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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 2001 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 2001 PANEL MEMBERS James Economy, University of Illinois, Chair David W.Johnson, Jr., Agere Systems, Vice Chair Dawn A.Bonnell, University of Pennsylvania Karla Y.Carichner, Conexant, Inc. Stephen Z.D.Cheng, University of Akron Michael J.Cima, Massachusetts Institute of Technology F.W.Gordon Fearon, Dow Corning Corporation Katharine G.Frase, IBM Microelectronics Division Sylvia M.Johnson, NASA-Ames Research Center Rodney A.McKee, Oak Ridge National Laboratory 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 2001 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 15–16, 2001, in Gaithersburg, Md., and documents provided by the laboratory.1 1   Department of Commerce, Technology Administration, National Institute of Standards and Technology, Ceramics Division: FY2000 Programs and Accomplishments, NISTIR 6594, National Institute of Standards and Technology, Gaithersburg, Md., January 2001. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Materials Reliability Division: FY2000 Programs and Accomplishments, NISTIR 6595, National Institute of Standards and Technology, Gaithersburg, Md., January 2001. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Polymers Division: FY2000 Programs and Accomplishments, NISTIR 6596, National Institute of Standards and Technology, Gaithersburg, Md., January 2001. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Metallurgy Division: FY2000 Programs and Accomplishments, NISTIR 6597, National Institute of Standards and Technology, Gaithersburg, Md., January 2001.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 LABORATORY-LEVEL REVIEW Technical Merit According to laboratory documentation, the mission of the Materials Science and Engineering Laboratory (MSEL) is to help U.S. industry improve the quality, reliability, and manufacturability of materials and the products made from them by developing and maintaining measurement tools, standard test methods, standard reference materials, and evaluated data on material properties. The MSEL is organized into five divisions: Ceramics, Materials Reliability, Polymers, Metallurgy, and Neutron Research (see Figure 6.1). The report of a special subpanel reviewing the last division is attached at the end of this chapter. The main body of this chapter is concerned with the review of the Ceramics, Materials Reliability, Polymers, and Metallurgy Divisions. The overall technical merit of ongoing programs in the MSEL remains high. The panel is consistently impressed by the quality of the MSEL staff and their knowledge of their fields. With few exceptions, projects under way at the MSEL are of high technical merit relative to the state of the art. Detailed reviews of the programs can be found in the divisional reports below. Program Relevance and Effectiveness The MSEL clearly has many ties to its customers in industry and other sectors. It regularly seeks customer input into new program directions through mechanisms such as workshops, consortia, and participation in industry roadmapping efforts. The results of programs are generally well disseminated to specific customers, and MSEL’s use of the World Wide Web to disseminate results continues to increase and improve. 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 units.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 Despite clear goals and customers for individual MSEL projects, the panel was not able to discern how those projects fit in to an overall MSEL plan. The panel believes that opportunities for synergies resulting in increased customer impact exist within current programs. The panel suggests clearer articulation of laboratory-wide goals and vision. This would help individual researchers to place their work in the greater context of the laboratory and focus their projects more tightly against larger objectives. The laboratory would then be better positioned to have a major positive effort on measurements and standards roadblocks facing its customers. It would also make it easier for MSEL stakeholders to understand the value of the laboratory’s efforts, their potential impact, and the critical national needs that they meet. Laboratory Resources Funding sources for the Materials Science and Engineering Laboratory are shown in Table 6.1. As of January 2001, staffing for the Materials Science and Engineering Laboratory included 163 full-time TABLE 6.1 Sources of Funding for the Materials Science and Engineering Laboratory (in millions of dollars), FY 1998 to FY 2001 Source of Funding Fiscal Year 1998 (actual) Fiscal Year 1999 (actual) Fiscal Year 2000 (actual) Fiscal Year 2001 (estimated) NIST-STRS, excluding Competence 30.9 30.6 30.1 30.6 Competence 0.0 0.3 0.1 0.4 ATP 3.0 2.5 2.7 1.9 Measurement Services (SRM production) 0.7 0.9 0.7 0.6 OA/NFG/CRADA 4.9 3.8 3.9 4.0 Other Reimbursable 0.2 0.2 0.6 0.5 Totala 39.7 38.3 38.1 38.0 Full-time permanent staff (total)b,c 209 199 178 163 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 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 2001 permanent positions, of which 135 were for technical professionals. There were also 40 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers. The laboratory’s budget, when inflation and cost-of-living salary increases are taken into account, has been slowly but steadily declining for a number of years. The laboratory has done an admirable job of operating under these circumstances, making tough decisions on program prioritization and utilizing guest researchers and term employees to obtain critical skills where permanent hires are not possible. However, the panel is very concerned at the effect that the declining budget has had on MSEL staffing. The laboratory director presented data that showed the number of staff decreased from 359 full-time equivalents (FTE) to 306 FTE between 1995 and 2000. In the short term, this decrease in staff has been effectively dealt with (see preceding paragraph), but in the longer term, the situation will not allow the laboratory to remain a healthy research organization. Long-term effects of this situation include loss of critical mass in key areas, complete loss of competence in other key areas, and loss of the corporate memory necessary to reconstitute lost programs should new need arise. For example, the laboratory has a considerable stock of SRMs for polyethylene production and characterization. But when this stock is depleted, it will no longer have the staff skills in processing and synthesis required to produce more SRMs, much less to develop enhanced ones. Prioritization has shifted the focus of much of the laboratory’s work to newer and emerging technologies, such as microelectronics. While this shift seems appropriate to the panel given the resource restraints, it threatens the nation’s competence in more mundane but important areas such as the characterization of structural damage in massive pipelines. These choices have been forced upon the laboratory in times of unprecedented national prosperity. The panel is very concerned about how the laboratory will fare in an economic downturn and questions which capabilities critical to our economy will be lost in that scenario. The laboratory has also been forced to make difficult trade-offs between capital equipment upgrades and hiring or retention of staff, almost always choosing staffing over equipment. However, the panel wishes to point out that staff can be more effective and productive with reliable and up-to-date equipment. Thus, putting some funds into capital equipment rather than staff can effectively increase the number of FTEs available to work on research problems. More specific concerns about resources can be found in the divisional reports that follow. 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 the leadership for the nation’s measurements and standards infrastructure for ceramic materials. The division is organized into six groups: Ceramic Manufacturing, Phase Equilibria, Film Characterization and Properties, Materials Microstructural Characterization, Surface Properties, and Data Technologies. The Ceramics Division underwent significant reorganization in the last year, resulting in the distribution of its mechanical properties activities among the relevant research areas and the organization of division activities around cross-group and cross-division programs. These programs are more closely tied to technology areas and therefore to customers. The panel believes that this focus will create stronger links between fundamental science and technical need, will facilitate interactions with the industrial customer base, will increase the overall impact of division activities, and will be a positive

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 force in the evolution of research activities and standards development. The size of the division decreased by about 11 percent in the past year owing to retirements and relocations. The resulting restaffing opportunity gives the division a chance to think about how it will position itself to continue its leadership role in the area of ceramics. As part of an interdivisional program to address materials measurements and standards issues relevant to the microelectronics industry, the Ceramics Division is carrying out research on texture quantification of thin-film microstructures, on domain stability measurements in ferroelectric films, and on processing and characterization of ultrathin oxide films. These programs are based on input from an industrial advisory panel that rated recent progress in these areas as excellent and was pleased with the relevance of the division’s efforts. A highlight of recent work is progress in texture measurements, which is relevant because the properties and performance of electronic devices can be strongly dependent upon the texture of the various material layers they are composed of. An October 2000 workshop sponsored by NIST indicated a strong need for texture standards. As a result, the division is organizing a round-robin measurement activity that will compare texture measurements obtained on the same samples using different techniques, and using the same techniques but different apparatuses. This is a first step toward understanding specific standards requirements in this area. Theoretical and experimental studies of phase equilibria are traditional strengths of the division that are now being applied to nontraditional materials related to computing and telecommunications, with good results. For example, the Ceramics Division’s decision to direct efforts toward dielectric ceramics for wireless communications has had results. The electronics and wireless communication industries depend on decreasing component size and integration to achieve miniaturization. Low-loss, high-dielectric-constant materials with very well controlled expansion and dielectric coefficients are important for resonators and other high-frequency components. The industry meets the material requirements for these components by preparing ceramic composites with many additives. The phase equilibria are complex and are very important because they define the appropriate firing conditions for the desired phase assembly. This program is exploiting the insight that first-principles computational methods can bring to guide experiments and to propose previously unreported structures with unusual properties. The group has assembled a team of theoreticians who are working with experimentalists on materials problems for the wireless industry. Phase diagram work enables the development of new and improved materials by providing an understanding of the conditions under which specific compositions form and why they have particular properties. The division has shown remarkable depth in its analysis of Ca-Al-Nb-O systems, for example, elucidating differences in dielectric behaviors and in electronic structure between species. Other materials under study for the wireless industry include candidate materials for high-frequency base station resonators. The Ceramics Division is also pursuing phase equilibria studies for the manufacture of high-temperature superconducting wires. Earlier division work on Bi-Sr-Ca-Cu-O (BSCCO) conductors yielded critical results for the current generation of high-Tc wires. The next generation wires will be “coated” conductors based on Ba2YCu3O6.9. This past year the group began a series of experiments on phase equilibria in the BaO-BaF2-CuO-Y2O3 system. This study is relevant since the two primary domestic industrial efforts will use reactions in this system to manufacture coated conductors. Ceramics coatings research focuses on thermal barrier coatings (TBCs). Life prediction, an important element of this research, is an important goal for the industry. Because the service life of these coatings cannot yet be accurately predicted, their use in turbine engines is currently limited to the safe operating temperature of the underlying metallic turbine component. At present, therefore, TBCs only lengthen the useful operating life of the component, they do not enable higher engine temperatures. The division has been developing standard test methods and instruments such as instrumented indentation and photoluminescence spectroscopy for in situ coating stress measurements. The division is also

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 developing structure-based prediction tools, including some based on the MSEL object-oriented finiteelement (OOF) analysis software tool. Indeed, the coatings program has been an important vehicle for evaluating OOF. The relationship between thermal conductivity and the microstructure of coatings has been demonstrated by comparing OOF predictions with data. The division will extend this analysis to the fracture behavior of coatings, an important step toward their life prediction. The group is also expanding its research to include wear coatings, which face problems similar to those of TBCs. In the ceramics manufacturing program, division researchers have identified the primary issues surrounding the characterization of powder size in nanosized powders: absolute measures of particle size and distribution are lacking, and available instruments yield different results. However, the division does not seem to have clearly identified the next step in this project. Research in machining damage to ceramics materials has expanded into contact reliability of the finished part. These efforts are examining damage to ceramics in diesel engine applications. Many of the fundamental technical issues that affect the successful machining of these materials have been identified. The division hopes to obtain further focus in these areas from a planned industrial workshop on the characterization of nano-powders and machining damage. In general, the ceramics manufacturing program could benefit from a clearer vision and a clearer statement of its role and its planned contributions to the overall program goals of providing techniques and standards to industry. Industrial input to this program has been obtained from the Ceramic Processing and Characterization Council (CPCC) and the Ceramic Machining Consortium (CMC). The CPCC is being reorganized, and the CMC is terminating in the fall of 2001, as planned. These two events may result in less industrial input for the ceramics machining program. The panel feels the division must compensate for that loss by, for example, establishing an industry advisory panel similar to that used in microelectronics. In the past year the ceramics machining program added several staff members who formerly worked on mechanical properties research. Division management must complete integration of this program, taking into account the new researchers; set clear program priorities, as the program encompasses many aspects of ceramic manufacturing; and establish specific, industrially relevant goals for projects. The panel endorses the efforts of the division in the past year to address these issues and encourages continued progress. A project that the Ceramics Division is calling nanotribology is currently working on the durability of magnetic hard disks. It is examining the interfacial phenomena that lead to damage when the magnetic recording head contacts the disk. A new measurement technique that utilizes acoustic emission of scratching is being evaluated for its usefulness in examining the effect of speed on this contact damage. NMR and electron spin resonance (ESR) are being utilized to examine the atomic bonding of surface layers. The MSEL sponsored a workshop entitled “Nanotribology: Critical Assessment and Research Needs,” which attracted about 120 participants from industry, academe, and government. The purpose was to identify a number of broader issues of friction, wear, adhesion, and lubrication at the nanoscale. The division does not currently address these issues, so in this sense its project is misnamed. However, given NIST’s core competencies, there is an unrealized potential to make a major impact in nanotribology. The division is exploring opportunities for collaborations with laboratories that are working on force measurements, device scale measurements, micromanipulation techniques, AFM calibration standards, and other relevant techniques. The NIST fellows whose work falls within the purview of the Ceramics Division provide extraordinary technical expertise in ceramic technology, especially mechanical behavior and characterization. Highlights of their work include new approaches to dental restoration materials, understanding of the creep behavior of improved silicon nitride, and a fundamental understanding of the wetting and dewetting of grain boundaries in alumina. Although the fellows are not formally associated with the Ceramics

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 Division, their work is commonly connected to it, and their presence raises the prestige of the division in the broader community. The panel identified several areas where a closer collaboration between the fellows and the staff members would be fruitful, including nanotribology, aspects of ceramic machining and contact stresses in ceramics, and the development of mechanistic models. The fellows could provide both technical direction and mentoring of staff. Program Relevance and Effectiveness The term “ceramics” as used by the division includes nonoxides and encompasses films, coatings, multilayers, nanoparticles, and single crystals. This is completely in line with technological developments and is appropriate given NIST’s customer base. Although the impact of NIST contributions to industry is often difficult to quantify, some examples are provided below. The NIST Recommended Practice Guide, Particle Size Characterization2 is a good example of an outcome of demonstrated importance to industry. A large raw material producer has expressed interest in providing this guide to its customers so that they can compare size results in cases of significant discrepancies between the producer and customer. Phase diagram work provides guidance to the wireless communication industry for the development of materials with better properties or lower cost and may eventually enable the prediction of properties and the intelligent design of new materials. The effort is guided by collaborative work with industry and academia. The program has carried out basic research that aims for solutions to practical problems. Industrial collaborations have provided sharpened program focus and found end users for the results. One example of a successful program is the identification of two low-loss high dielectric constant phases in the CaO-Al2O3-Nb2O5 system that are in equilibrium at high temperature and that have opposite temperature coefficients. This can enable the manufacture of composites that have the desired overall temperature coefficients for use in dielectric resonators. In general, this effort is an excellent example of how basic research can have a direct impact on industrial applications. Researchers throughout the world are very closely following the Ceramic Division’s high-Tc phase relationship studies, as the technology for the next generation of superconducting wire is developing very rapidly. Talks presented by NIST staff are routinely some of the best attended at technical conferences on superconductivity. The data evaluation and delivery program is a clear example of an excellent program fulfilling the mission of NIST. The division has combined phase equilibria and crystal structure data in a Web-accessible document, the Ceramics WebBook.3 This results in wide dissemination of the material (the Ceramics WebBook is the eleventh most accessed Web site at NIST). The Ceramics Division actively publishes in the most prestigious journals and presents results at many conferences. Staff are also the key organizers of workshops, including—in the past year— workshops on the use of first-principle calculations for predicting physical properties and phase dia- 2   U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, NIST Recommended Practice Guide, Particle Size Characterization, NIST SP 960–1, National Institute of Standards and Technology, Gaithersburg, Md., 2000. 3   The Ceramics WebBook is available online at <http://www.ceramics.nist.gov/webbook/webbook.htm>.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 TABLE 6.2 Sources of Funding for the Ceramics Division (in millions of dollars), FY 1998 to FY 2001 Source of Funding Fiscal Year 1998 (actual) Fiscal Year 1999 (actual) Fiscal Year 2000 (actual) Fiscal Year 2001 (estimated) NIST-STRS, excluding Competence 9.3 9.4 9.2 9.5 Competence 0.0 0.0 0.0 0.1 ATP 0.7 0.7 0.8 0.6 Measurement Services 0.2 0.3 0.2   (SRM production)   0.2   OA/NFG/CRADA 1.3 1.2 1.5 1.3 Other Reimbursable 0.1 0.1 0.2 0.2 Total 11.6 11.7 11.9 11.9 Full-time permanent staff (total)a 62 59 57 51 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. grams. Staff members continue to be recognized by being presented with external awards, including— again, in the past year—the election of a staff member to the National Academy of Engineering and the awarding of the American Physical Society’s Maria Gepphart Mayer Distinguished Scholar Award to another staff member. Division Resources Funding sources for the Ceramics Division are shown in Table 6.2. As of January 2001, staffing for the Ceramics Division included 51 full-time permanent positions, of which 43 were for technical professionals. There were also 6 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers. It is clear that the flat funding of the Ceramics Division has a negative impact on the ability of the division to address its mission. Flat funding and mandatory cost-of-living increases to staff have led to an overall decrease in the number of permanent staff and an increasing reliance on temporary employees (postdoctoral and visiting researchers). While the division chief has managed to minimize the impact to date, an extension of this flat-funding trend will have a negative outcome in terms of performance and output. Materials Reliability Division Technical Merit The Materials Reliability Division states that its mission is to develop and disseminate measurement methods and standards enhancing the quality and reliability of materials and provide technical leader-

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 ship in their introduction to appropriate industries. The division is organized into three groups: Microscale Measurements, Microstructure Sensing, and Process Sensing and Modeling. The Materials Reliability Division has expanded its programs to include the electronic materials industry while continuing in several key infrastructure support efforts. The Microscale Measurements Group is working on measurement techniques for evaluating the mechanical, thermal, electrical, and magnetic behavior of thin films and coatings. Projects focus on the smaller size scales relevant to features of electronic chips and packaging. They are investigating reliability issues such as thermomechanical effects, particularly at interfaces; new materials such as damascene copper, lead-free solders, and exotic dielectrics; and size scales below 1 μ. The Microstructure Sensing Group applies ultrasonic measurements to the characterization of materials on size scales ranging from atomic dimensions through microstructures to macrostructures, with the aim of predicting material performance. Its projects currently focus on the elastic properties of thin films and bulk materials and the study of internal friction. The Process Sensing and Modeling Group develops measurement technology for determining material characteristics and for implementing process control. Projects currently focus on characterizing materials using x rays, the characterization and control of traditional and new joining technologies (welding, soldering), and the development of standard reference materials (Charpy impact testing, ferrite). The Materials Reliability Division has an opportunity to become the leader in each of the three areas in which it has a group. Emerging technologies such as optoelectronics reliability and materials assessment require significant background information and multidisciplinary study. The division is in a strong position to capitalize on the diverse talents of its staff and their relationship with other NIST laboratories to provide the basic measurements and standards guidance needed in these areas. Despite considerable budget challenges the division continues to combine development of state-of-the-art testing methods with unique and creative approaches to sample preparation and handling and equipment. The results are impressive. Two outstanding examples are provided below. The division has modified existing equipment to perform ground-breaking ultrasonic measurements of the mechanical properties of thin films. Electromagnetic-acoustic transducer techniques have been used to measure the dispersion produced by 10- to 20-μ-thick electroplated films on aluminum. An acoustic microscope is being modified to rapidly determine signal versus distance between part being probed and the acoustic transducer. This can be used to deduce the elastic modulus of films 1 to 10 μ thick. Finally, an atomic force microscope was modified to permit measurements of the cantilever’s resonant frequency as a function between the tip and the sample surface. This measurement can be related to the Young’s modulus of the surface to produce a two-dimensional map of the sample surface with nanoscale resolution. The Materials Reliability Division has developed high-energy x-ray diffraction techniques to probe intermetallic interfaces in solder joints. Conventional scanning electron microscopy (SEM) techniques have a limited penetration depth, requiring a solder joint to be cross-sectioned in order to be examined. The division used a high-voltage industrial x-ray tube with a tungsten target to perform x-ray diffraction studies of these joints. This extended the penetration depth from the micrometer to the millimeter range. Work continues on refining this technique and interpreting the complex diffraction patterns that result. Program Relevance and Effectiveness The panel concurs with the decision of division management to focus on issues relevant to the semiconductor, computing, and telecommunications industries. The development of measurement techniques and standards is key to the success of both existing and newly emerging markets in these

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 industries. With its expertise, NIST has the opportunity to drive developments in these sectors. However, although newer industries such as microelectronics have a strong need for new measurement techniques and standards, several key traditional industries depend on the division as their main and sometimes sole resource for materials information. For example, the Materials Reliability Division has the only capability in the nation to determine the structural integrity of major pipelines. The division must carefully balance its programs between new and traditional industries. Because of its recent change in focus, the division must engage in strategic planning to determine how it can build on its existing strengths to impact these new areas of application. The panel strongly believes that the division should provide leadership in future standards for these industries. Current projects must be chosen carefully to provide a base from which to lead in standards. To do this successfully, the division must be tightly connected to the relevant industries. A well-rounded understanding of industry’s directions and the support it needs for both new and old products is required if the division is to appropriately drive standards development. Having a clear strategic plan and communicating it to customers along with the overall issues addressed, corresponding projects, and planned impact, will give the division the type of industry feedback it needs to be successful. Division staff members face the challenge of making their work known to an entirely new community. The traditional industries served by the Materials Reliability Division are familiar with the NIST laboratories and the division’s contributions. The new industries that the division seeks to reach need a succinct introduction to the division’s work. Industry partners and membership in appropriate industrial organizations are good starts to this introduction. Group leaders and many of the staff are members of such organizations. Moreover, a large percentage of the projects the panel reviewed were linked to industrial customers, many of which are large organizations with strong leadership in the industry (e.g., IBM, Motorola, and Intel). Contact with smaller advanced companies can aid in providing direction and should not be overlooked. Communication with industry must occur at all levels of the division hierarchy. Each staff member is a potential ambassador for the division. The division has been successful at getting its current results into the hands of customers. However, more effort on communications with customers would increase the impact of the division. Division management should focus on succinctly communicating the division’s mission and strategy. A part-time consultant assisting in communications might be a creative use of resources. Division Resources Funding sources for the Materials Reliability Division are shown in Table 6.3. As of January 2001, staffing for the Materials Reliability Division included 20 full-time permanent positions, of which 18 were for technical professionals. There was also 1 nonpermanent or supplemental personnel, such as a postdoctoral research associate or a temporary or part-time worker. The panel was impressed with the high quality of the division staff. Staff members have pursued new techniques and equipment to successfully apply their skills and knowledge to new areas of materials and measurement methods. One measure of the quality of the staff is the number of patents (3) and publications (90) produced by the division in the past year. The panel could also clearly see the staff’s enthusiasm for its work. In general, staff members see the division’s new direction as an exciting opportunity to study and contribute to new technologies. A NIST-wide employee survey taken in 2000 confirms high morale, job satisfaction, and satisfaction with the performance of the division’s supervisors. While the current staff is very impressive, increased staffing is necessary to achieve long-term vitality in current program directions. The division is in a critical phase of its changeover to a new customer base. Resources must be and are being spent to learn about these customers. However, each

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 For the second year in a row, the panel is calling attention to the need for a new transmission electron microscope. This will need to be a special budget item, as the normal procedure—whereby capital spending is a portion of the base budget and capital dollars may not be carried over from year to year— will never provide sufficient funding for this type of tool. The base budget will also need to be adjusted to accommodate the depreciation of such a tool. Ironically, because of the declining budget, the management team is not anxious to acquire better tools in the laboratories, despite their ability to bring new technical advances and improve the productivity of the staff: Indeed, it is concerned that depreciation would further strain division budgets and probably lead to additional reductions in staff! Financial constraints certainly affect the types of projects the Metallurgy Division can undertake. The management team has done an excellent job of using these constraints to ensure that each program has focus, relevance, and appropriate resources and to ensure that the portfolio of projects is optimized. However, if staff attrition continues, there is a very real risk that the permanent staff will become too small or too narrow in the scope of their expertise to sustain the division’s mission. MAJOR OBSERVATIONS The work of the Materials Science and Engineering Laboratory is of high technical merit and is well recognized externally. Laboratory managers understand that to maintain forefront work on metrology, they must foster the basic science that underlies this metrology. Laboratory researchers are well coupled to their customers through industry groups; however, the panel suggests clearer articulation of laboratory-wide goals and vision. This would help individual researchers to place their work in the greater context of the laboratory and focus their projects more tightly against larger objectives. The level of morale at the laboratory is quite high. Researchers report that they derive job satisfaction from a work environment that allows them to be productive. Declining resources and the reduction of permanent staff put at risk some of the MSEL’s core competencies and its ability to delve into new program areas with the needed level of effort. While the laboratory has compensated effectively for the loss of permanent staff through use of postdoctoral and term employees and guest scientists, overreliance on temporary personnel can negatively affect the long-range capabilities of the laboratory. Restricted budgets have caused the laboratory to shift resources away from equipment purchase toward support of staff. However, the panel notes that leadership in measurement science demands cutting-edge equipment, and such equipment can enhance the productivity of current staff. The laboratory is effective in disseminating its program results. Particularly noteworthy is its initiative in publishing NIST recommended practice guides and its use of the Web for making program results readily available to the public. MSEL information distribution, both in published form and Web-based, provides an educational benefit to the nation. The laboratory reports encouraging feedback from educational institutions on how the information has made their teaching more effective. The panel was pleased to observe that the laboratory had implemented many of the recommendations from the previous review, such as an expansion of the dental program into the broader area of biomaterials, the expansion of work on the characterization of electronic materials and microstructure, and expanded use of the postdoctoral program.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 REVIEW OF THE NIST CENTER FOR NEUTRON RESEARCH This annual assessment of the activities of the NIST Center for Neutron Research (NCNR), part of the NIST Materials Science and Engineering Laboratory, is performed by the Subpanel for the NIST Center for Neutron Research. The report is based on site visits by individual subpanel members, a formal meeting of the subpanel on March 6–7, 2001, in Gaithersburg, Maryland, and documents provided by the NCNR.4 Members of the subpanel included Albert Narath, Sandia National Laboratories (retired), Chair; Zachary Fisk, Florida State University; Sol M. Gruner, Cornell University; Eric W.Kaler, University of Delaware; Charlotte K.Lowe-Ma, Ford Motor Company; and David C.Rorer, Brookhaven National Laboratory. Technical Merit According to NCNR documentation, the mission of the NCNR is to operate the NIST research reactor cost-effectively while assuring the safety of the staff and general public; to develop neutron measurement methods, to develop new applications for these methods, and to apply them to problems of national interest; and to operate the research facilities of the NCNR as a national facility serving researchers from industry, university, and government. It is the considered judgment of the subpanel that the NCNR continues to execute its mission responsibilities with exemplary effectiveness and to build on its outstanding record as a world-class neutron science facility. It provides valuable support to internal NIST research programs and also supports a very large and technically diverse external user community. The NCNR is organized into three units: Neutron Condensed Matter Science, Research Facilities Operations, and Reactor Operations and Engineering. Within the Neutron Condensed Matter Science unit, there are six groups: Chemical Physics of Materials, Surface and Interfacial Science, Macromolecular and Microstructure Science, Crystallography, Diffraction Applications, and Magnetism and Superconductivity. These groups are organized along scientific themes, but in addition to performing research, staff in the Neutron Condensed Matter Science unit are also responsible for instrument development and the support of user communities. Below the subpanel comments on the various activities under way in each of these groups, as well as on the NCNR’s effort to build a program in life sciences and on the status of the Research Facility Operations and Reactor Operations and Engineering units. The NCNR continues to support a broad spectrum of exciting scientific research. NCNR management and staff successfully apply an interdisciplinary approach to facility utilization, including collaborations with on-site visiting scientists as well as external scientists. Among other benefits, these collaborations have led to improved theoretical modeling and interpretive capabilities, thereby enhancing the significance of the experimental measurements. The value of past instrumentation development efforts is clearly demonstrated by the high-quality science and the many results published recently. The Chemical Physics of Materials Group develops, provides, and utilizes inelastic neutron-scattering methods for the study of atomic and molecular excitations in materials. Scientific projects under 4   U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, NIST Center for Neutron Research: FY 2000 Programs and Accomplishments, NISTIR 6598, National Institute of Standards and Technology, Gaithersburg, Md., February 2001.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 way include probing disorder in confined methyl iodide, investigating ligand dynamics in a manganesepyrazine complex, observing H2 adsorbed on carbon nanotubes, following dynamic changes in the molten globule-native folding step in α-lactalbumin, and determining the role of particle size during cement hydration. The results from the cement hydration study are particularly noteworthy and could have a significant impact on future processing procedures of a poorly understood but ubiquitous building material. In addition to the scientific projects, the group is also responsible for leading the operation and research programs on five neutron spectrometers: the high-flux backscattering spectrometer (HFBS), the neutron spin echo (NSE) spectrometer, the filter analyzer neutron spectrometer (FANS), the Fermi chopper time-of-flight spectrometer (FCS), and the disk chopper time-of-flight spectrometer (DCS). Most of these instruments are relatively new, and they are very effective scientific tools. The first user experiments on the HFBS occurred during 1999, and the very high intensity, the energy resolution, and the dynamic range of this instrument make it popular and useful. The NSE spectrometer was first made available to users in 2000, but improvements to its capabilities continue, with plans to put in a new area detector and a new polarization analyzer. Also in 2000, Phase I of the FANS was installed and commissioned, with the intensity having been improved by a factor of 20 compared with that available in the old spectrometer. Finally, while the FCS has been used since the early 1990s for the study of low-to medium-energy dynamics in materials, the first experiment utilizing the DCS, a newer time-of-flight spectrometer with greater flexibility in energy resolution and Q range, occurred in 2001. The Surface and Interfacial Science Group carries out a high-quality research program and provides a suite of state-of-the-art reflectivity instruments for users. Scientific projects include work in the areas of solid state physics and soft condensed matter science. In the first area, recent advances include the measurement of a novel interlayer coupling in magnetic semiconductor superlattices and the imaging of buried domain walls. Some examples of the significant work in the second area are the measurement of the exchange of surfactant molecules at a gold surface under the control of electrochemical potentials and the first measurements of polymer thin films in supercritical carbon dioxide. In a significant result that will improve data analysis techniques for reflectivity instruments users, the group has demonstrated, based on first principles, how to invert neutron reflectivity data to produce the scattering length density profile across a hybrid bilayer membrane. All of these activities provide clear evidence that the Surface and Interfacial Science group is functioning effectively at the forefront of its scientific field, but the group is also making contributions to other areas of interest at the NCNR. Many of the scientific questions tackled in this group are closely related to work under way in the Macromolecular and Microstructure Science Group, and some of the Surface and Interfacial Science group results feed directly into the growing activity around biological structure characterization. The scientific goal of the Macromolecular and Microstructure Science Group is to develop new methods to relate submicron structure and dynamics to bulk properties and function. This work is complemented by the staff support of NCNR’s collection of small-angle scattering instruments and of the large and vigorous collection of outside users of these instruments. This group has been highly successful in its research activities, its relationships with users, and its instrument-related work. High-quality scientific projects under way range from studies of complex fluids to polymer synthesis and phase morphology to examination of macromolecular conformation. The group’s accomplishments have been impressive, including several significant scientific firsts and the demonstration of the potential for development of a novel phase-contrast imaging method. The group also continues to provide advances in instrumentation and methods relevant to the macromolecular and microstructure sciences. For example, a continuing program of upgrades is under way on the NSE instrument, which has produced useful data this year. A significant milestone was the

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 recent introduction of the ultrasmall-angle scattering instrument to the user community. This instrument is a perfect crystal diffractometer that allows measurement of intensity at values of momentum transfer (Q) more than an order of magnitude lower than was previously possible. This new capability allows scientists to close the gap between the existing small-angle neutron scattering (SANS) instruments and static light scattering measurements and to measure structures up to nearly a micron in size. Application of this method to a range of hierarchical structures is likely to be particularly useful. In the Crystallography Group and the Diffraction Applications Group, research activities include internal staff investigations of fundamental questions, collaborative projects with other NIST scientists, and work on diffraction applications relevant to industry. Examples of these efforts include the examination of crystal structures of dielectric ceramics for wireless communications; the determination and analysis of structures of novel intermetallic and ruthenate superconductors as well as perovskite-like cuprate superconductors; the assistance provided on studies of magnetic spinels and giant and colossal magnetoresistant materials; structural studies of zeolite and molecular sieve materials; and the use of stress, texture, and elastic constants measurements to increase understanding of metal coatings and metallurgical issues. The technical work is interesting and of high quality, but the significance of some of the internal research projects within the Crystallography Group is not immediately obvious. The group might benefit from clarifying its intended impacts and developing a clearer vision for its future direction. The Diffraction Applications Group appears to have a reasonably clear vision of which difficult-materials-related questions are worth tackling and have a significant level of interest for industry. One particularly notable example is the effort to model, even at an empirical level, macroscopic materials features that could explain observed microscopic stress measurements. Overall, the panel expects that the diffraction applications projects will continue to benefit from continuing industrial liaisons; the use of complementary characterization techniques, such as optical metallography; planned work on finite element modeling; and external collaborations. The Crystallography Group and the Diffraction Applications Group are active in supporting and upgrading the NCNR diffraction instruments, the high-resolution powder diffractometer (BT-1), and the residual stress diffractometer (BT-8). These instruments are 9 and 5 years old, respectively, but are undergoing modifications and upgrades as appropriate. In the past year, the groups have improved the data collection capabilities of BT-1 and BT-8, enhanced NCNR capabilities for residual stress, texture, and elastic properties measurements, and continued development of user-friendly public-domain software for analyzing neutron data. This upgrading of older, more difficult software is useful for the NCNR users and others in the neutron community, and the groups’ efforts in this area have been reasonably well received by outsiders. The staff also continue to participate in international round-robins in which the diffraction-related capabilities of various laboratories are evaluated and compared. These activities are noteworthy efforts to clarify measurement and data interpretation issues. While this work is not particularly glamorous, it does fit well with the NIST mission and has value for the external community. Overall, the subpanel believes that the level of effort expended on these nonresearch activities, such as the standards- and software-related work, is appropriate. In the Magnetism and Superconductivity Group, research centers on the study of the structure and dynamics of strongly correlated complex materials. The primary tools are the triple-axis crystal spectrometers and the SANS instruments. Current investigations extend over a broad range of topics and address problems of fundamental scientific interest. In many projects, especially those studying magnetic thin films and layered materials, results have important technological implications for magnetic recording and other practical applications. Active collaborations are under way with numerous researchers drawn from university, industrial, and government laboratories.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 Recent accomplishments in the magnetism and superconductivity area demonstrate that the work at the NCNR is progressing at a commendable rate and making key contributions to elucidating the behavior of these complex materials. Examples of current projects include studies of magnetic phase transitions in frustrated spin systems, investigations of charge ordering and polaron formation in the prototype colossal magnetoresistive oxides (La1–xCax)MnO3, characterization of the structural and magnetic properties of double perovskite systems, and the first observations of a metastable, superheated vortex lattice and a supercooled vortex liquid. The NCNR does not have a specific team dedicated to life sciences research but instead is reaching out to partner with biologically oriented researchers elsewhere at NIST and with external scientists. The subpanel applauds the efforts to date. While there are a wealth of ways in which neutron techniques can be used to study biological systems, it will require a dedicated effort on the part of NCNR scientists to inform the relevant communities about these opportunities and stimulate the interest of life science researchers. The NCNR continues to publish good examples of the interesting scientific problems that can be tackled using neutron-based experimental methods, and the subpanel believes this is the best way to inform and convert the biological researchers. In collaboration with external scientists, NCNR staff are currently working on projects in three areas: (1) quasi-elastic scattering studies of macromolecular dynamics in order to investigate the folding of aqueous proteins, such as the details of the molten globule state of bovine α-lactalbumin, (2) SANS studies of the radius of gyration of proteins in solution, and (3) neutron reflectivity studies of the profile of adsorbed lipid layers with imbedded molecules, such as mellitin. All three areas have yielded significant scientific results. A particular example is the SANS studies, where data have indicated that there may be a disparity between the x-ray crystal structure and the solution structure of a nucleic acid-receptor/nucleic acid complex. However, a more careful follow-on SANS study of the complex identical to that used to determine the x-ray crystal structure is needed before the evidence can be considered compelling. All of the high-quality science and powerful instrumental tools described above depend on safe, effective operation of the reactor and research facilities. The subpanel continues to be impressed with the capabilities and accomplishments of the NCNR staff responsible for maintenance of the reactor and the development of important new components for the facility. The liquid hydrogen cold source, which provides beams of cold neutrons for the instruments in the main beam hall, continues to deliver outstanding performance at an unprecedented availability rate. Nonetheless, NCNR staff have begun in-house design and construction of an improved liquid hydrogen source, the advanced cold source. The new geometry of this source is expected to result in a 50 to 80 percent increase in the neutron flux at wavelengths of 0.02 to 1.0 nm. Fabricating this unique device has been an enormous challenge. Ellipsoidal parts have been machined out of solid blocks of aluminum using a state-of-the-art computer-controlled machine to achieve the necessary high precision. The next major hurdle was the quality assurance procedure required to guarantee leakproof welds during assembly of the nested ellipsoids inside a conical vacuum chamber. It is a credit to the patience, perseverance, and ingenuity of NIST staff that the design for the advanced cold source has successfully passed destructive-proof testing and that construction of the reactor-qualified device is now nearing completion. The reactor appears to be functioning well. In 2000, it operated for 198 days, 74 percent of the maximum practicable operating time (266 days, or seven cycles, out of a calendar year). The extra downtime mainly consisted of scheduled breaks to perform planned maintenance: six weeks for a scheduled replacement of the shim arms and five weeks for a management-ordered replacement of the graphitar bushings in the refueling plug. In addition, a one-week delay was purposely inserted before starting a cycle to maximize the uptime during a summer training session for new users of the facility. In addition to these planned breaks in operation, 17 other days were consumed by an unscheduled

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 extended shutdown that occurred so that staff could search for the source of a small amount of heavy water that was observed to have accumulated in the collection system of the thermal column facility. This water collected while the reactor was operating; however, during the 17-day shutdown and several subsequent operating cycles, no additional water was detected in the collection system and the source of the water observed earlier could not be pinpointed.5 Even from the time the original accumulation of heavy water was observed, it was clear that the water did not originate from the reactor itself and that it posed no danger. Nonetheless, the NCNR staff chose to conduct a prompt and painstaking investigation; this decision is evidence of the seriousness with which management takes its responsibility to run this facility safely and reliably. The emphasis on safety is also demonstrated by the continuing effective management of industrial safety and radiation exposures. For example, there were no lost workday cases during the year 2000, for the fourth year in a row. The radiation protection program is outstanding. Of 652 people who wore radiation badges, 306 received no measurable dose, 309 received less than 50 mrem, and the remaining 37 received a total of only 5.89 rem. This level of protection is applauded by the subpanel and also by the external Safety Audit Committee, which notes in its September 2000 report that “radiation exposures have remained approximately level, although the number of experimenters has increased and the reactor group seems to have performed more ‘hot’ work. This is one of the reflections of a highly qualified operating staff working with a highly qualified health physics staff.” Finally, the panel notes with approval that the effort to relicense the reactor for another 20 years of operation appears to be on track, with submission of the application scheduled for 2004. One element of the preparation is the rewriting of the Safety Analysis Report. This task includes updating the thermal hydraulics calculations to ensure reactor safety under postulated accident conditions. The work on these calculations will be contracted out and should be completed over the next year, which is an adequate time frame. Program Relevance and Effectiveness As noted in past reports, the recent precipitous decline in the availability of neutron-science facilities in the United States has forced the NCNR to step up and play the role of primary national user facility for U.S. neutron scientists, and the panel commends the NCNR for successfully meeting this challenge. Currently, other older facilities have been shut down or have limited capabilities and access, and new facilities, such as the Spallation Neutron Source (SNS), are not likely to be completed soon.6 5   At the beginning of 2001, heavy water again began accumulating in the collection system, this time at a much faster rate. In these circumstances, the staff were able to determine that the water was coming from a section of the thermal column cooling system piping located within the reactor shield. Reactor operators then diverted the heavy water flow through another pipe and stanched the flow into the collection system. Since water is no longer accumulating and the diversion does not interfere with safe and effective operation of the reactor, permanent repairs to the thermal column cooling system have been deferred until the long shutdown, which is scheduled to begin in the summer or fall of 2001. 6   The Brookhaven High Flux Beam Reactor (HFBR) has been shut down permanently. Even before the HFBR was shut down, the domestic neutron scattering resources available to U.S. researchers were marginal at best in comparison to facilities available in Europe and Japan. The only other U.S. reactor supporting neutron research, the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory, was shut down last October for extensive facility modifications and upgrades, and it is uncertain when the facility will become operational again. It is unlikely that the Spallation Neutron Source (SNS) currently under construction at Oak Ridge will achieve full operational status during this decade. The only other pulsed neutron sources (at Argonne and Los Alamos National Laboratories) have limited technical capability and can support only relatively small numbers of users.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 Therefore, for at least the next several years, the NCNR will be the primary resource for the U.S. neutron science community. While the NCNR staff have coped with increasing demands from U.S. researchers over the past several years, the burden continues to increase, and a visible commitment from the Department of Commerce in support of the NCNR’s effort to meet the nation’s neutron needs is required to prevent the relevant research communities from atrophying. A sense that U.S. scientists could be denied access to cutting-edge neutron-based instrumentation for a number of years would provide a strong disincentive for young scientists contemplating neutron science as a career and would negatively impact progress in the field. The NCNR has developed an impressive suite of instruments, and the NCNR user community continued to grow at a modest rate during fiscal year 2000; the center currently supports approximately 1700 users. Instrument time is heavily oversubscribed on most of the instruments open to use by the external scientific community. In this environment, the recent renewal of National Science Foundation (NSF) support for the Center for High Resolution Neutron Scattering (CHRNS) is particularly welcome, as it will provide additional funding for microstructural research efforts. An especially important element of the planned CHRNS activities is refurbishment of the current 8-m SANS instrument in order to recommission it as a 9-m instrument and make it available to the NCNR’s users. This new capability will make a substantial contribution to reducing the current excess demand for SANS beam time. User satisfaction with the NCNR facility remains extremely high. The experienced NCNR staff are a valuable resource, and efforts to develop new instruments, improve current equipment, and provide support tools demonstrate that the NCNR places a high priority on effectively serving its many users. Ongoing work on improving the sample environment for experiments on the SANS and neutron spin echo machines is particularly appropriate. Also, the spectrometer and analysis software developed in-house has been significantly upgraded in terms of user friendliness recently, although it could stand additional improvements. The NCNR not only supports current users effectively but also reaches out to educate and train new users, particularly through its popular neutron-scattering summer school. This annual weeklong program took place for the sixth time in June 2000 and was attended by 32 graduate students and postdoctoral fellows. This 2000 program focused on SANS and neutron reflectivity techniques, and the hands-on experience was a unique and valuable opportunity for the attendees. In collaboration with their broad user community, the NCNR staff produce a wide array of scientific results. The specific activities presented to the subpanel were uniformly interesting and of high quality, and the overall importance of the research projects done at NCNR is attested to by the long list of publications in peer-reviewed journals. The 420 papers attributable to NCNR and collaborating institutions and accepted by or published in archival journals during fiscal year 2000 demonstrate that a large quantity of valuable work is being accomplished there. While this output is impressive, it is difficult to judge the significance of any individual project to quantify the impact of NCNR scientific results on problems of great national interest. Results for various queries of citation indices were not available when the subpanel met. However, the subpanel notes that the question of how to measure the value of research is a complicated one for all scientific organizations, not just NCNR. In addition to playing an important role in fundamental scientific research, neutron science has applications to important industrial questions. Although the number of instrument sessions allocated to industry is not high, some of the individual NCNR programs are in close contact with industrial researchers and are addressing questions of great relevance to industry. To support these efforts, mechanisms exist to allow companies to conduct proprietary research when necessary. The NCNR can fully recover the costs of experiments whose results will not be shared with the larger scientific community, and procedures are in place for turning off auto backup and archiving of data during these studies.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 With these options available, no barriers to industrial liaisons with NCNR appear to exist. However, it is not clear if NCNR staff are currently clear on the procedures to handle proprietary work or if many industry researchers are aware that NCNR is open to proprietary projects. In addition, the biggest obstacle to industry-NCNR interactions may be a lack of knowledge and understanding on the part of corporate research organizations about how neutron-based tools can be used to answer important industrial questions. In the life sciences area, the NCNR program is relatively small, but it can be expected to play a critical role in fostering interest in the use of neutrons to study biological systems and in maintaining a research community in this area during the 7 to 10 years before the SNS is operational. The present level of such research in the United States is well below the level of 15 years ago and certainly not comparable to the thriving activities of Europeans in this field today. The NCNR push to stimulate neutron-based life science experiments is the key to revitalizing this area of research in the United States. Resources Funding sources for the NIST Center for Neutron Research are shown in Table 6.6. As of January 2001, staffing for the NIST Center for Neutron Research included 92 full-time permanent positions, of which 86 were for technical professionals. There were also 13 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers. The NCNR management and staff have admirably balanced competing demands for resources over the past several years as needs and opportunities continued to increase but available resources remained essentially constant. It is unlikely that cost-effectiveness can be improved significantly over what has already been achieved. In the future, demands on this national facility will only increase, and allocating TABLE 6.6 Sources of Funding for the NIST Center for Neutron Research (in millions of dollars), FY 1998 to FY 2001 Source of Funding Fiscal Year 1998 (actual) Fiscal Year 1999 (actual) Fiscal Year 2000 (actual) Fiscal Year 2001 (estimated) NIST-STRS, excluding Competence 14.8 14.5 15.9 15.4 Competence 0.1 0.2 0.2 0.1 ATP 0.3 0.3 0.3 0.3 OA/NFG/CRADA 1.9 1.6 1.9 2.4 Other Reimbursable 0.1 0.2 0.2 0.2 Totala 17.2 16.8 18.5 18.4 Full-time permanent staff (total)b 84 85 85 92 NOTE: Sources of funding are as described in the note accompanying Table 6.1. aTotals for the NCNR include only normal operation costs. Fuel cycle and upgrade costs associated with the reactor, totaling approximately $6.8 million this year, 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 2001 the funds necessary for facility operation, user support, infrastructure improvements, and research activities will continue to require a delicate balancing act and difficult decisions. A critical element in the success of the NCNR is the excellence of its technical staff. The support of the user community reflects the motivation and technical competence of the in-house personnel. However, these staff scientists need to have intellectually challenging assignments if their competency is to remain current, so they must have the chance to actively participate in fundamental research projects. Providing opportunities for intellectual stimulation is increasingly difficult as the burden of supporting larger numbers of users on increasingly complex instruments grows. While many of the users are experienced and require little assistance, there is a substantial call on the time of staff scientists for training new users and for the routine configuration of the instruments at the start of an experiment. If scientists are overwhelmed by user support obligations, detrimental effects on in-house research and staff morale are likely. Senior NCNR management appear to be aware of this possibility and are taking some steps to prevent staff burnout, including the recent development of new policies to help staff balance work and personal commitments and the continuing emphasis on developing ways to improve instrument automation. Automation tools are particularly valuable, as experiments run 24 hours a day, 7 days a week when the reactor is operating, placing a heavy burden on both NIST staff and visiting users. Another possible approach to increasing the productivity of the scientific staff would be to shift some of the experimental setup and more routine support activities to technicians. In the crystallography and diffraction applications areas, the staffing appears to be stable, but overall the population of these groups is aging. The subpanel commends the researchers’ noteworthy efforts to systematically transfer existing crystallographic expertise to younger members of the staff through internal study seminars. Hiring postdoctoral fellows and bringing in term appointments can also be a useful mechanism for providing periodic revitalization. The overall staffing levels for crystallography projects seem adequate, but the work on diffraction applications appears to be slightly understaffed. Personnel shortages could impact the timeliness and, hence, the effectiveness of NIST work in this area. The small size of the life sciences effort at the NCNR reflects the limited availability of personnel with appropriate skills and of time on reactor instruments. NCNR staff and external collaborators have been unable to secure funding from the National Institutes of Health to support a SANS instrument dedicated specifically to biomembrane work. While the lack of success in this effort has been a disappointment, the subpanel notes that it may be due to the relatively low level of awareness in the larger biological community of neutron-related approaches. The subpanel therefore encourages the NCNR to continue to work with external biologists and biophysicists to obtain the funding needed to support the instruments and research that will demonstrate to scientists and funding agencies the value of neutron science for tackling biological questions of global interest. Plans for refurbishing the infrastructure of the facility are moving ahead. During a shutdown scheduled for late 2001, staff expect to install the new cold source and bring the new larger-capacity, plume-abatement cooling tower on line. Assembly of this new tower is a big project involving the construction of a large new concrete basin and the installation of a taller set of towers that use heat exchangers to warm the air and eliminate the condensation that is responsible for the visible plume. The plan calls for other improvements to the facility infrastructure during the shutdown, such as replacement of service water piping, electrical wiring, switchgear, and transformers. All of these improvements are essential to continue the outstanding performance of a facility containing components that will soon be 35 years old. Given the NCNR’s position as the primary U.S. facility for neutron research at this time, there is a great deal of pressure to maximize the reactor’s running time over the short term. However, management has carefully planned these upgrades and obtained the necessary funding and is correct in

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001 going forward with the scheduled shutdown to perform the needed improvements. The subpanel commends the NCNR management for this decision as these actions are necessary to ensure the reliable operation of the reactor and researchers’ access to high-quality, neutron-based experimentation tools in the long term. The shutdown was originally scheduled for 2000, but the fabrication of the cold source and the design and construction of the cooling tower are both taking longer than originally planned, so the long shutdown had to be shifted to late 2001. Now the upgrades to the facility, including the new cold source and the replacement of the cooling towers, are expected to be completed by the spring of 2002. The decision not to rush any of the key safety and quality assurance steps involved in design and construction of the source or the tower is another indication that NCNR management continues to make safe operation of the reactor its highest priority. Major Observations of the Subpanel The subpanel presents the following major observations: World-class neutron science is being performed at the NCNR, which supports a very large and technically diverse user community. The recent decline in the availability of neutron-science facilities in the United States has elevated the NCNR to a position as the only major national user facility in this area, and the future of the field in the United States depends on a critical mass of researchers continuing to have access to the neutron-based instruments of the NCNR. The excellent technical staff are the key to the effectiveness of the NCNR. It is therefore important that these scientists be allowed to balance their support of the growing user community with participation in intellectually stimulating research. Management should continue its efforts, such as the development of instrument automation programs, to ensure that the burden of training and supplying assistance to external users does not overwhelm the in-house staff. Given the resource constraints under which the NCNR has operated over the past several years, management and staff have admirably balanced competing needs for funding for facility operation, user support, infrastructure improvements, and research activities. Currently the NCNR appears to be operating as cost-effectively as possible. Reactor operations and engineering activities continue to be performed in an exemplary fashion. Preparation for major upgrades to the reactor, including a new cold source and cooling tower, is progressing and the improvements will be welcome. All operating decisions are made with an appropriately conservative approach to ensuring safe operation of the reactor. Formation of a life sciences program at NCNR is moving ahead. While limited resources have slowed progress somewhat, the quality of the scientific results produced in collaboration with external scientists fully justifies continuing the efforts to secure funding for an instrument dedicated to biological applications and to foster the development of a biological neutron community in the United States.

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