above, has engaged an industrial advisory panel to evaluate the work. The guidance received from the working group in contact fatigue is valuable. The program has identified that existing rolling contact fatigue testing methodologies lack reproducibility and that no basic understanding exists of the relevant phenomena that control the outcome of the tests. This is an important opportunity for future work. The thermal barrier coatings work is of interest, but the program should consider expanding industrial contacts in this area for further guidance. The Phase Equilibria Program is addressing problems of considerable technical interest. Resulting presentations at technical meetings have resulted in valuable interchange with peers and have aided industry and academia in understanding and developing new materials. The program has also provided one of several excellent opportunities for summer undergraduate research fellowships (SURF) students. Both the productivity of this program and its technical relevance are outstanding. Even the first-principles effort is involved in applications through a working group and workshops. The potential of this basic effort is considerable, and it should be continued. The Powder Measurements Program has been extremely effective in disseminating results and information during the past year and at gaining direction from industrial collaborators. More than 3,800 hard copies and more than 13,000 Web downloads of the “Particle Size Characterization” Recommended Practice Guide (RPG) were distributed. More than 400 copies of “The Use of Nomenclature in Dispersion Science and Technology” RPG were requested between October 2001 and March 2002. The program’s focus group conducted a workshop on nanopowder measurement needs, and attendees included electronic materials suppliers, pharmaceutical companies, instrument manufacturers, national laboratories, armed services laboratories, and universities. The results were used to propose the research agenda for the newly focused program. Division Resources Funding sources for the Ceramics Division are shown in Table 6.2. As of January 2002, staffing for the division included 52 full-time permanent positions, of which 44 were for technical professionals. There were also 4 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 TABLE 6.2 Sources of Funding for the Ceramics Division (in millions of dollars), FY 1999 to FY 2002 Source of Funding Fiscal Year 1999 (actual) Fiscal Year 2000 (actual) Fiscal Year 2001 (actual) Fiscal Year 2002 (estimated) NIST-STRS, excluding Competence 9.4 9.2 9.6 8.8 Competence 0.0 0.0 0.1 0.1 ATP 0.7 0.8 0.7 0.2 Measurement Services (SRM production) 0.3 0.2 0.2 0.0 OA/NFG/CRADA 1.2 1.5 1.0 0.9 Other Reimbursable 0.1 0.2 0.2 0.1 Total 11.7 11.9 11.8 10.1 Full-time permanent staff (total)a 59 57 51 52 NOTE: Sources of funding are as described in the note accompanying Table 6.1. aThe number of full-time permanent staff is as of January of that fiscal year. Materials Reliability Division Technical Merit The mission of the Materials Reliability Division is to develop and disseminate measurement methods and standards enhancing the quality and reliability of materials and to provide technical leadership in their introduction to the appropriate industries. The division is organized in three groups: Microscale Measurements, Microstructure Sensing, and Process Sensing and Modeling. This division has continued to shift its focus to the electronics industry while maintaining several key infrastructure support efforts. It is also exploring opportunities to apply its unique expertise in new directions, such as health care research. The Microscale Measurements Group is working on advanced measurements for microelectronic chip and chip package failure modes. The group has made significant advances in areas including quantitative assessment of the role of strain in electromigration failure, establishing standard methods for mechanical testing of thin films, quantifying interfacial thermal resistance in packaging systems, and establishing a high-temperature SRM for thermal coatings. The Microstructure Sensing Group studies the use of advanced ultrasonics for microelectronic applications. This group continued to develop and apply measurement technology to improve understanding of the properties and performance of materials. Advances were made in the past year in the ability to make quantitative measurements of thin-film mechanical properties using acoustics. A Green’s function analysis technique was developed that allows for the measurement of anisotropic film properties. TiN hardness measurements were made and correlated to nanoindentation results. The group has also made progress in using carbon nanotubes as atomic force microscopy cantilever tips for making conductivity measurements. The Process Sensing and Modeling Group concentrates on developing material measurement tech-

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 should develop a new project or research topic that is uniquely suited to being tackled with neutron diffraction. Staff are to be commended for their commitment to enhancing the effectiveness of the diffractometer and improving the effectiveness of users’ interface with this instrument. Several improvements to the diffractometer have been made in the past year, including the replacement of the existing silicon monochromator crystal with a germanium crystal that has a new cut and orientation. The new germanium monochromator will theoretically yield a higher-intensity incident beam at the sample, although the impact of this change on data collected using the diffractometer will not be known for some time. The efforts to upgrade the capabilities of the diffractometer are important, as they make this instrument a more flexible alternative to instruments being developed for neutron powder diffraction at SNS. Other recent accomplishments in crystallography include the development of a new data collection front end for the diffractometer, new Web-based methods to monitor the instrument, Web-based access (via an intranet) to data archives, an expanded and improved GSAS user interface with standardized output, and new internal algorithms for GSAS. All of these efforts are appropriate projects and are consistent with the NCNR mission of developing and applying neutron measurement methods. In diffraction applications, the team has a clear focus and definite goals, supported by a substantial outreach effort to several external communities. These interactions with outside scientists have helped the team staff put together a portfolio of projects that are particularly suited for neutron diffraction and have notable impact in external industrial and materials communities. The team’s work includes determining strains and composition versus depth in plasma-sprayed and thermal barrier coatings, evaluating the parameters that control stress and elastic properties in sprayed coatings, determining stresses in new types of welds, relating weld stresses to crack propagation (in a collaboration with a well-known expert in plasticity modeling), determining local effects on elastic property uncertainties from analytical work and from modeling techniques using object-oriented finite element analysis, and working with the European Committee for Standardization to develop standards for neutron diffraction-based residual stress. These activities are consistent with NCNR’s mission to develop neutron measurement techniques and to apply them to problems of national interest. Another example of a team project with national significance is the effort to verify experimentally (by measuring the stresses present in representative metal-formed parts) the stress distributions derived from finite element models being used by U.S. Council for Automotive Research and by the rail industry. In addition to using the residual stress diffractometer at NCNR and collaborating with researchers at organizations outside NIST, the team also takes advantage of other materials characterization techniques (e.g., orientation imaging electron microscopy, x-ray diffraction, SANS) and collaborates with other NIST units (such as the Metallurgy Division) to strengthen the quality and impact of its research efforts. In addition to the research activities described above, the team is responsible for the neutron diffraction residual stress instrument. Experiments on this diffractometer fill an important role for the industrial and academic communities that need to perform residual stress measurements. This work is currently carried out by only three people and could benefit from at least part-time technical assistance with sample handling and instrument setup. Since the capability to do such residual stress measurements is not currently planned for the start-up phase of the SNS, it is likely that the residual stress instrument will continue to be a linchpin of certain user communities, and thus improvements to this diffractometer continue. This year, a doubly-bent monochromator was added, and a substantial increase in the intensity of the Fe(211) diffraction peak resulted.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 Chemical Physics The Chemical Physics Team carries out a number of projects for the study of the motion of atoms and molecules. Topics under investigation range from hydrogen bond dynamics in crystals to biopolymer dynamics in aqueous solutions. The scope of the problems attacked as well as the level of science is impressive, and interesting and important research is under way. One example is the use of Debye-Waller factors to study the thickness dependence of the time scales of local motion in polymer films. Such studies shed light on the nature of the glass transition, which remains a hotly debated area of condensed-matter chemical physics. Other work includes investigation of the nature of hydrogen bond hopping in large-unit cell crystals that have several modes for proton motion. These studies were very nicely complemented by simulations. Work of biological relevance includes measurement of the solution dynamics of proteins (cytochrome C) in native, unfolded, collapsed, and alpha-helical conformations. This is a proof-of-concept type of study to show that quasi-elastic scattering can provide information on protein structure in various buffer environments. Finally, the team has examined hydrogen diffusion in crystals where the lattice structure contains the motion to be highly anisotropic, 2d in this case. There exist only a finite number of hydrogen-containing interstitial sites with a substantial filling factor. These studies thus relate to the problem of 2d hopping in systems with strong excluded volume correlations; this fundamentally interesting problem could well engender strong interest in the theoretical community. In addition to performing research, the Chemical Physics Team also is responsible for the scientific support for NCNR’s five spectrometers, designed for inelastic/quasi-elastic scattering in different regimes. This collection of instruments enables experiments focused on times ranging from 100 ns down to 0.01 ps. This impressive dynamic range allows scientists to probe many types of nuclear motions in liquids and solids, and in the last operating cycle these spectrometers were used by more than 200 scientists from more than 50 institutions. As with other teams in NCNR, the Chemical Physics Team is making instrument development plans with the goal of becoming complementary to the SNS. Condensed Matter Physics The Condensed Matter Physics Team continues to carry out its strong research program. The focus is on problems at the forefront of the field of strongly correlated materials as well as important and interesting problems relevant to technological applications. Projects under way include work on elucidating the electronic underpinning of the unusual heavy electron Skudderudite PrOs4Sb12; the discovery of a new class of magnetic excitation in frustrated magnetic materials; an important study of spin-diluted La2CuO4near the percolation threshold; investigation of edge states in Haldane gap systems; the finding of mesoscopic phase separation in a Fe/Re double perovskite; a study of digital ferromagnetic superlattices of Mn/GaAs, a system of great interest to the spintronics community; the determination that state-of-the-art high-density storage media have less than the expected optimal microscopic magnetic polarization characteristics; and an excellent study on the lattice dynamics of very-high-dielectric-constant relaxors. These projects address highly topical problems, and the results are published in leading journals, such as Science and Physical Review Letters. The powder diffractometer (BT-1), the spin-polarized triple-axis spectrometer (SPINS), and the polarized neutron reflectivity instruments have all been essential for carrying out this work. The team takes full advantage of its excellent external collaborations with researchers in industry, government laboratories, and universities, while maintaining strong rapport within the team, which has a strong staff of postdoctoral research fellows.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 Life Sciences In 2001, NCNR joined with five universities5 to form the Cold Neutrons for Biology and Technology (CNBT) collaboration. This collaborative team recently received funding from the National Institutes of Health to support a variety of initiatives: a new diffractometer/reflectometer for biological structure studies, some time on the 30-m SANS instrument, staff members and postdoctoral research fellows (hired by the universities and placed at NIST), and new computer-modeling and laboratory capabilities. The subpanel commends NCNR’s efforts to explore ways that neutron research can impact new scientific fields and believes that the work in this area has promise. The partnership with universities is appropriate, and obtaining funding from a new source (NIH) is a notable achievement. As NCNR moves forward in this area, challenges as well as opportunities will of course arise. Planning for new projects of biological relevance or actual biology-related research is under way in several of NCNR’s scientific groups. In the Macromolecular and Microstructure Science Team, staff will focus on using SANS to study the structure of transmembrane proteins. In the Chemical Physics Team, efforts have already begun in the uncharted and potentially crucial area of the dynamics of biomolecules, with the project on observing the solution dynamics of proteins (cytochrome C). This work may lead eventually to the quantitative investigations of biological functional dynamics at the molecular level; undertaking such studies would certainly be a worthy and timely venture. The challenges facing NCNR as it moves into biological research relate mainly to the difficulties inherent in any change of focus at a research institution. The primary task will be the missionary element (a key component of all NCNR programs): reaching out to biologists to demonstrate the relevance and value of neutron techniques to problems of interest to the biological community. Building relationships with biological scientists is essential, as their expertise is needed to help staff determine which specific biological problems both would be susceptible to being tackled with neutron-based methods and would produce results of interest to key biological scientists. For example, what protein structures or dynamics should be studied? It is not currently clear to the subpanel who will perform outreach to biologists for NCNR. NCNR staff are not yet fully familiar with the relevant external communities, and the number of NCNR staff in this area is limited, so perhaps the university scientists in the CNBT will take on this critical task. The lack of in-house staff with biological expertise raises other questions that NCNR must tackle as it moves forward in this new direction. Does NCNR want to expand the number of permanent personnel in this area, or will it rely on temporary staff and collaborators within and outside NIST? Currently, in addition to its university partners, NCNR is working closely with the NIST Biotechnology Division (of the Chemical Science and Technology Laboratory) on the biostructure work. In any case, NCNR will have to be prepared to adjust a variety of its standard experimental approaches to take into account the different kinds of samples on which biological research is focused. For example, in reflectivity studies in the surface and interfacial science area, the preparation of a biological sample will probably require a greater investment of time and effort than is typically needed for hard materials. The NCNR has indicated that it plans to add a wet laboratory on-site to support biology users, but the subpanel cautions that the equipment and safety issues for such a facility will be markedly different from those usually faced by NCNR staff, and NCNR should draw on those both within and outside NIST who have appropriate expertise to advise the center on the construction and use of such laboratories. 5   The members of the NIH-funded CNBT are NIST, the University of California at Irvine, Rice University, the University of Pennsylvania, Duke University, and Carnegie Mellon University.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 Reactor Operations and Research Facilities The primary focus of reactor operations in the 2001-2002 period was a long-awaited, extended shutdown that began in August 2001. Major upgrades to the facility were carried out during this shutdown, including the installation of a new cold neutron source, replacement of the main electrical transformers and switchgear that supply electrical power to the reactor, and replacement of the cooling towers. In addition, temporary repairs were made to the leaking thermal-column cooling system. During the shutdown, the NCNR staff overcame a variety of obstacles and maintained an ambitious shutdown schedule; their performance was nothing short of astonishing. The reactor was restarted on March 8, 2002, only 1 week later than originally scheduled. It is a credit to the planning and resourcefulness of the operations management and staff that multiple large and complex projects were carried out simultaneously and were successfully accomplished. From the perspective of the neutron research community, the most significant development was the installation of a new cold neutron source. The old source was highly successful and still functioned outstandingly, but NCNR management clearly recognizes the need for continuous improvement, and it actively supports and encourages innovation by members of the staff. The new cold neutron source is the culmination of several years of designing, machining, welding, and testing. Preliminary measurements of the cold neutron beam from this source indicate that a doubling of flux has been obtained at wavelengths from 0.02 to 1.0 nm, which means that design expectations have been met or exceeded. The subpanel is impressed by NCNR’s willingness to undertake this long and complex task and applauds its success. Replacing the main electrical power supply components and the cooling towers was essential for extending the life of the facility, and it had to be done to support the renewal of the reactor’s operating license for another 20 years. Taking the electrical power supply out of operation was a particularly disruptive operation that had to be carefully planned and coordinated to minimize its impact on the other activities at NCNR during this shutdown. All went as planned with both replacement projects (electrical system and cooling towers). The one exception is that some rework is required on the cooling tower basin because of a contractor error in pouring the concrete. This oversight will be corrected by the contractor during a routine shutdown in warmer weather, and no impact on the operation of the towers is foreseen. The final major activity of the shutdown was the work on the thermal column cooling system, which is located behind heavy radiation shielding. State-of-the-art fiber-optic inspection equipment was used to determine that the heavy water leaking within this system, originally suspected to originate only from piping, was also issuing from cracks in the welded seams of the aluminum thermal column tank. Temporary repairs to the tank were made, and a new tank is being designed and fabricated and should be completed by the end of 2002. It should be noted that a recurrence of leakage before the tank is replaced should not present a hazard, since any leaking water would be safely captured by a closed collection system. Another leakage problem is occurring in the corroded copper tubes that carry cooling water for the bioshield. This is a recurring problem, currently at the level of no more than an annoyance, although it may worsen over time. Preemptive efforts are under way to develop a method for prevention or repair of such leaks without having to dismantle the bioshield. The feasibility of various techniques such as chemical coating, plating, and sleeving the internal surface of the copper tubing are being investigated as possible remedies for this problem. Ultimately, if these efforts are unsuccessful, eventual replacement of parts of the bioshield with its embedded cooling system may be required at some time in the future. This would be a significant undertaking, but far from impossible.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 The shutdown occupied a great deal of the operations staff’s time and attention, but appreciable progress continues to be made on preparing for the application to relicense the NCNR’s reactor for another 20-year period. Several key facility upgrades were completed during the shutdown, and the focus is now on determining the expected lifetime of the aluminum reactor vessel. Bombardment by neutrons causes transmutation of the aluminum into silicon, which gradually causes the material to become less ductile. The rate at which ductility is lost depends on the particular alloy of aluminum used and the ratio of thermal-to-fast neutrons impinging on the vessel wall. The safety issue of concern is to determine when the vessel may become subject to stress-corrosion cracking or brittle failure. NIST has contracted with Brookhaven National Laboratory to develop a computational model of the reactor that will determine the neutron fluence and energy distribution throughout the vessel. If required, a materials surveillance program will be set up to periodically examine aluminum coupons taken from discharged vessel internals. The condition of the vessel itself could then be inferred from the calculated neutron fluence on the coupon and the condition of the material determined by metallurgical examination of the coupons. Computer modeling and any required tests could be completed in ample time to support the submission of the relicensing application at the end of 2003 or the beginning of 2004. NCNR is also making headway on the Safety Analysis Report, another key element of the relicensing effort. A draft of this report is due to be completed at the end of 2002 and reviewed during 2003. The subpanel is impressed with the attention paid to safety at NCNR. The emphasis on safety is not limited to operations personnel or to the NCNR staff but is also evident in the training and work controls set up for more than 1,500 external users each year. Several new safety enhancements were added to NCNR during the extended shutdown. A walkway around the guide hall, where the instruments are located, has been painted bright blue to call attention to the fact that this area must be kept clear of equipment, cables, and other objects that might present tripping hazards or that might block egress in an emergency. Also, within the reactor building, the new electrical wiring that supplies power to the beamline instrumentation allows experimental equipment to be shut off from a location far enough away to protect personnel in the event of a fire or of high radiation in the immediate area of the equipment. These enhancements are evidence of management’s strong commitment to a proactive approach to safety. A key focus of safety efforts at all reactor facilities is minimizing the radiation doses received by staff. NCNR has an excellent record in this area. This year, larger-than-usual radiation doses (although still well within safe levels) were received by members of the operations staff and some contractor personnel during the shutdown, primarily as a result of the need to inspect and repair or replace highly radioactive components. As indicated by personal dosimetry monitoring, the total dose received by these personnel during the shutdown amounted to approximately 17 rem, most of which was associated with the cutting and removal of shields. Removal of the old cold neutron source and installation of the new one was also a “hot” job, giving personnel associated with the task a total dose of slightly more than 8 rem. Considering the complexity of this work and the high radiation levels that were present owing to activated components, the doses received were actually rather modest. (The highest individual doses were received by a contract welder [1.9 rem] and a reactor operator [0.9 rem]; these doses are well below established safe limits for occupational workers.) Nevertheless, the subpanel hopes that the experience gained during the recent shutdown will be used to plan even more effective methods for reducing the doses received by operations personnel in future high-radiation jobs of this nature. Program Relevance and Effectiveness The primary customer of NCNR is the neutron science community of researchers who use the reactor and associated instruments at NIST to perform fundamental and applied research in a wide

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 variety of fields. The subpanel commends NCNR staff for their continued focus on effectively serving these users. During the past year, the facility served a total of 1,744 participants, including researchers from 49 different industrial organizations and 124 universities. Work done by these researchers and by NCNR staff provided the basis for more than 365 papers accepted or published in archival journals in FY 2001. Through these publications, the impact of the NCNR facility is felt even beyond its sizable user community. NCNR also continues to organize and host popular annual summer programs to train new members of the neutron science community. In the summer of 2001, 33 people, mainly graduate students and postdoctoral research associates, attended a week-long course on methods and applications of neutron spectroscopy; preparation is already under way for the 2002 program on neutron small-angle scattering and reflectometry from submicron structures. Many different models are used to support the users of NCNR. Some people are part of research collaborations with NCNR scientists, who do the experiments on NCNR instruments. In other cases, external scientists apply for beam time on the instruments to do their own research projects. An NCNR Users Group exists (run by and for the users to address air concerns and needs), but the subpanel was informed that this group has little to do because users are, on the whole, remarkably pleased with the quality of the instruments available and the support received at NCNR. A major facilitator of the external use of NCNR instruments is the National Science Foundation (NSF), which supplements NIST support for the Center for High Resolution Neutron Scattering (CHRNS) at NCNR. CHRNS consists of six instruments, the 30-m SANS at NG-3, the USANS, the SPINS, a time-of-flight disk-chopper spectrometer (DCS), a high-flux backscattering spectrometer (HFBS), and a neutron spin echo (NSE) spectrometer. The last three instruments were added to the CHRNS umbrella this past year, and NSF’s support of these inelastic scattering instruments has allowed NCNR to expand the amount of user time available on them. However, the applications for this newly available beam time still exceeded the amount of time being offered; the user base and desire for access to these instruments clearly exist. NCNR staff have recently made a number of commendable efforts to improve user experiences at their facility. The development of new instruments and the upgrades of older instruments continue, and current plans call for the eventual refurbishment of all the thermal instruments, which will result in a significant improvement in the overall capabilities accessible at NCNR. A past concern has been the quality of the data-gathering and analysis tools available to users, and the neutron science and research facility operations personnel have devoted a significant amount of effort to improving the situation. New tools developed during the extended 2001-2002 shutdown include the data analysis and visualization environment (DAVE) software for treating and analyzing time-of-flight, backscattering, and triple-axis data sets and the data reduction and analysis software (IGOR) for SANS and USANS data. The effectiveness of these programs will be tested by users in the next round of experiments. Other new approaches designed to improve user experiences include the recent hiring of two SANS “operators,” who will be present at the start of each new experiment undertaken by a team of external users. Before each new team arrives, the operator will ensure that all equipment needed for mounting, maintaining, and demounting samples is ready for use and that the data acquisition and computing resources at the SANS instrument are in good working order. The operators can assist with setting up spectrometer configurations that have been predetermined by the users and the instrument scientist contact at NCNR; with mounting sample holders and other ancillary equipment such as constant-temperature environments, magnets, rheometers, and so forth; and with identifying and solving problems that otherwise might create hardships for the users of the SANS instruments. The subpanel expects that these personnel will provide an excellent enhancement of NCNR’s already-strong resources for user assistance.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 While the primary focus of these new approaches to user support is enhancing the users’ experiences at NCNR, another important benefit is that of using NCNR personnel’s time more efficiently. This not only enables NCNR to support an ever-increasing number of users at the facility but also allows the in-house staff to spend time on their own research activities and not be overwhelmed by instrument support obligations. The increased flux provided by the new cold neutron source will reduce the amount of beam time needed for some types of experiments and will make new types of research possible, and so both more and new users will probably be drawn to NCNR. It is not clear to the subpanel that if the number of users increases significantly, the current staff level will be adequate to provide the high level of scientific and technical support that NCNR users are accustomed to receiving. Different neutron science teams at NCNR have different approaches to their respective external user communities. The Macromolecular and Microstructure Science Team is very active in promoting use of its instruments by researchers from academia, industry, and government laboratories, through instrument Web sites, individual contacts, and extensive participation in conferences. The Surface and Interfacial Science Team works with an extraordinarily active user community for the reflectivity instruments, whose beam time is always oversubscribed; here the typical mode of operation with outside users is through collaborations. In the Crystallography and Diffraction Applications Team, the availability of on-site staff for assistance with the BT-1 and BT-8 diffractometers is particularly attractive to industrial collaborators, who are often pressed for time and generally have inadequate personnel resources of their own to devote to complex instrument setup. In general, methods of interacting with industrial users vary across NCNR. On some instruments, companies provide support through participating research teams (PRTs); on other instruments, staff have very active nonproprietary industrial collaborations; and on some topics, practically no interactions with industry occur. Although not all teams are equally engaged with liaisons with industry or receptive to the possible performance of proprietary work, the spectrum of interactions appears to represent a good overall balance for NCNR-industrial interactions. However, the software tools and support for some instruments are so clearly designed for open, nonproprietary work that an industrial user would be severely handicapped if an attempt was made to do proprietary work at NCNR on those instruments. For instruments on which beam time is available to the general scientific community, that beam time is allocated by the Program Advisory Committee (PAC). This advisory committee is composed of nine neutron scientists (not from NCNR) who meet twice a year to review the proposals submitted for the various user instruments (currently there are 10 such instruments). For all of these instruments, the number of days of beam time requested in proposals have exceeded the number of days available—in several cases by a factor of 2.5 or more. However, NCNR staff and the PAC are able to accommodate a good percentage of the proposals by juggling the amount of time given to each research team, and when the subpanel spoke with the chair of the PAC, it was agreed that, while the instruments were fully used, and some worthwhile proposals were not getting as much time as they perhaps deserved, overall the proposal pressure was not unbearable. A past concern of the subpanel, NCNR management, and the PAC itself has been the rising number of proposals that the PAC must review. (This growth is due in part to the increasing number of instruments, and time on those instruments, open to users.) A few years ago, the PAC began offering users the option of an alternative proposal mechanism. Instead of a proposal for a certain number of days for a certain project within the standard 6-month time period, experienced, heavy users of the facility could submit a program proposal to cover a series of related experiments over a 2-year period. This approach has worked well, and the PAC continues to improve on it. For example, the PAC is looking back at the first round of program grant awardees to check the level of output (i.e., publications) to ensure that good use is being made of the beam time, and the PAC is looking forward to preparing for

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 the second round of program proposals by defining more clearly who may apply for these grants and by adjusting the criteria for the awards and making the criteria uniform across the instruments. The PAC has managed to adjust well to changing circumstances, and the subpanel notes that in addition to the increasing number of proposals the PAC will also soon be facing changes in the types of proposals received, as NCNR’s emphasis on biological applications of neutron science expands. New instruments and new uses for existing instruments will arise. The expertise on the PAC will have to evolve to allow the PAC to deal effectively with all these changes. The subpanel suggests that the PAC and NCNR might consider instituting formal terms of service for PAC members (so, for example, the PAC would consist of a team of people serving staggered 3-year terms). This approach would allow members to understand the length of the commitment they are making to the NCNR and would enable the expertise of the membership to be adjusted to reflect new priorities and directions at the center. Resources Funding sources for the NIST Center for Neutron Research are shown in Table 6.6. As of January 2002, staffing for NCNR included 90 full-time permanent positions, of which 83 were for technical professionals. There were also 18 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers. NCNR continues to accomplish an amazing amount with very little money compared with the budgets of, for example, DOE user facilities. NCNR is run in a highly cost-effective and efficient manner. A key element of its success despite limited fiscal resources is the effective leveraging of funds. The NCNR’s long-term relationship with NSF continues to bear fruit; CHRNS has been expanded, and work on a new instrument, a multi-analyzer crystal spectrometer (MACS), is under way with NSF and Johns Hopkins University. The CNBT, discussed above, involves five universities and TABLE 6.6 Sources of Funding for the NIST Center for Neutron Research (in millions of dollars), FY 1999 to FY 2002 Source of Funding Fiscal Year 1999 (actual) Fiscal Year 2000 (actual) Fiscal Year 2001 (actual) Fiscal Year 2002 (estimated) NIST-STRS, excluding Competence 14.5 15.9 15.5 15.6 Competence 0.2 0.2 0.1 0.1 ATP 0.3 0.3 0.3 0.0 OA/NFG/CRADA 1.6 1.9 2.7 1.6 Other Reimbursable 0.2 0.2 0.1 0.2 Totala 16.8 18.5 18.8 17.6 Full-time permanent staff (total)b 85 85 92 90 NOTE: Sources of funding are as described in the note accompanying Table 6.1. aTotals for NCNR include only normal operation costs. Fuel cycle and upgrade costs associated with the reactor, totaling approximately $6.8 million in FY 2002, are excluded. bThe number of full-time permanent staff is as of January of that fiscal year.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 NIH. An agreement is in place with Brookhaven National Laboratory for a long-term alliance to support work on new magnetic and ferromagnetic materials. All of these partnerships bring funding and expertise to NCNR. The subpanel is pleased to see that support for reactor operations and engineering continues at all levels of management above NCNR (in the Materials Science and Engineering Laboratory, in the NIST director’s office, and at the Department of Commerce). This support has been critical for the safe and productive operation of the research reactor, and it is to be commended. A strong and healthy internal science program is a vital element of the vibrant research atmosphere that exists at NCNR. Unfortunately, funding for the science activities has been squeezed over the past several years, as the priority is always (and appropriately) maintaining the reactor, and then the instruments, in good operating condition. Thus, the $6 million neutron science initiative in NIST’s FY 2003 Presidential Budget is critical. This new funding would go toward instrument operation, user support, and, most importantly, science. While not entirely dedicated to science at NCNR (it would also support relevant materials science, physics, and chemistry research in other NIST laboratories), this funding would be a great opportunity to strengthen the science activities of NCNR’s condensed-matter science teams. It would also provide the freedom to move in new strategic directions, that is, to add new inhouse expertise in biology. A strong and diverse intramural science program is critical to driving creative instrument development and to effectively serving a vigorous user community drawn from a wide range of scientific fields. One of the primary drivers for expanding the support of the science programs at NCNR is ensuring that the NCNR scientists are not overwhelmed by routine user-support tasks. It is vital for staff to have time to perform their own research and to reach out to research communities. Such outreach builds awareness of the applicability of neutron science techniques to a variety of scientific problems, keeps staff informed of new developments in their own fields, and allows NCNR to build a reputation that will assist it in recruiting postdoctoral research associates and permanent staff. Communication with people outside NIST who do neutron research must be supplemented by contact with people from the broader communities that benefit from the results of NCNR users’ research. These interactions will help NCNR staff to understand and describe the motivation and context for their work, the applications enabled, and the important and interesting scientific questions tackled. A formal and active visitors program might be one approach to bringing in new expertise or perspectives (such as in theory or biology) that are not available on a permanent basis at NCNR. Another key element of external interactions is access to expertise or equipment not available on-site. Research is almost always strengthened by looking at a problem from a different perspective or with a different tool. For example, in the surface and interfacial science area, neutron reflectivity is a powerful approach, but complementary x-ray reflectivity measurements of a given sample often provide useful added information. While such x-ray experiments typically have required access to a synchrotron facility, in fact adequate measurements can be made with properly instrumented laboratory x-ray sources. The recent acquisition of an x-ray reflectivity instrument located on the NIST campus in the Materials Building (235) will thus be helpful to the NCNR staff and to users performing reflectivity measurements. This is just one example of the potential synergies between NCNR and the expertise, projects, and facilities available throughout the rest of NIST. Other facilities that might productively be shared include nuclear magnetic resonance spectrometers; other expertise that might be tapped includes theoretical and modeling capabilities. While NCNR is physically somewhat isolated from the rest of the NIST campus, shared equipment or cohosted talks might provide the basis of some productive, long-term relationships. Access to theoretical expertise for NCNR internal science projects has been an ongoing point of

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 concern for this subpanel. Currently, NCNR is obtaining some input in this area and does have ongoing modeling and simulation work, but the subpanel continues to believe that NCNR’s programs would benefit from increased theoretical input. Theory can provide new or different perspectives on existing problems and can be a source of new problems or topics to explore. Theoretical expertise can be brought to NCNR in a number of ways. As mentioned above, one is collaborations or interactions with theorists from other NIST units. A second possibility is a visitors program, although this approach works best when there is a theorist on the permanent staff who can help the visitor connect with the appropriate NCNR staff or if there is a preexisting collaboration between the visitor and NCNR experimentalists. A third possible approach is hiring a person who does both theoretical and experimental work, and a fourth option is hiring an experimentalist who has a history of attracting theorists (as visiting scientists or collaborators) for his or her work. Staff morale is high at NCNR. Personnel recognize the unique role they play in maintaining the field of neutron science at a healthy level in the United States, and they are justifiably proud of the quality of the reactor, instruments, and science that together make up this outstanding facility. With the construction of the SNS under way, recruitment of some of the NCNR staff to this facility has begun, though only a few people have elected to go to the SNS. NCNR management has expressed the view that training both users and (a few) employees for this large new facility is part of NCNR’s responsibility to the neutron community. Each year, the subpanel comments that three of the four most senior managers at NCNR will shortly be or already are eligible for retirement. NCNR is to be commended for recognizing the situation, for having a succession plan in place, and for preparing to manage the transition. Such a transition, even with training and careful preparation, will not be easy. Changes in management style plus long periods of time with “acting” leaders (given government’s slow process for new hires or promotions) have the potential to make the next several years a stressful time for NCNR. The transition plan and process will deserve close attention by MSEL and NIST management, and the subpanel believes that all parties recognize this need. The subpanel also notes that transitions and change, while potentially sources of tension and stress, can also be times of great opportunity, and the next few years will also give NCNR a chance to consider new focus areas and to move in new directions. The issues related to succession planning and training are particularly critical in the reactor operations area. NCNR has enjoyed a long period of very low staff turnover in this area, which has undoubtedly been an important factor in the high reliability and safety of the reactor operation. Recently, however, the number of personnel retiring has increased, and replacements have had to be recruited. The U.S. Navy continues to be a source of highly qualified operations and maintenance personnel, but recruiting and retaining management and engineering personnel of the same high caliber as those who may be retiring could become a problem in the near future; with the dwindling number of U.S. research reactors has come a sharp reduction in the pool of experienced managers and engineers who will be available. Although NIST still has a recruiting advantage (owing to a desirable, semiurban location and the opportunity to work with the cutting-edge technology used at this facility), succession planning and searches for qualified candidates should continue to be conducted well in advance of anticipated vacancies. Space continues to be tight at NCNR, although progress on this issue is being made. The addition to the building has been completed. Office and laboratory space is being reorganized to take advantage of this new space and to make on-site laboratory support available for users. As noted earlier, plans are being made to add wet-laboratory capabilities to support biological experiments. Site security became a high-visibility concern after September 11, added precautions were taken in the fall of 2001. If more security measures are required, NCNR might consider looking at approaches

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 used at other government and industrial laboratories to control site access (e.g., computer tracking of visitors at Brookhaven National Laboratory or photo identification cards for visitors as used in industry and at NIH). The subpanel strongly believes that security is the responsibility of the federal government as a whole, and additional money should be allocated to NCNR to fund new security measures. Responsiveness The subpanel believes that NCNR has been responsive to comments and suggestions provided in past assessment reports. Most of the issues raised in these reports are long-term, and the subpanel looks for annual progress rather than complete resolution. For example, succession planning and the training of future leaders are serious tasks at NCNR, given the demographics of the current management personnel and of the staff in reactor operations. Each year, the subpanel observes that work continues on this difficult front, and it is pleased to see that NCNR, MSEL, and NIST management all recognize the importance of this task. Another concern of the subpanel is that scientific staff be able to balance time spent on routine support of users with research and instrument development projects. In response, NCNR is investigating ways to automate tasks and hire technicians dedicated to user support. The neutron science initiative proposed in the FY 2003 budget, if funded, will provide an important opportunity to strengthen the science programs at NCNR and expand in new directions. Other examples of positive changes at NCNR reflect NCNR’s responsiveness not only to the subpanel but also to the facility’s user community. Improvements in the data reduction and analysis software available to users, improvements in the support of ancillary instrument equipment, and improvements in the proposal process all responded to concerns expressed by the subpanel and the users and should, therefore, be commended. Major Observations The subpanel presents the following major observations: The NIST Center for Neutron Research is an essential national user facility with high-quality science, instruments, and reactor operations. Each of these elements is critical to NCNR’s success, and plans to bolster the internal science programs with new funds and hires should receive support. NCNR management and staff do not rest on past accomplishments but are dedicated to continual improvement of the facility. New instruments are developed and old ones enhanced. The relatively young cold neutron source was replaced with a new and better version, and a new scientific focus on biology was launched. The dedication of the staff to effectively serving NCNR’s users is impressive. Decisions about instrument development take into account the eventual construction of the SNS, and plans are made with the short-term goal of training and maintaining a robust U.S. neutron science user community for the SNS and the long-term goal of providing critical complementary capabilities once the SNS is operating. Reactor operations continue to be first-class. During the recent extended shutdown, the time was used effectively to accomplish several major, complex repairs and improvements. The subpanel is also pleased to note that relicensing plans are on track.