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1 ~ Materials Science and Engineering Laboratory: Division Reviews CERAMICS DIVISION Technical Merit The Ceramics Division's mission is to work with industry, standards bodies, academia, and other government agencies in providing leadership for the nation's measurements and standards infrastructure for ceramics materials. During 2002, the Ceramics Division, in response to ongoing funding challenges, eliminated low-priority projects, reduced its total number of personnel, and reduced permanent staffing by 10 (a 25 percent reduction in force). The panel reviewed the process used to eliminate projects, and it concurs with the division's assessment and actions. The division also reorganized the remaining programs and personnel into four groups: Electronic and Optoelectronic Materials, Characterization Methods, Data and Standards Technology, and Nanomechanical Properties. The panel reviewed six division programs (composed of 16 projects) in detail for their performance during 2002: Advanced Manufacturing Methods, Data Evaluation and Delivery, Materials Property Measurements, Materials for Opto- and Microelectronics, Materials Structure and Characterization, and Combinatorial Methods. The panel's overall opinion is that the division not only maintained the quan- tity and quality of its technical output during a difficult year, but is also in a better position to increase its output during 2003. Overall, the Ceramics Division published 120 publications in FY 2002 (86 in archival journals), which represents 20 percent of all MSEL's publications. The following subsections discuss and evaluate the technical merit of the work in progress for each program. NOTE: Chapter 6, Materials Science and Engineering Laboratory," which presents the laboratory-level review, includes a chart showing the laboratory's organizational structure (Figure 6.1) and a table indicating its sources of funding (Table 6.1~. 207

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208 Advanced Manufacturing Methods AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 The Advanced Manufacturing Methods Program included two projects: Process Modeling for Low Temperature Co-fired Ceramics (LTCC; eliminated in 2002) and Rolling Contact Damage/Fatigue. The objective of the LTCC project was to model the sintering processes in order to enable predictions of the distortions that occur during the manufacture of LTCC products. In last year's panel report, it was noted that the microstructure scale of the modeling approach (approximately hundreds of microns) might preclude translating the results to the much larger-scale distortions for example, camber (bending)- of manufacturing interest. The technical output from this project was also low in 2002 (one conference . . . . . .. . . . . . ~ ~ ~ . ~ . . paper), and during the year the division chose to terminate the LTCC project as part of its restructuring. Under the circumstances, the panel does not disagree with this action. In the Rolling Contact Damage Fatigue project, an International Energy Agency task has been established to conduct an international round-robin comparison of rolling contact fatigue test methods among U.S., Japanese, and German participants. For the three-ball test, there appears to be the need both for better instrumentation to understand the range of applicability of the test and for carefully controlled measurements to provide a more scientific basis for the test. If this project is to be continued, such additional levels of rigor will be essential. Data Evaluation and Delivery The Data Evaluation and Delivery Program is focused on linking disparate structural and property databases to provide a basis for understanding existing materials and potentially for designing new materials. Most materials databases focus on a specific area, such as structure, properties, or phase equilibrium. However, most questions of current interest to the scientific and industrial communities do not concern one particular area. but rather the relationships between areas (em.. structure and oroner- . A. . .... . . .. ,% . . . . . .. . .. ,%. . . ~ , ~ ~ hi, .. ~ ~ ~ . ... . .. .. .... ,% . . . . . . ,% .. . ,% . ties). Most exciting IS the posslulllty of ~avmg quick access to Information on a vast array of structures and properties simultaneously in order to postulate properties of structures not yet synthesized. In keeping with the goal of achieving such a capability, one of the objectives of the Data Evaluation and Delivery Program is to enable seamless transitions from one data set to another. The Materials Property Data project compiles data, for example, on the elastic properties, hardness, toughness, flexural properties, specific heat, and sound velocities of many inorganic crystal structures. Keeping the data- base current in any one of these areas is an enormous task. The current inorganic structural database consists of 65,000 crystal structures that are updated twice a year. These updates are derived from the primary literature and typically consist of 1,500 to 2,000 new entries each year. The individual entries are only the beginning, as the true value of the database can only be derived from being able to link different entries by similarities and differences. With so many updates required each year, the traditional method of manually checking individual entries for consistency has had to give way to more automated approaches. The panel heard plans for constructing software tools to automate critical evaluation of entire collections of data. The panel believes that more extensive tools for identifying trends in and outliers among the data sets would offer great opportunity for scientific discovery. Materials Property Measurements The Materials Property Measurements Program has always had a strong emphasis on mechanical behavior and has built a reputation for quality research in the area of brittle fracture. Some of this expertise is being summarized in a new NIST Practice Guide, Predicting Mechanical Reliability for

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS . . ~ . 209 . . At, . . ~ Brittle Materials. Lifetime prediction has become increasingly important in many industries, and such guides are invaluable to technology managers for creating studies that are statistically valid. This program consists ot two projects: Mechanical Property Measurements and Microstructural Design. In 2002, plans were begun to shift this program's emphasis from macroscopic behavior to a focus on nanometer-scale mechanical property measurements. Properties such as nanohardness and elastic prop- erty measurement on small-scale samples have implications for advanced technologies. For example, mechanical properties of thin films have broad applications in many industries, including electronics, automotive, aviation, space, and medical devices. The panel has strongly endorsed this shift in focus to an area that could greatly benefit from NIST expertise, particularly in terms of test method and standards development. Work is beginning on Standard Reference Materials for nanoindentation. No such SRMs now exist, despite the rapid growth in sales of these instruments. Finally, instrumentation and test methodologies are being developed for friction measurements at the nanometer scale. Such measure- ments are increasingly important in Microsystems and nanodevices. Materials for Opto- and Microelectronics The four projects in the Materials for Opto- and Microelectronics Program are all heavily linked with other NIST divisions and laboratories. The first, Optical and Structural Characterization of Opto- electronic Semiconductors, is focused on stress and composition standards in AlGaAs films, optical properties of AlGaN, and also InGaAsN studies. The measurements in this project appear to be very precise and carefully analyzed. The second project, Phase Equilibria and Properties of Dielectric Ceramics, is focused on funda- mental materials properties of ceramic materials, from both empirical and first-principles points of view. The NIST team has a long-standing, solid reputation of scientific contributions, and 2002 was a particu- larly good year for research output, with many publications, invited papers, and even popular articles. The third project is Phase Relations of High Tc Superconductors. This project, which also has a very good, long-standing reputation, was funded in part for several years by DOE. The reported phase diagrams reveal information critical to the successful development of those high Tr superconductors. - The NIST efforts are highly leveraged with many outside collaborators. The fourth project is Nanotribology, focused specifically on hard disk drives. Unique measurements and analysis techniques have been established that is, a high-speed impact test, finite-element impact modeling, and carbon overcoat characterizations that have yielded valuable information about the drive head and disk materials and behaviors in operation. Also in this program is a task called Charac- terization of Ultra-Thin Dielectrics. This task has focused on silicon oxide-nitride-oxide stacks for flash memory and on high-k dielectrics for small-dimension silicon devices. Materials Structure and Characterization The Materials Structure and Characterization Program is one of the larger programs in the Ceramics Division. Its primary objective is the development and the application of state-of-the-art instrumentation and measurement capabilities to advanced materials. This program operates, maintains, and develops unique facilities for materials characterization at the National Synchrotron Light Source at Brookhaven National Laboratory and at the Advanced Photon Source at Argonne National Laboratory. It is the panel's belief that there may be no better example of the leveraging of government investment in unique facilities among the widest-possible community. The instrumentation capabilities that this program has built are unprecedented in the field of structure determination of materials and interfaces. The technical

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210 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 output of studies using these instruments has immediate applications in science and technology. The investigations range among a wide variety of fields, such as advanced coatings, fuel cells, optoelectronic materials, and pharmaceuticals. Projects in the Materials Structure and Characterization Program also focus on standards. The panel heard from staff about a project devoted to developing diffraction Standard Reference Materials for use in the 20,000 laboratory diffractometers worldwide. Specific emphasis is being given to providing such SRMs in thin-film form to assist the electronics industry in using diffraction data to analyze stress states and composition variations in deposited thin films. The NIST team is constructing diffraction equipment capable of first-principles measurements of lattice parameters on samples to be used for diffraction SRMs. This equipment will greatly increase the reliability of interpretation of user results and will make possible reliable comparisons of measurements taken from different instruments. Finally, the program has incorporated the Powder Measurements project that was in the Ceramics Division for several years. This project is now focused on measurements and SRMs for nanometer-scale particles. These materials are of increasing interest for diverse fields such as optical materials and pharmaceutics. Combinatorial Methods The Combinatorial Methods Program represents a small effort in the Ceramics Division but is part of a large effort in the MSEL. The unique contributions of the Ceramics Division team are a dual-beam, dual-target pulsed laser deposition system that is used to fabricate several inorganic films for acquiring library data; a high-throughput spectroscopic reflectometer with a bifurcated fiber-optic probe for rapid mapping of thickness and index or refraction; and a NEXAFS (near-edge x-ray absorption fine struc- ture)-based imaging technique with submonolayer sensitivity. Program Relevance and Effectiveness The Rolling Contact Damage Fatigue project's identification of existing test methodologies that lack reproducibility and are not well understood provides opportunities for this program's increased effectiveness in the future. The Data Evaluation and Delivery Program' s effectiveness is measured primarily by direct sales of its databases or by visits to its Web site. During the past year, sales of Phase Equilibria books and CDs exceeded $100,000, and the Ceramics Property Database was NIST's eleventh most active Web site. The program's most significant accomplishment for the year 2002 was the issuance of a PC version of the Inorganic Structural Database. Much of this database is licensed to diffraction instrument manufac- turers to install with the software in their instruments. There may be no better way to disseminate this database than to have it readily accessible when researchers obtain new structural data. Researchers in academia and industry often search among these structures when taking even simple powder patterns rather than having to synthesize or obtain standards to compare against. As the software tools for critical evaluation of data are fully developed, new avenues of distribution may be created. The Materials Property Measurements Program had an active year in the standards area. ASTM test methods for machining effects on strength (C1495) were developed, and methods in fractography (C1322) and rectangular beam flexural strength testing (C161) were revised. The team also led a VAMAS (Versailles Project on Advanced Materials and Standards) study group on an international, interlaboratory comparison of indentation test procedures on thin-film specimens; developed an instru- ment to observe in situ crack evolution and determine the critical load to produce damage of dental bilayers; and developed a stereological technique to measure distributions of grain boundary configura-

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS 2 lions. These grain boundary configurations will be used in NIST object-oriented finite-element analysis software. Under the Materials for Opto- and Microelectronics Program, the careful work in the Optical and Structural Characterization of Optoelectronic Semiconductors project is definitely relevant to industry needs, in terms of both the materials chosen for analysis and the characteristics studied. The level of effectiveness of the work will be judged by publications, specific industrial interactions, and SRMs. The panel encourages increased dissemination of results from this good technical work. For example, the Phase Equilibria and Properties of Dielectric Ceramics project has selected relevant materials systems for study and has aggressively reported quality results to the technical community. In the Phase Rela- tions of High TC Superconductors project, focusing on tape materials/interface issues as a future direc- tion is important for conductive tape applications of interest to DOE. The significance of the Teratology of Hard Disk Drives project to the drive industry and its suppliers is shown by the industrial donations of equipment, personnel, and funding that the project has received over several years. A remarkable number of invited talks have also resulted from this work. The Characterization of Ultra-Thin-Dielec- trics project identified several companies as potential customers of the NIST research, but the project would have increased impact if direct contact were made with those companies to ensure that the scientific studies are addressing the most important issues in the industry. The Materials Structure and Characterization Program, through its beam-line facilities, has been involved in several high-profile structural characterization studies during the past year, including char- acterization of nanoparticle assemblies with number density gradients and measurements to help un- ravel the solid-state physics of magnesium diorite superconductors. Across a wide range of topics, the SANS (APS) (small angle neutron scattering [Advanced Photon Source]) facility was used by 62 universities, 32 government laboratories, and 9 industrial users, leading to 28 archival NIST papers, 22 invited talks by NIST scientists, and 51 papers by the facility's users. The National Synchrotron Light Source was oversubscribed by more than a factor of two. Division Resources As noted at the beginning of this chapter, the staff of the Ceramics Division was reduced by 10 people in 2002 (four retirements and six reduction-in-force actions). The division was led by an acting division chief for most of FY 2002, and a new division chief was appointed in early calendar year 2003. While the panel concurs with the decisions made by the division management team, there is concern that the basic fundamentals that caused the financial circumstances of 2002 have not changed specifically, that mandated increases in salary without a concomitant increase in base funding will distort the distribution of spending between salary and other object codes. MATERIALS RELIABILITY DIVISION Technical Merit The mission of the Materials Reliability Division is to develop and disseminate measurement methods and standards that will enhance the quality and reliability of materials for industry. The division is organized in three groups: Microscale Measurements, Microstructure Sensing, and Process Sensing and Modeling. However, the division's technical programs cross disciplines and are better grouped according to the division's centers of excellence in technical focus areas: Micrometer-Scale Reliability, Nanotechnology, Biomaterials Metrology, Infrastructure Support, and the World Trade

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212 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 (:enter investigation. These technical focus areas are well aligned with those outlined in the overall NIST Draft Strategic Plan (the NIST 2010 plan) and highlight the division's unique capabilities for addressing reliability issues in these emerging areas. The Micrometer-Scale Reliability project works on understanding and predicting failure modes in a variety of material systems under constrained geometries and scaling effects. This project also studies the roles of stress, strain, and temperature in microelectronics and photonic devices. It continues to apply and develop methodologies for measurements of state-of-the-art materials. Further advances were made in the development of pattern-plated materials to study the mechanical behavior of electrodepos- ited thin films. AC-stressing methods for the fatigue testing of fine-scale metals were used. In addition, the team advanced its work in thermal scanned-probe microscopy methods for determining damage mechanisms associated with thermomechanical loading and applied electron backscatter diffraction methods for elastic strain field mapping. The Nanotechnology project works to develop metrologies for nanoscale properties and studies the physical properties of thin films and nanostructures. The team has projects in Brillion scattering for thin- film analysis, conductive atomic force microscopy using carbon nanotubes, atomic force microscopy, nanoscale modeling, mechanical properties of thin films, thermal barrier coating evaluations, and X-ray methods. The work of the Biomaterials Metrology focus area represents a new technical direction for the division; it aims to apply materials science to biomaterials research. The team is now concentrating on the mechanical properties of polymer scaffolds, cellular-engineering Microsystems, and pediatric pul- monary hypertension. By consulting with biomedical experts at the University of Colorado Health Sciences Center and Colorado Children's Hospital, the team has identified a good match between its materials expertise and the critical research area of cardiovascular disease. A fully functioning bio- materials laboratory with advanced metrology capabilities has been established. The team addressing the Infrastructure Support Program provides expertise in failure analysis and failure prevention for large structures. The team continues to be a leader in providing Charpy impact standards by making significant contributions to improving both the SRMs and the test. The staff also have strong international connections and are working toward setting an international standard for Charpy impact testing. The team provides service to the Bureau of Reclamation in metallurgical issues arising during inspections of water-retaining structures, such as the planned repairs to the Folsom Dam in California, and other evaluations for local municipalities. The team's expertise in weld repair and consumable development yielded repair procedures for cracks in the skin of the U.S. Capitol dome in FY 2002. Other activities include waveform-based acoustic emission methods beyond those commer- cially available for the study of transient-energy release and work in conjunction with the DOT and DOE to improve pipeline safety. In support of homeland security, the work on infrarstructure support applies multidisciplinary skills in metallurgy, physics, and materials science to analyze the structural steel from the World Trade Center' s Twin Towers and WTC Building 7. The team evaluated the chemical composition and micro- structure of steel from the WTC and tested its tensile and creep behavior to evaluate how the material reacted to the extreme conditions produced in the tragedy. This work has been done in conjunction with the Building and Fire Research Laboratory and will sunnort improvements in the design. construction. maintenance, and use of buildings in the future. ~ ~ ~ ~ , , The division continued to excel during the past year with high technical merit and output more than 60 publications, more than 20 invitations to make presentations at technical conferences, and two patents. The staff has received appointments to numerous journal and conference proceedings editorships and is represented on the American Physical Society's Keithley Award Committee.

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS Program Relevance and Effectiveness 213 The Materials Reliability Division continues to provide the national technical leadership required to address the broad range of materials quality and reliability issues that impact industry and the nation. The division houses world experts in a broad range of fields, from nanoscale metrology to large-scale structures. FY 2002 highlights include the continued development of the Biomaterials Metrology effort in support of the NIST Strategic Focus Area of Health Care and the response to the World Trade Center investigation. The panel was very impressed with the progress made within the year in the Biomaterials Metrology project, establishing an impressive set of programs in cardiovascular disease that exploit the division's advanced expertise in metrology in a new direction for the division. In the WTC investiga- tion, the division became a key player in the metallurgical work, applying its capabilities, which are unique among NIST resources, to provide the very rapid response required. In FY 2002, the Materials Reliability Division responded very effectively to the panel's recommen- dation to focus the division around its core competencies and the key SFAs. The reorganization of the division into centers of excellence Micrometer-Scale Reliability, Nanotechnology, Biomaterials Me- trology, Infrastructure Support, and the World Trade Center evaluation has allowed the division to break down some organizational barriers that were present under the previous structure and to utilize resources better across the entire division. The division continues to do novel and important work for the microelectronics and photonics industries and is now extending its influence into health care with the establishment of its new thrust into Biomaterials metrology. The division has a broad range of customers from industrial partners, to governmental agencies, to national laboratories of other countries, to academic institutions. The division is focused on developing tools and metrics that can be used by its partners, and it serves as an active center for measurements. For example, the division worked with collaborators to disseminate its work in thermal-scanned probe microscopy for packaging reliability. The panel approves these efforts to ensure that the division's work is aligned with the SFAs and that it is useful for its many partners. However, the panel believes that in some projects the division is too often in a supporting role within MSEL and not directly connected to the industry partner. The panel maintains that even in interlaboratory collaborations, direct connections between division personnel and external customers would be beneficial in order to effect a more efficient introduction of the division's developed technology to the appropriate industries. The panel is also concerned that the division is not compensated for its measurement services and recommends that it look for "best practices" within NIST and the MSEL to determine a way to be compensated for measurement services provided to companies. The Materials Reliability Division' s rapid response to the World Trade Center disaster exemplifies the value of the division' s unique technical expertise. The panel recommends that the division build on its success with the infrastructure reliability projects, including the WTC work in FY 2002, by proactively identifying exploratory projects that address other infrastructure reliability issues that could have sig- nificant impact on homeland security. The division offers a depth and breadth of experience in investi- gating material and structural failures that could not be easily or quickly replaced. As demonstrated in the WTC and Capitol dome investigations, it provides a vital body of expertise for quick response to infrastructure issues. The program in Biomaterials Metrology has made rapid progress and is a good model for the division with respect to utilizing its core competencies in the SFAs. For example, an outside consultant was engaged to advise on key areas in health care in which the division's strong expertise could be exploited in developing metrology tools, micromechanical testing, and mechanical modeling; this action led to the rapid identification of important research areas in cardiovascular disease. The program's

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214 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 regular status meetings to review the research, obtain input from external experts, and solicit input from ~ ~ . ~ ~ . ~ , ~ ~ ~ ~ ~ ~ , ~ ~ , ~ ~ IT ATE ~ ~ ~ ~ ~ r , ~ the bench level on keeping the program goals within Nlbi l s picas are an admirable example of the collaborative nature of the projects in this program. The division has a high level of relevance and effectiveness as evidenced by the large number of papers published in journals, the awards received by the researchers, and the number of Web site downloads. Many of the projects, such as those within the ATP and Director's Choice Awards, have direct measures of effectiveness with well-defined milestones. The panel believes, however, that some projects, especially the base-funded programs, could benefit from clearly articulated milestones and from regular status reviews of progress toward the milestones. Strict milestones may not always be appropriate for long-term research projects, but the panel recommends that projects be reviewed within a flexible structure. Regular reviews with group leaders could determine if progress was satisfactory, if milestones were being met, if the project was within the original scope and within the SEA, and how project goals should evolve. This process might also help in effectively using resources in a flat budget environment. The majority of the Materials Reliability Division' s research programs are long term, but their focus changes in response to customer needs and the requirements of NIST. The long-term research programs provide not only technical leadership in their respective areas, but also expertise that can be called quickly into action, as evidenced by the homeland security activities. Division Resources Although the Materials Reliability Division has maintained strong technical leadership in its areas of expertise, the panel is concerned with the continually declining number of permanent staff. The division has done a good job of meeting staffing needs creatively within a flat base budget, but this has been achieved primarily through temporary appointments and the use of nonpermanent staff. The continued erosion of the permanent staff base will jeopardize critical efforts such as succession planning and maintaining a strong base of permanent experts. The panel is also concerned with the slow pace of the search efforts targeted toward finding a replacement for the retiring division chief. With the retirement of the current division chief and the inevitable management changes to the organization, maintaining continuity in the current focus of the division is strongly recommended. After 2 years of realignment within the division toward a more focused mission, core centers of excellence, and programs well aligned with the SFAs, the division is just starting to produce the results that these changes were meant to promote. Among the workforce in the division, the changes seem to have had a positive impact as evidenced by the results of the NIST employment survey in which the division staff rated their work environment and their relationship with the division management very favorably. In general, their responses to these types of questions about such issues were more favorable than were the responses from NIST overall. The panel feels that a clear message from the division management assuring staff that the current focus will continue is essential. While the changes within the division have been very positive in increasing cross-functional inter- actions with the Gaithersburg divisions, the panel would like to see more interaction between the MSEL management in Gaithersburg and the Boulder staff, either through on-site visits or telecommunications. The NIST policies and processes on intellectual property appear not to be communicated effectively to the staff. The NIST counsel's office appears to respond well only to "boilerplate" issues, and the staff tends to avoid using the intellectual property mechanisms in place because of both perceived and real barriers. The panel recommends a review of the policies in order to establish a more user-friendly process.

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS 215 Facilities for the division in Boulder have not improved significantly, although the staff has man- aged to work within the constraints of the laboratories and has done an admirable job of setting up new laboratories and equipment within the existing facility. However, as the research activities probe ever smaller length scales, apparatus must be made extremely stabile against vibration. Most of the facilities available to the division cannot currently meet this requirement, and so on-grade offices must be converted into laboratories with the attendant lack of regular laboratory outfitting. The panel recommends follow-up on its recommendation from last year for the development of a critical, "must-have" list of capital equipment needed to maintain the division's status as a worldwide center of excellence in materials reliability. Within the constraints of 1-year, use-it-or-lose-it capital budget cycles and the need to purchase major pieces of equipment that may require more dollars than are available in a single year, the panel recommends that the division explore alternatives to acquiring costly but critical equipment for example, equipment leasing options. METALLURGY DIVISION Technical Merit The Metallurgy Division provides critical leadership in the development of measurement methods, standards, and fundamental understanding of metal behavior. This information is needed by U.S. mate- rials producers and users in order to provide materials needed for existing and emerging technologies. The division is organized in five groups on the basis of materials class and category of expertise: Electrochemical Processing, Magnetic Materials, Materials Performance, Materials Structure and Char- acterization, and Metallurgical Processing. Individual programs are not confined to the group structure and typically span more than one group and frequently more than one division of the Materials Science and Engineering Laboratory. This matrix structure provides great flexibility in program definition, makes possible the assembling of the spectrum of expertise required for each program, and encourages strong collaboration between groups and divisions. This strong collaboration across groups and the supportive environment are among the truly remarkable characteristics of the Metallurgy Division and the NIST MSEL in general and a true strength of this laboratory. The consensual process in choosing programs and priorities is one of the principal factors engendering the exceptionally high morale of this division, even in the face of essentially static budgets and numbers of Permanent staff. . The division's particular technical strengths are in diffusion, phase transitions, structural character- ~zat~on, and modeling, and, in special areas, synthesis. The programs of the division can be divided into three broad categories: 1. The development and promulgation of standards, especially measurement standards, in mature areas of technology; 2. The development of scientific understanding in areas of technology of some maturity that are challenged by advances in materials or processing demands; in such areas materials processing being one current empirical approaches are not adequately extensible, and deeper fundamental knowledge is required; and 3. The exploration of new areas in which it is perceived that industry will in the foreseeable future require knowledge and support. An example in category 1 is the International Hardness Standard Program, perhaps the best present current example of a traditional NIST standards program. The new-science content is modest, but the

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216 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 need for standardized measurement techniques and standards reference samples is great. The effort in unifying the Rockwell-C hardness scales makes NIST the world leader in that field, and the Rockwell Hardness Measurement Practice Guide (available on the division's Web site at www.msel.nist.gov/ practicoguides/SP960_5.pUf) is a logical and valuable output. An example in category 2 is the Light Metals Forming Program in its various facets. As the automobile industry moves to lightweight bodies with new alloys such as ultralight high-strength steel and more formable aluminum sheets, there is a greater need than in the past to understand formability and springback issues related to stamping operations. Currently, the automotive industry has the capa- bility to determine the relevant process parameters through numerical simulation. It is, however, a difficult task to fully understand the microstructural mechanisms that govern the plastic deformation of the materials. NIST scientists have provided invaluable experimental data as well as material modeling support to the original equipment manufacturers. In category 2, industry has encountered problems and is looking to NIST to provide a deeper understanding of the root causes of problems. Examples in category 3 are the Ballistic Giant Magnetoresistance project in magnetics and the Nitride Metallization of Optoelectronic Devices project in microelectronics. In both cases, the Metal- lurgy Division is anticipating areas of probable technological and scientific need. Such work entails high risk but potentially high payoff. The exceptional overall materials expertise residing in the Metallurgy Division enables it to marshal a strong effort in newly activated programs, as was observed with the World Trade Center investigation. Program Relevance and Effectiveness The Metallurgy Division's customers represent a wide range of industries, as well as universities. The most obvious and dominant customers are the automobile, aerospace, and magnetic data storage industries and the portions of the electronics industry involved with electrodeposition and interconnect. With the exception of the electronics industry, these tend to be mature industries, a subject that is discussed below. The evidence is strong that the division's programs are relevant to the current and future needs of its customers. Programs are typically formed through a pull by the industry and concurrent analysis of its technology and problems. Areas are then identified in which the scientific strength of the division positions it to make special and unique contributions to the specified technologies. Examples of this approach abound, such as that of the lead-free solder, superconformal film growth, and the metal springback and formability programs. The Ballistic Giant Magnetoresistance and the Optoelectronic Nitride Coating projects address future industrial needs. The division does an excellent job of preserving a core competency to be applied to real problems. In response to questions arising from the World Trade Center building collapse, in-house expertise was marshaled to develop a high-deformation-rate, high-temperature experimental system to address a new set of needs arising from the analysis of this incident. There is abundant evidence that the results of the division's research are being disseminated to and are utilized by industry: for example, the ongoing demand for Standard Reference Materials and stan- dard samples; the large number of hits on the division's Web site; letters of appreciation from industry; collaborations on specific issues; and the many instances in which collaborating companies, or simply industry-associated companies, have incorporated NIST results into their ongoing development efforts. In a number of cases, the output utilized by industry is an improved model of the behavior of interest and the generation of reliable input parameters for existing or new model systems. Recently, the automotive industry has looked to NIST to provide a deep scientific understanding of material behavior during plastic deformation and the know-how to turn such understanding into mathematical models for use in

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS 217 simulations. The division staff clearly works hard at making contact with its customers and communi- cating useful results to them. Overall, the panel believes that the programs of the Metallurgy Division are well attuned to custom- ers' needs. The panel is concerned, however, that in some instances links to applications could be stronger. In the Plastic Deformation Program, for instance, the roughness project would benefit from more user input, and in the phase diagram arena, the extension to systems of 10 or more components, while a tour de force, is probably not as useful as more attention to ternary or quaternary systems. Division Resources Funding for the Metallurgy Division has been essentially flat for several years. Given mandatory salary increases and the rising cost of expendable and support personnel, the size of the full-time equivalent research staff has diminished significantly over the past decade. The panel notes with ap- proval that the decline has been halted in the past 2 years and may be slightly reversed. The panel notes also that the funding per full-time employee is roughly $200,000, including overhead (out of which capital purchases are amortized). This funding, though certainly not overgenerous, is also certainly adequate. The principal complaint by the staff, and a valid one, is the difficulty of acquiring capital equipment. For a laboratory that has the responsibility for setting national and world standards, it is important that the equipment be state of the art. This is frequently not the case. To acquire a major piece of equipment, such as a focused ion beam system or transmission electron microscope, it is necessary for three or four divisions to pledge most of 1 year's capital budget to that purchase. There is no apparent escape from this capital resource shortage within the present budgeting process. A one-time-only capital grant of significant magnitude, and outside the present requirement for amortization by the operating budget, would be of enormous benefit to the Metallurgy Division and the Materials Science and Engineering Laboratory as a whole. The core value of the Metallurgy Division is the competency of the permanent staff. The key challenge to the division management is to maintain a central competency capable of executing the division's mission with respect to both present and future needs. The panel has some concern that the primary customer base of the Metallurgy Division is waning industries (automotive, steel, aluminum, aerospace). The question then arises as to whether the division should be moving actively to dissolve the present core competencies and to replace them by more modern competencies, such as those that underpin the information revolution. The panel is in unani- mous agreement that such an accelerated dissipation of the present capability would be an enormous mistake. The division' s competency in the essential disciplines of metallurgy is unique in its breadth and strength and is in its own right a national treasure. The value of the core competency in metallurgy was demonstrated recently by the role that the division has been playing in analyzing the collapse of the WTC's Twin Towers. There is no other group to which the nation could turn for equivalent expertise in this effort. In a nation with an aging infrastruc- ture for instance, its bridges and pipelines such expertise may be essential not only in analyzing future structural failures but also in devising strategies to minimize such failures. The panel foresees also that the Metallurgy Division will be called upon in the near future to generate similar programs in support of the homeland defense mission. The staff of the division must, over time, be updated with young employees, but turnover at the rate of one staff member per year seems an appropriate pace. In hiring new staff, however, the division must make sure that it is acquiring the expertise to support emerging industries, not restricting hires to replacing, more or less in kind, present areas of emphasis.

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224 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 Technical Merit The mission of NCNR is (1) to operate the NIST Research Reactor cost-effectively while assuring the safety of the staff and general public, (2) to develop new methods and applications for neutron measurements, and (3) to apply these methods and applications to problems of national interest. The NCNR is responsible for operating its research facilities as a national facility serving researchers from industry, universities, and government. The panel continues to be impressed with the high quality of the NCNR's scientific programs and its safe and effective management of the reactor. The instruments available to the neutron research commu- nity that uses the NCNR are among the best in the world, and the research occurring on these instru- ments is influential in a number of scientific fields. The NCNR is a facility of substantial national importance. According to a survey performed bv the Institut Laue-Lan~evin in 1999 through 2002. the NCNR has ranked second worldwide among neutron science facilities in the number of papers pub- lished in high-impact scientific journals such as Science, Nature, Physical Review Letters, and the Journal of Molecular Biology. This opinion is reinforced by the June 2002 report of the federal- government-wide Interagency Working Group on Neutron Scattering (organized by the Office of Sci- ence and Technology Policy), which finds that "the NIST facility is the only U.S. neutron science facility that currently provides a broad range of world-class capability." Now and in the immediate future, the NCNR will be the principal site at which to do neutron research in this country, as the reactor at the Brookhaven National Laboratory has been shut down, and it will be approximately 4 years before the Spallation Neutron Source (SNS) at Oak Ridge National Laboratory comes online and another 2 years after that before it is fully ready to serve the broader research community. However, the staff at the NCNR continues to actively plan for complementing SNS and its capabilities when it becomes operational. Decisions about what new instruments to develop and whether to refurbish or replace various older instruments are being made in the context of the capabilities that will be available at SNS and the types of experiments that are better suited to the NCNR's steady neutron source. This effort is fully consistent with the recommendations of the Inter- acencY Working Group on Neutron Scattering. Decisions about facility improvement at the center also take into account external input from a number of sources, including the NCNR Users Group and its Program Advisory Committee, this panel's annual assessment, and the 1999 NRC report on managing the nation's multidisciplinary user facilities.2 The NCNR staff' s awareness of the overall context in which neutron research occurs and of the constant evolution of the field is exemplary. Continual improvement of the NCNR facility is critical, as a user community for SNS will exist only because of those users' experience with and access to existing neutron research centers, of which the NCNR is the largest and most effective in the United States. In fact, many of SNS's users will have been drawn into neutron science by results obtained at the NCNR and will have been trained at this facility. The NCNR is divided into three groups: Neutron Condensed Matter Science, Reactor Operations and Engineering, and Research Facilities Operations. The Neutron Condensed Matter Science Group has the prime responsibility for the second part of the NCNR's mission and provides scientific leadership for the third part. The group carries out a program of research relevant MSEL and NIST programmatic needs, develops the scientific basis for 2National Research Council, Cooperative Stewardship: Managing the Nation's Multidisciplinary User Facilities for Re- search with Synchrotron Radiation, Neutrons, and High Magnetic Fields, National Academy Press, Washington, D.C., 1999.

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS 225 instrumentation, develops new applications of neutron methods to service a broad range of problems, and provides scientific leadership for the instruments in the user facility. The Neutron Condensed Matter Science Group is divided into five teams, each of which both performs research and supports the instruments used to do the research. This support includes improving existing instruments, developing new instruments, and facilitating the effective use of the instruments by the NCNR's national user community. This group is also home to the National Science Foundation's (NSF's) Center for High Resolution Neutron Scattering (CHRNS), which provides users with access to a range of neutron scattering instruments. The NCNR is developing a research effort in the life sciences, which is now supported in part by recent funding from the National Institutes of Health, to form the Cold Neutrons for Biology and Technology (CNBT) collaboration. The work of these groups is discussed in the subsections that follow. The Reactor Operations and Engineering Group has the prime responsibility for the first part of the mission. It handles the day-to-day operation of the reactor, the planning and execution of upgrades and maintenance, and regulatory compliance. In addition to these ongoing duties, at the present time this group is heavily engaged in preparing an application to relicense the reactor for an additional 20 years, through 2024. The Research Facilities Operations Group, together with the Reactor Operations and Engineering Group, ensures the safe and effective functioning of the reactor and the efficient production of neutrons for research. The work of these groups is discussed below, in the subsection entitled "Research Facilities and Reactor Operations." Overall, NCNR scientists' strong, collaborative relationships with users of the facilities' instru- ments maximize not only the efficiency and effectiveness of the work done but also the quality of the results produced at the NCNR. In the following subsections selected projects that highlight the technical quality and merit of the work at the center are discussed, by group. Neutron Condensed Matter Science Scientists in the Neutron Condensed Matter Science Group are pursuing a variety of research topics uniquely suited to investigation by using the properties of neutron spectrometry, scattering, reflectom- etry, and diffraction. These topics range from understanding polaron dynamics, twisted magnetic struc- tures, charge-orbital-driven transitions, and hydrated clathrates to measuring and modeling manufactur- ing-induced stress distortions in metals. The topics presented to the panel were impressive in their depth, in the quality of the experiments, and, perhaps most importantly, because the kinds of questions and experiments being pursued foster the development of new interpretations, new questions, and new instrumentation. Particularly notable is the excellent research program concentrated in the area of strongly correlated materials. This program emphasizes oxide materials, including polaronic properties of colossal magne- toresistance manganites and relaxer ferroelectrics and magnetic properties of e-doped cuprate supercon- ductors. The experiments conducted on frustrated magnetic systems and the reflectometry studies of buried magnetic twists are leading edge. The small effort in measuring and modeling manufacturing- induced stress distortions in metals continues to fill an important niche for industry by putting current empirical finite-element methods on a more robust, scientific basis. Development of the state-of-the-art triPle-axis spectrometer is on schedule and will be an important ~ ~ . . . ~ . . ~ ~ ~ . . . ~ _ To_ To ~~ _ T . ~ ~ ~ ~ ~ . . ~ ~ ~ addition to the instrumental capability at the N(:NK. the Neutron (condensed Matter Group has excel- lent postdoctoral fellows and maintains a very strong outside collaborative network of users.

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226 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 Access to appropriate levels of expertise in theory and modeling as related to the experimental program at the NCNR has been an ongoing concern of this panel. The NCNR leadership has taken this observation very seriously and, within the confines of the various constraints (budgetary, space, and so on), has responded very positively. A modest group now exists that includes two permanent team members and several long-term postdoctoral researchers, together with several short-term visitors, some of whom are quite senior. Current activities center on first-principle simulations of lattice vibrations, numerical studies of Hubbard models as applied to the magnetic oxides, and studies related to neutron scattering instrumentation. These investigations are world-class science that couple nicely with other research activities of the NCNR. The panel would especially like to underscore the recent elegant application of hidden symmetries in the orbitally degenerate Hubbard Hamiltonian, as applied to the metal oxides, which enormously enhances the capabilities of numerical simulations of spin/orbital ordering. Center for High Resolution Neutron Scattering A major facilitator of access to the NCNR instruments by external users is the NSF, which supple- ments NIST support for the Center for High Resolution Neutron Scattering at the NCNR. CHRNS consists of six instruments: the 30-m small-angle neutron scattering (SANS) instrument at NG-3 (neu- tron guide 3), the ultrasmall-angle neutron scattering (USANS) instrument, the spin-polarized triple- axis spectrometer (SPINS), a time-of-flight disk-chopper spectrometer (DCS), a high-flux backscatter- ing spectrometer (HFBS), and a neutron spin echo (NSE) spectrometer. The SANS instrument was constructed using NSF funds, and CHRNS pays 100 percent of its operating costs. CHRNS and the NCNR each contributed 50 percent of the construction costs for SPINS and the USANS, and they share the operating costs equally. DCS, HFBS, and NSE were added to the CHRNS umbrella in 2001, and NSF's support of 60 percent of the operating costs for these inelastic scattering instruments has allowed the NCNR to expand the amount of user time available on them. Greater than twofold increases in neutron flux are provided by the advanced cold source, placed into operation in March 2002, for the longer-wavelength (cold) neutrons of importance for these instruments. The CHRNS-supported instru- ments are among those most in demand. For example, requests for usage of DCS was 3 times greater than the time available in the December 2001 proposal round and 2.5 times greater in the September 2002 round. The six CHRNS instruments hosted 440 users in 2002, including 118 graduate students. The CHRNS instruments collectively cover seven orders of magnitude in time and length scales of 0.2 to 2000 nm (five orders of magnitude), including the regions of importance for nanoscale and mesoscale science. The instruments enable scientific studies of high impact on the structure and dynam- ics of many different materials of fundamental and technological importance. SANS alone attracts about 180 users per year; they work primarily in complex fluids and gels, polymers, structural biology, and magnetic and superconducting materials. HFBS, DSC, and NSE are each the only instruments of their respective type in the United States. Because of new ideas in tuning resolution and intensity, DCS is an extremely flexible instrument covering a wide range of science. It is currently the best instrument of its kind in the world. Recent studies on DCS include dynamics of proteins encapsulated in gels, vibrational densities of states in glassy materials, diffusion of hydrogen in single-walled nanotubes, and water dynamics in mesoporous solids. CHRNS has recently decided to focus the funding that it has available from NSF and the NCNR for upgrades on two rather than three instruments, namely, SPINS and a 10-m SANS. These upgrades continue its exemplary record of improvements in instrument capabilities. The timetable for the sub- millisecond time-resolved SANS project will be extended, with a near-term focus on expanding its in, of,

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS 227 science case. This is a commendable example of the NCNR's philosophy of adequately funding the highest-priority projects rather than spreading resources across all projects. CHRNS has a strong record of education and outreach activities that are favorably impacting the next generation of U.S. neutron scatterers. CHRNS funds undergraduate students who work at the NCNR as part of NIST's Summer Undergraduate Fellowship Program. CHRNS's summer schools attract more than 30 participants annually, of whom more than 30 percent are women or members of underrepresented groups. In 2002, 21 Ph.D. degrees were awarded that were based in part on work done at CHRNS instruments, with five of those going to women and one to a member of an underrepresented group. Life Sciences and the Cold Neutrons for Biology and Technology Collaboration In 2001, the NCNR joined with five universities (the University of California at Irvine, Rice University, the University of Pennsylvania, Duke University, and Carnegie Mellon University) to form the Cold Neutrons for Biology and Technology (CNBT) collaboration. This group received funding from the NIH, an impressive "first" in NIH involvement. The funding has been used to support a variety of initiatives: a new diffractometer/reflectometer for biological structure determination, time on the 30- m SANS instrument, staff members and postdoctoral research fellows (hired by the universities and placed at NIST), as well as new computer-modeling and laboratory capabilities. This support is particu- larly timely given the growth in the numbers of published papers describing neutron scattering by biological macromolecules and by complex fluids. The NCNR has made splendid use of the new NIH resources. Active collaboration on RNA is occurring with groups at Johns Hopkins University and the University of Maryland. Several new lines of research are now under way in computer modeling, structure determination, and molecular dynamics. Summer schools on neutron scattering should be particularly attractive to those studying biomolecules. The NCNR is working to show biologists and biophysicists by specific example the value of neutron scattering to an understanding of the workings of biological macromolecules. Projects that illustrate the power of neutron scattering include ribozyme folding under the influence of added counterions, com- parisons of hydration and structure of bound versus free proteins, and characterization of protein/DNA assemblies. For example, single proteins, observed free and encapsulated in porous materials, reveal differences in internal motions as well as the expected differences in rotation and translation. Diffusion of water confined in approximately nanometer-diameter pores will likely reveal properties of water on protein surfaces, in protein cavities, and especially in transmembrane ionic channels. The timeliness and impact of the results from these projects could be improved with the addition of another person doing molecular dynamic simulations to help interpret the scattering data and with the addition of another experimentalist on SANS. Research Facilities and Reactor Operations The Research Facilities Operations Group has the role of managing shared resources in support of the neutron science program at the NCNR. The activities of the group include beam-line operations; instrument maintenance, development, and upgrades; facility operations; and software support. This group consists of 40 staff members, including scientists, engineers, and technicians, of which 33 are NIST employees. This staffing level allows the NCNR to maintain effective support for instruments at approximately 4.5 support staff per instrument, which is essential for the efficient running of the facility.

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228 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 The group is well organized and efficient; morale among the staff is high. In an environment in which the workload is demanding and varied, clear priorities have been set and communicated to the teams. The panel fully endorses the decision to give highest priority to maintenance and support for running instruments, to be followed by support for instruments under development. The Research Facilities Operations Group has 10 major development projects under way, including new instruments and upgrades to both instruments and support systems, all of which are progressing well. Understanding that robust instrument development is essential for the continued health of the facility, the NCNR maintains a target of completing 1.5 to 2 new instruments or major instrument upgrades per year. In addition to maintaining operating instruments, this goal will create a severe load on the staff of the group it is well recognized that an engineering group of 12 staff would be required to maintain this development plan. Current instrument development obligations will consume all NCNR engineering resources for the next 5 years. This group is following commendable paths to optimize the use of resources, including the follow- ing: increased emphasis on standardized components and approaches, increased use of external engi- neering and manufacturing, a move toward team-based design efforts, and the installation of automated facility monitoring systems. The management and staff of the group understand that these efforts should be expanded to ensure that resource sharing and communication are achieved across all U.S. neutron (and X-ray) facilities to prevent any duplication of effort. Despite these moves toward increased effi- ciency, it is clear that without increased support, the group cannot sustain the level of support required for the operation of instruments. An appropriate (however lamentable) solution would be to remove selected instruments from the user program as new instruments come online in order to maintain the crucial level of 4.5 support staff per instrument. The $6 million neutron science initiative in NIST's FY 2003 Presidential Budget is critical to maintaining the growth of the NCNR as a major user facility. The NCNR management recognizes that setting priorities for new instruments and upgrades re- quires a clearly defined process involving input from in-house scientists and the user community while maintaining an overview of the broader U.S. neutron scattering context, including the new opportunities that will be available at the SNS in the future. The NCNR management is participating actively in regular meetings of the U.S. neutron facility managers, as recommended by the Interagency Working Group on Neutron Scattering, in order to address issues of resource sharing and coordination of facility development. The panel was impressed by the highly successful design, installation, and operation of the new cold neutron source. The performance easily meets the predictions, with an increase of more than a factor of two in flux at long wavelengths. The achieved reliability of 99.95 percent is truly impressive and is the direct result of the careful design of a passive control system and modification of the compressors. The panel commends the NCNR management for its foresight in building two cold neutron source inserts in parallel, one of which will serve as a spare, hence ensuring reliable operation of the facility with reduced incremental cost. Additional successful improvements, which have significantly enhanced the performance of the instruments, include replacement of the crystal filter for the SANS instrument with a new optical filter providing a significant increase in flux at long wavelengths, and a rebuilding of the channeled guide for the DCS spectrometer that has led to improved performance at high energy resolution. Installation of a new optical filter for guide NG-7 is pending a suitable shutdown opportunity. The Research Facilities Operations Group has an important role to play in the success of the NCNR as a user-based neutron facility, and it is achieving this role efficiently and reliably. A transparent organization has been set in place with clear priorities and goals. Management of the group requires an unusual combination of engineering capability, scientific knowledge, and understanding of the needs of

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS 229 the user community. The Research Facilities Operations team recognizes the importance of maintaining this expertise as the facility develops. The Data Analysis and Visualization Environment (DAVE) project was initiated in November 2001 in response to a clear need for a user-friendly, coherent data reduction, visualization, and analysis software. The progress made by the eight-member development team, which combines the expertise of instrument scientists and computer scientists, is impressive. Since the public release of the DAVE software in December 2002, it has been employed by users of NCNR spectrometers and members of the neutron scattering community analyzing data obtained on neutron spectrometers all over the world. The DAVE development team recognizes the importance of incorporating standardization among software packages developed at different facilities. Although based on an internal data format, the software will support standard formats such as NEXUS. The future maintenance and development of DAVE will require an allocation of significant resources. The panel commends the efforts of the DAVE team to share the development of the software environment with users outside the NCNR and with other facilities. The major emphasis of the Reactor Operations and Engineering Group this past year has been on matters related to the anticipated relicensing of the reactor for 20 more years of operation. Considerable care has been taken to identify, examine, and anticipate all of the technical and logistical issues related to both regulatory matters and to reliable operation for future world-class scientific research. All of these activities are progressing on schedule to meet the anticipated submission date of the relicensing applica- tion to the Nuclear Regulatory Commission in 2004. One of the very valuable features of the NCNR reactor is the well-established characterization (energy spectrum, and so on) of the neutron fluxes that it produces in its various possible operating modes. It is very important that great care be taken to avoid any future modifications of the reactor that would result in destabilizing that scientific knowledge base or the capability of the reactor to continue to produce neutron fluxes necessary for cutting-edge research. Completed in 2002, the new cold neutron source more than doubles the neutron flux in the 15-\ to . . . . . . ... . _ . . do. . . . . . . ... 20-5 wavelength range with lesser, but still significant, gains at shorter wavelengths. A new electrical supply for the reactor building was installed, with improved transformers and switchgear. This improvement provides increased capacity for both current and future operating and experimental facility loads. New cooling towers, required for the extended life of the reactor under relicensing, became opera- tional. The improved design of the towers successfully eliminates the large highly visible water vapor plumes in cold weather, which have aroused repeated statements of public concern. The reactor uses semaphore-type control rods (shim arms). New shim arms and shim arm assem- blies have been fabricated to meet future needs. There is now on hand a shim arm supply of at least 4 years. Shim arms for an additional 28 years are currently being manufactured. Increased reserves of nuclear fuel and heavy water are being developed to assure future reliable and scientifically stable operations in the extended licensing period. A new digital instrumentation console for reactor operations and safety monitoring is being de- signed with the assistance of Brookhaven National Laboratory. Care is being taken to ensure that in the new design no important safety features (e.g., "operator friendliness") are lost. A mock-up will be built near the present control room to allow the reactor operators to consider it and offer their comments. One new area of regulatory activity that has expanded greatly over the past year is that of physical security. The Nuclear Regulatory Commission has issued a number of directives requiring attention to this issue and significant expenditures. A new vehicle-exclusion area has been constructed, new vehicle

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230 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 barriers have been installed, and further improvements are under way. Additional surveillance equip- ment has been installed. The availability of the NIST Research Reactor at power in 2002 has been outstanding, with 153 days of full power, 94 percent of which were operational. Considerable attention continues to be given at all levels to operational safety, radiation protection, and industrial safety. Nuclear Regulatory Commission inspections have emphasized all of these, and the commission's inspection reports have been very favorable. Because of the number of high-radiation-area maintenance tasks, exposure of personnel to radiation was somewhat higher last year than in the past, but levels of exposure are still acceptably low because of the strong NIST commitment to ALARA exposure as low as reasonably achievable. The industrial safety record is also very good. One minor, lost-time accident occurred last year, but there have been none in previous years. The Brookhaven National Laboratory has been awarded a contract to perform new safety analyses of the reactor using state-of-the-art calculation methods. For the cases examined to date, the new analyses show that calculations originally performed in licensing the reactor were conservative. This effort will be completed in 2003 and will be submitted to the Nuclear Regulatory Commission in the relicensing Safety Analysis Report. One issue receiving much attention is the condition of the aluminum reactor vessel resulting from its neutron bombardment and how well it is expected to perform out to the end of the 20-year relicensing period. In-house assessment of this question using data from the Brookhaven research reactor thus far appears to indicate that there is no serious problem. If the final results of the assessment suggest the need for additional data to support the Safety Analysis Report, samples can be taken from a rabbit tube in the reactor vessel. Another problem area is the thermal column cooling system tank, which began leaking heavy water. Close examination of the tank showed that the leaks were at welds, which could not be repaired in place. To deal with this problem, several actions have been taken. The heavy water supply for the thermal column cooling system has been isolated from the reactor heavy water primary cooling system, and the thermal column now has its own heavy water supply. Any leakage is collected and saved. Reducing the flow of cooling heavy water to the thermal column has caused the leaks to self-heal, so currently there are no detectable leaks. To ensure that a replacement tank is available on short notice if the leaks resume and increase, a completely new tank has been fabricated and will be delivered very soon for installation, if needed. In the meantime, if necessary, the heavy water could be replaced by ordinary water and the reactor could continue to operate, but without the thermal column. A more troublesome problem is the leakage occurring in the copper tubes carrying the cooling (light) water in the biological shield. The precise cause of this leakage has not been determined because of the inaccessibility of the tubes, which are embedded in cast-in-place lead and concrete. Various devices are being used and/or developed to examine the tube walls' interior surfaces, but the small size of the tubes and right-angle bends have made it very difficult to introduce surveillance instruments at the locations of leakage. Work on this problem is ongoing. Currently the leaking tubes are resealed with a propriety solution applied during shutdowns. Pressure indicators on all of the individual tubes are regularly monitored manually from the C-100 catwalk installed to provide safe access to the contain- ment ring header. A contractor using a test rig onsite is developing what might be a better method of sealing the leaks by pumping a different proprietary mixture into the tubes. If this is not successful, the problem may continue to be treated by sealing the leaking tubes with the current procedure, a process that has worked for 15 years. The problem is more of a nuisance than a threat.

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS Program Relevance and Effectiveness 231 The primary customer of the 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 variety of fields. The panel commends the NCNR staff for its continued focus on effectively serving these users. The NCNR provided the basis for more than 318 papers accepted or published in archival journals in FY 2002 and for 79 invited talks by NCNR staff. The NCNR hosted a summer school in FY 2001 on structural studies with SANS and reflectivity, which was attended by 40 people, mostly graduate and postdoctoral students. The NIST neutron facility has been a leader in serving industrial needs at neutron sources. During the past year, the facility served a total of 1,776 participants, including researchers from 47 different industrial organizations and 127 (U.S.) universities, many of whom are working on industrial projects. Many different models are used to support the users of the 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. A past concern has been the quality of the data-gathering and analysis tools available to users, and the neutron science and Research Facilities Operations personnel have devoted a significant effort to improving the situation. New tools now available to users include the DAVE software for treating and analyzing time- of-flight, backscattering, and triple-axis data sets. In addition, the data reduction and analysis software (IGOR) for SANS and USANS data is widely and easily applied by users. The Program Advisory Committee (PAC) allocates beam time on instruments that are available to the general scientific community. This advisory committee is composed of 8 to 10 neutron scientists (not from the 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 has exceeded the number of days available in several cases by a factor of two 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. When the panel 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. The PAC workload has also been streamlined by a new online proposal evaluation system. A past concern of the panel, NCNR management, and the PAC itself has been the rising number of proposals that the PAC must review. 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 has examined the produc- tivity of the first round of program grant awardees with respect to the level of output (i.e., publications) and has found that it is excellent. Previously the panel recommended that the PAC and the 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 has been adopted. Center Resources The NCNR continues to produce amazing accomplishments with very little money compared with the budgets of, for example, DOE user facilities. The NCNR is run in a highly cost-effective and

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232 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 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, with an expansion of CHRNS and funding of CNBT. With the increasing emphasis on soft matter and biomolecular studies in the NCNR, the panel continues to believe that exploring potential partnerships, recruiting new researchers, and/or establish- ing a visitor program would offer advantages of increased synergy between theory, experiment, and interpretation. The panel applauds current management support of the synergies between theory/model- ing and experiment and encourages continuance of this trend. Staff morale is extraordinarily high at the 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. Staff are appreciative of the collegial and scientifically exciting environment that NCNR man- acement has fostered. With the construction of the SNS under way. recruitment of some of the NCNR ~ I, stats to this taclllty has begun, though only a tew people nave elected to go to the ANN. N~NK management has expressed the view that training both users and (a few) employees for this large new facility is part of the NCNR's responsibility to the neutron community. Yet, NCNR management ~ 1 1 ~ ~ O . . . . ~ . ~ . . . . . . ~ . . ~ continues to take a longer-term view of the N(:NK7S ongoing value to the Umted States and the U.~. research community by supporting internal facility improvements (redoing laboratory space for biologi- cal use, for example) and instrument upgrades appropriate for thermal neutrons, by addressing security needs, and by pursuing relicensing. Since there is little likelihood of increased resources, the panel commends NCNR management for scenario planning that includes evaluating possible vertical cuts in instrumentation support rather than horizontal cuts that would result in more generally ineffectual instrumentation and project support. Each year, the panel comments that three of the four most senior managers at the NCNR will shortly be or already are eligible for retirement. The 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 the NCNR. The transition plan and process will deserve close attention by the MSEL and NIST management, and the panel believes that all parties recognize this need. The panel also notes that transitions and change, while potentially sources of tension and stress, can also be times of great opportunity: The next few years will also give the NCNR a chance to consider new focus areas and to move in new directions. Members of the center staff are aware of the coming transitions but somewhat worried that their current insularity may leave them unprepared to deal with future change or that the current collegial atmosphere may degenerate into squabbling over budget and instrument-support resources. The issues related to succession planning and training are particularly critical in the reactor opera- tions area. The 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. Re- cently, however, the number of personnel retiring has increased, and replacements have had to be recruited. Succession planning and searches for qualified candidates should continue to be conducted well in advance of anticipated vacancies. Successfully completing the current search for a nuclear engineer is critical to maintaining the high level of ongoing reactor operations. The panel commends the proactive stance that NCNR management is taking in upgrading to indus- trial safety standards. However, there is cause for concern over difficulties in meeting new security

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MATERIALS SCIENCE AND ENGINEERING LABORATORY: DIVISION REVIEWS 233 requirements with little or no increase in funding and personnel resources to make needed changes to computers and computer security. The number of reactor-licensed operators at the NCNR has grown to 20, providing a more comfort- able staffing level than that of several years ago. Several new operators have been hired and have qualified as senior reactor operators. However, several senior operators are approaching the time when they may choose to give up active employment. The panel believes that the development of a plan to systematically capture the corporate knowledge of all senior employees at the NCNR would have substantial long-term benefits. This may be particularly important in the future, because new operators coming out of the military nuclear service appear to be less broadly trained than operators were in the past. While knowledgeable in matters focused on control room operations, they do not have the general breadth of technical training outside of the control room that is important for successful accomplishment of the NCNR mission. Responsiveness to Panel's FY 2002 Assessment The panel believes that the NCNR has been responsive to comments and suggestions provided in past assessment reports. Most of the issues raised in those reports are long term, and the panel looks for annual progress rather than complete resolution. For example. succession planning and the training of ~ . ~ ~ . ~ ~ . ~ future leaders are serious tasks at the NCNR, given the demographics of the current management personnel and of the staff in reactor operations. Each year, the panel 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. Resources continue to limit the effectiveness and scope of the center. Every effort should be made to protect and enhance the funds available to NCNR. Other examples of positive changes at the NCNR reflect its responsiveness not only to the panel but also to the facility's user community. Improvements in the data reduction and analysis software avail- able to users, improvements in the support of ancillary instrument equipment, and improvements in the proposal process all responded to concerns expressed by the panel and the users and should, therefore, be commended. The panel raised issues in the FY 2002 report:3 two key issues, the center's responses, and the panel's assessment of those responses are given below. First Sample Issue Panel comments in FY 2002 report: "The scientific output of the team in crystallography is of high quality, although, due perhaps to the small size of the team and the demands of supporting the BT- 1 diffractometer, its scientific projects tend to move forward slowly. The team should develop a new project or research topic that is uniquely suited to being tackled with neutron diffraction." Epp. 203-2041 Center's response: "We believe that our research on zeolites and other oxides is world class, and especially suited to neutron methods. In line with the concerns expressed, we have strengthened our efforts in this area." 3National Research Council, An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002, National Academies Press, Washington, D.C.

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234 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 Panel's evaluation of center's response: The panel commends the center's management for addressing this concern. The merging of theory and scattering experiments on clathrate hydrates and the integration of temperature-dependent structural crystallography with studies of electronic transitions in complex oxides are noteworthy as these studies are well-suited to investigation using neutrons. Merging complementary X-ray and neutron structural studies of zeolites and mesoporous materials with molecu- lar and mesoscale modeling should yield important results on difficult materials of notable scientific and industrial interest. The panel notes the efforts within the crystallography team to support future capabili- ties at SNS by investigating new image plates and detectors and developing new data interpretation algorithms. Second Sample Issue Panel comment in FY 2002 report: "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." [p. 2061 Center's response: "We agree with the concern, and anticipate that the CNBT consortium will be a prime element in this effort. We are pleased to note that a Director has been hired Dr. Mathias Losche, a recognized expert in membrane biophysics. Additional efforts will begin when Mathias settles in at NIST in the next few months." Panel 's evaluation of center's response: The center's CNBT consortium will be a prime element in this effort. A consortium director has been hired, as mentioned above, and this will enable progress.