Chapter 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 1998 Chapter 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 1998 PANEL MEMBERS James E. Nottke, DuPont Company (retired), Chair Robert L. Brown, The Gillette Company Stuart L. Cooper, University of Delaware John A.S. Green, Aluminum Association James D. Idol, Jr., Rutgers University Lawrence C. Kravitz, Consultant, Rockville, Md. Frederick F. Lange, University of California, Santa Barbara Merrilea J. Mayo, Pennsylvania State University Donald E. McLemore, Raychem Corporation Boyd A. Mueller, Howmet Corporation Donald R. Paul, University of Texas at Austin Dennis W. Readey, Colorado School of Mines Walter L. Winterbottom, Alumax Engineered Metal Processes, Inc. Submitted for the panel by its Chair, James E. Nottke, this assessment of the fiscal year 1998 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 19–20, 1998, and documents provided by the laboratory.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 LABORATORY-LEVEL REVIEW Laboratory Mission According to NIST documentation, the mission of the Materials Science and Engineering Laboratory (MSEL) is to stimulate more effective production and use of materials by working with materials suppliers and users to assure the development and implementation of the measurements and standards infrastructure for materials. The programs within the MSEL are all supportive of the mission. The programs reviewed by the panel appeared to be targeted at measurement methods, Standard Reference Materials, or Standard Reference Data for materials users and suppliers. The laboratory works with various members of the supply chains to assist them in making the best use of advances in standards and measurement technology in the area of materials. Efforts are currently under way to use the Internet as a more efficacious way to disseminate results and inform potential partners of relevant activities. These efforts should enhance the effectiveness and productivity of the laboratory and help it to efficiently fulfill its mission. Technical Merit and Appropriateness of Work The projects undertaken by the MSEL generally have excellent technical merit and are conducted close to or at the current state of the art. The findings and teachings of the laboratory are held in the highest regard by technical personnel in industry in both the United States and abroad. Such standing is important if the laboratory is to continue to have a positive impact on the materials supply chain. Several examples of the quality and impact of the laboratory's programs are described in the divisional reviews below. The laboratory continually initiates new projects, and the involvement of industry in the selection process via topical workshops has kept the portfolio of programs current with needs of the commercial sector. The divisions balance their own work on new methodologies with the development of new programs across division or even laboratory boundaries. This flexibility has enabled several multidisciplinary projects to be conducted in an efficient manner. As originally observed by the panel in the 1997 assessment, the MSEL, and other similar organizations, are currently undergoing a major transition in the ways that they disseminate technical information. Although publications, conferences, and first-hand discussions will continue to be important, a rapidly growing segment of the user community gathers information and conducts significant amounts of business via the Internet. If the laboratory is to maintain its image as the premier source of measurements and standards technology, NIST must have a highly effective presence in cyberspace. In the panel's judgment, the MSEL has made significant progress in this area since last year 's assessment; the new materials on the laboratory Web site are of excellent quality and very easy for users to access. Keeping the information current, maintaining suitable and up-to-date links to other major sources, and extending the existing Web information need to remain high priorities. Another way in which the laboratory has made a notable improvement in dissemination methods is the development of “Technical Notes” within the Materials Reliability Division. These

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 documents are a new technique that allows division personnel to communicate a detailed understanding of measurement and standards procedures to their general users. Impact of Programs The attached reports on individual divisions mention several examples of the impact of laboratory programs on various industries. The increased focus of program planning on the planned outcomes and the impact of newly initiated projects should further increase the value of innovations delivered by the laboratory to suppliers and users of materials. Laboratory Resources Funding sources1 for the Materials Science and Engineering Laboratory (in millions of dollars) are presented below:   Fiscal Year 1997 Fiscal Year 1998 (estimated) NIST-STRS, excluding Competence 31.4 31.1 Competence 0.2 0.0 ATP 3.4 2.7 Measurement Services (SRM production) 1.0 0.7 OA/NFG/CRADA 6.6 5.6 Other Reimbursable 0.6 0.4 Total 43.2 40.5 Staffing for the Materials Science and Engineering Laboratory currently includes 209 full-time permanent positions, of which 174 are for technical professionals. There are also 47 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers. 1   The NIST Measurement and Standards Laboratories funding 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 it is allotted 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 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.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 The balance of funding sources is judged by the panel to be appropriate. The laboratory is able to control its own program portfolio, and yet other agencies can still contribute to work that allows them to benefit from the unique expertise and equipment found in this laboratory. The panel applauds the increased congressional appropriations for construction, renovation, and facilities and looks forward to a resulting improvement in facilities and capabilities. In the MSEL, only the ceramic thin films effort is judged to be directly hampered by facility inadequacies at this time. DIVISIONAL REVIEWS Ceramics Division Division Mission According to NIST documentation, the mission of the Ceramics Division is to stimulate the more effective production and use of ceramic materials by working with suppliers and users to assure the development and implementation of essential measurements and standards. The Ceramics Division's mission statement parallels the NIST mission. Moreover, the activities within the division are consistent with and accurately reflected by its mission statement, as the division strives to provide measurement methods, SRMs, and Standard Reference Data for materials producers and users. The seamless manner in which projects increasingly traverse divisional boundaries is a clear indicator that the mission of the division is well integrated with the missions of the MSEL and of NIST. In addition, the panel observes that the division chief continues to improve the programmatic conformance to the NIST mission through his reorganization of the division. His strong leadership, enthusiasm, and direction have a positive impact on the staff and on the projects. Technical Merit and Appropriateness of Work The Ceramics Division is now the largest or one of the largest ceramics research groups in the United States, and it has an historical reputation for excellence. The division programs are well directed at the mission of developing measurements and standards. Nevertheless, the management realizes that this division cannot be the leader in all areas of ceramics research. Accordingly, the senior personnel have chosen to concentrate on fields in which the division can have unique impact and are targeting areas that are clearly linked to industrial need on a national scale and also are relevant to the production of standards, data, or reference materials. The panel requested an extensive review of the work on thin films processing, since this program was formed recently from a merger of several other projects and groups and now uses a large fraction of the personnel and resources available to the Ceramics Division. Although most projects are chosen to be in areas where the division has the expertise and resources to make the most impact, the work in thin films is slightly different. This focus was selected not so much

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 because of existing expertise but more because of the perceived increase in importance of the area and the need to provide a focus for a significant fraction of the division's research. Ceramic thin films are undeniably important scientifically, technically, and industrially. Inorganic, single-crystal, and polycrystalline thin films have been and will be used for a wide variety of device applications including but not limited to nonvolatile memories, dynamic random access memory chips, pyroelectric detectors, field emission displays, microwave devices, and wear-resistant coatings. Since the industrial effort in thin film ceramic technologies is spread across a sizable and diverse group of small and large companies, a focal point for the standards and testing methodologies used in this field is sorely needed. In response to this need, several years ago division management chose to emphasize the area of thin films and consolidate people, projects, and other resources into this area. Several challenges exist when a research program is being developed in thin films. One is the diversity and breadth of the field, and another is the sheer number and kinds of materials used. Further challenges arise from the many types of devices of interest and the large number of industries of all sizes involved with the deposition and characterization of thin films. Finally, the rapid rate of industrial development in this field threatens to outpace the rate at which standards and testing methodologies can be created by NIST. One way to cope with all these issues and to ensure that the results of the Thin Film Group's efforts remain timely and technologically on target is for the Thin Film Group to establish and maintain a mechanism for formalized, periodic interaction, review, and guidance by an external advisory group. As an example of an issue where such a board might be helpful, the panel noted that two of the NIST thin film research areas, work on (Ba, Sr)TiO3 films for high dielectric applications and on modeling of film growth via laser ablation, have the potential for large-scale industrial impact, but both need to be well matched with industrial collaborators to enable the work to move beyond the bench top. An external advisory board could assist the NIST scientists in locating appropriate and compatible industrial collaborators in such instances. The thin films work is a new program, and it requires careful supervision for the reasons discussed above. However, even at this early stage, some very interesting results have been produced. For example, the formation of amorphous films appears to be related to whether thermodynamics would predict a two-phase mixture for the given composition. If this is a general result, it could have significant implications in a number of important applications of thin films, primarily in the electronics area. Most of the other programs in the Ceramics Division were not evaluated in as great a depth this year. However, it appears to the panel that the other projects continue to be technically important and of high quality. Some examples of noteworthy work are described below. The recent expansion of the Powder Characterization Program to include processing appears to be progressing well. Several large and small companies have recently joined the NIST-organized consortium. Many of the proposed research areas, such as the dispersion of dense suspensions and the replacement of mercury for porosimetry with a nontoxic alternative, reflect the new focus on how ceramic powders behave during the subsequent forming processes. This new work is of interest to and well supported by industry. Several consortium meetings have been held at NIST to help define industrial needs and to educate industrial representatives about the expertise available at NIST and the MSEL's strong commitment to industry. The next meeting will be a large symposium at the American Ceramic Society's annual meeting. This event

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 will combine presentations by industrial speakers with those by scientists from research and academic organizations. The Phase Equilibrium Program currently focuses on materials for wireless and microwave communications and on high-Tc superconductors. The discovery of improved dielectric materials is essential to continued progress in the rapidly growing wireless communications industry. Last year the panel was able to review the phase equilibria data generated at NIST for the wireless and microwave industry. This data set will make the development of new materials much easier. The recognition that NIST-Boulder possesses world-class expertise and facilities that allow the high-frequency electrical characterization of these materials has resulted in closer collaboration between NIST scientists in Gaithersburg and Boulder. It is the panel 's expectation that this increase in interactions will lead to improved fabrication and characterization of these materials and ultimately will provide new materials for industrial applications. On this year's site visit, the panel was impressed by the second general material class now being studied: the oxide superconductors in the multicomponent Bi-Pb-Ca-Sr-Cu-O system. These materials are gaining greater use for high-current transmission in the energy industry. Needless to say, the graphical representation of this six-element system is a complex issue in itself, perhaps even more complex than the intricate suite of experiments required to verify the phase relations. The group at NIST is one of the few teams in the world with the capability to realize the experimental results for such a complex, but important, materials system. The Coatings Program recognizes that the properties of the plasma-deposited coatings used by a wide variety of engine manufacturers strongly depend on the coating microstructures. By developing methods for the accurate prediction and measurement of these microstructures, the program can greatly improve engine performance. In this project, NIST itself does not have a large research effort but serves as a nucleus to bring industry and university people together to share information on coatings and properties. Therefore, for a relatively modest expenditure, a great deal of useful information is being exchanged. The fundamental design methodology for brittle materials was essentially established at NIST. More current research on deformation due to creep of ceramics and development of related standard test techniques are other examples of the leadership role NIST continues to play in improving the understanding of the mechanical behavior of ceramics. Within this group, the Theory and Modeling Program has coupled, through computer simulation, the mechanics and properties of polycrystalline materials. The potential of these simulations as a methodology for materials design will certainly aid in the development of high-temperature structural components and in the use of functional inorganics in device technology. In addition, NIST's continued work on the important task of establishing mechanical properties standards is widely appreciated by the technical community. Impact of Programs Current formal routes of dissemination include sponsorship of workshops, periodic meetings held by various consortia, staff presentations of papers and attendance at professional meetings, and participation of staff members in multiple interagency and standards committees. In addition, several of the programs, like those discussed in the previous section, have a significant number of industrial partners. These collaborations suggest that industry views working with

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 NIST as a way to gain useful information. Also, direct involvement of industrial participants makes information exchange very efficient. Active industrial collaboration in research projects is a mechanism of immediate technology transfer that is far more effective than reports, presentations, or technical papers. It is unclear, however, what mechanisms can be used to have the maximum impact on companies that do not participate directly in NIST research. The most rapidly growing information dissemination mechanism is the World Wide Web. Last year the panel suggested that NIST-level management could take a more active role in establishing guidelines for managing information on the Internet. However, this year the panel noted that as electronic communications are exploding at a phenomenal rate, the free-enterprise system seems to be working quite well. Nonetheless, NIST can still set the standard for technical information exchange by example. If the NIST Web pages do an excellent job presenting data, they could become the undisputed quality standard that all other technical organizations naturally follow. Such a leadership position in Web-based data dissemination is critical to NIST's future. Although achieving this position is certainly a formidable task, NIST's charter as a technical information provider makes this a goal of paramount importance. To illustrate some of the issues discussed above, some specific comments on the Ceramics Division Web pages are offered. First, easy accessibility to precise technical data is the scientific community's greatest need and should be the primary function of the division's site. The High Temperature Superconducting Materials Database currently available under the data link on the division's home page is an excellent example of the quality of data and data presentation that one should be able to expect from NIST. The staff is encouraged to continue to add such databases to the site. Assessing the impact of the division's programs on industry is quite difficult. One criterion that might be used is the frequency with which NIST-developed standards or data are bought, referenced, or used by industry; such counting should include secondary and trickle-down effects. Another obvious assessment criterion is whether industrial partners continue to participate in a CRADA or a consortium. The panel believes that the external economic impact evaluation of the ceramic phase diagram program greatly understates its value. Since the study only examined the impact on first-tier users, the methodology of this analysis did not seem to realistically estimate the actual economic benefits experienced by the affected industries or by society as a whole. There are isolated but notable instances where the technical work has been of excellent quality and the industrial impact has not been as broad as it should be. An example is NIST's effort to provide rational design criteria for brittle materials, particularly structural ceramics. Although these design criteria have been implemented by high-technology users, such as the designers of advanced heat engines, it is unfortunate that the much larger structural ceramics industry has not adopted the criteria.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 Division Resources Funding sources for the Ceramics Division (in millions of dollars) are as follows:   Fiscal Year 1997 Fiscal Year 1998 (estimated) NIST-STRS, excluding Competence 9.3 9.3 Competence 0.2 0.0 ATP 0.9 0.7 Measurement Services (SRM production) 0.3 0.2 OA/NFG/CRADA 1.4 1.6 Other Reimbursable 0.2 0.1 Total 12.3 11.9 The division has made a conscious effort to wean itself from OA funds and is currently not taking on additional OA funding without an explicit technical justification. This strategy allows the division to define programs based on technical merit and potential impact, rather than on momentary whims of federal or industrial funding agencies. This situation may change if the base federal funding earmarked for NIST continues its historical slow decline. Such a gradual decrease in the budget will mean that fewer technical people can be supported and the overall program scope will contract. The division has access to some very special, and in some cases unique, facilities. These include the laser ablation mass spectrometer, the microtribology laboratory, the nuclear magnetic resonance (NMR) imaging facility, beam lines on the NIST reactor, beam lines on synchrotron light sources, and a host of state-of-the-art mechanical testing equipment. Staffing for the Ceramics Division currently includes 62 full-time permanent positions, of which 53 are for technical professionals. There are also six nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers. The quantity of available space does not appear to be an issue at the moment and is unlikely to be an issue in the near future, since the number of division personnel is not increasing. Last year, it was noted that the lack of vibration-free and dust-free, clean-room space for film and coatings research severely constrains the research that can be undertaken in these technologically critical areas. This issue could be resolved by the construction of the Advanced Measurement Laboratory, since the division's nanoscale measurement efforts would be slated to move into 16 rooms in the new building.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 Materials Reliability Division Division Mission According to NIST documentation, the mission of the Materials Reliability Division is to develop measurement technology and provide standards technology to improve the quality, reliability, and safety of engineering materials. The division mission directly supports the programs of the MSEL and is congruent with the mission of NIST. The scope of the technical effort is appropriately limited in order to maintain critical mass within each project. The areas chosen for specialization appropriately complement other national efforts without duplication and address nationally important sectors of the measurements and standards arena. The division's current skill bases center on intelligent processing of materials, ultrasonic characterization of materials, and micrometer-scale measurements for materials evaluation. The division has shaped the present array of projects to maximize the capability of the limited number of staff members to develop and promote industrial measurement technology and standards, in conformance with the laboratory and NIST missions. Technical Merit and Appropriateness of Work The panel found that the projects undertaken in the Materials Reliability Division generally have high technical merit. These efforts include the extension of ultrasonic measurement technology to the characterization of material microstructure features such as texture, grain size, strain, dislocations, and recrystallization; the use of electron microscopy for nanoscale measurement of electronic packaging and thin film flaws; and the development of the measurement technologies required for the real-time control of the processing of structural materials. These NIST-funded programs address the measurement technology and standards requirements defined by the major MSEL thrusts. Projects to support SRMs for industry are also undertaken. The programs are therefore entirely appropriate to the NIST mission. An example of the high-quality work performed in this division over the past year is the computational work for the Acoustic Block Characterization project. Researchers have mathematically modeled the various error contributions to the measured acoustic transit time. This scientific method could be extended to all of the acoustic techniques employed in the division. The application regime of each measurement technique would then be defined quantitatively. Employing the expertise of physical metallurgists would be helpful for proof testing these quantitative limits. The overall technical advancement within the division over the past several years reflects effective organization and efficient execution of projects. The division devotes considerable effort to disseminating the results of the programs to industrial users. This effort includes leadership and participation in standards-setting committees, attendance at conferences and workshops, and publications. In addition, increased planning effort is being directed toward the a priori definition of expected project outputs. Planned outputs are now being defined as either new measurement techniques or as standard samples, and the potential methods of output dissemination are also addressed earlier in the projects.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 This year the division has initiated a Materials Reliability Series of substantial Technical Notes to offer industrial users a comprehensive background in specific measurements and standards procedures. This commendable program could be further improved by the development of a style guide for these notes. Such a guide would assist authors in shaping their notes into a uniform tutorial format optimized for user comprehension. The publication of two or three high-quality Technical Notes each year would be a reasonable goal for the division. Impact of Programs The current portfolio of projects is producing a steady stream of measurement and standards results. The division appropriately mixes work that produces short-term outputs and programs that build skills for longer-term impact. The effort to provide a national center for Charpy standard materials and the planned initiative toward a U.S. acoustic block standard are examples of work designed to have an immediate impact. The U.S. Nuclear Regulatory Commission (U.S. NRC) initiative to measure the remnant lifetime in nuclear power reactors, if successful, will also have a high impact on a national scale in a very short time. The effort on electronic packaging will have an immediate effect, which will result in a succession of impacts that may continue over the next 2 to 3 years. One underlying element of this program's success is the relationships developed with the microelectronics packaging industry. The panel hopes to see these interactions maintained and expanded. The work on advance acoustic sensors has the potential for impact over a middle and longer time range. The economic impact of these projects is very difficult to assess, and the results are subject to a high degree of uncertainty. The division's measurement technology efforts address major industry sectors, and therefore such contributions to these sectors may be reasonably expected to have a substantial impact. Division Resources Funding sources for the Materials Reliability Division (in millions of dollars) are presented below:   Fiscal Year 1997 Fiscal Year 1998 (estimated) NIST-STRS, excluding Competence 3.9 4.0 ATP 0.7 0.6 Measurement Services (SRM production) 0.4 0.2 OA/NFG/CRADA 0.8 0.8 Other Reimbursable 0.0 0.1 Total 5.8 5.7

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 develop and focus these projects on key industrial needs. With clearly defined goals, activities in these areas could become world class and foster core competency development. The Consortium on Casting of Aerospace Alloys, the Solder Jet Consortium, and the Lead-Free Solder Consortium are considered by the panel to be excellent examples of how NIST and industry can work together on materials issues. The efforts by the Consortium on Casting of Aerospace Alloys have been recognized by the Federal Laboratory Consortium Excellence in Technology Transfer Award. The Solder Jet Consortium identified the impurities that caused nozzle clogging, thereby extending the nozzle life from 8 hours to 1 month. The Lead-Free Solder Consortium has spawned the Solder Interconnect Design Team Consortium, which will continue and expand on previous work. In addition to the impact these three programs have already had, the bulk of the payback will occur in future years as the thermodynamic databases and models become available through commercial software and their use becomes integrated in industrial process development. The phase diagram modeling work conducted to support the Lead-Free Solder Consortium and the Consortium on Casting of Aerospace Alloys is outstanding. Although both of these programs are scheduled to conclude shortly, in the panel's view, phase diagram modeling is a core competency of NIST. The nickel-based phase diagram modeling efforts could be expanded to include the elements in the coatings on superalloys. In addition, evaluation of other alloy systems is also important to industry. For example, information about aluminum or magnesium would support initiatives such as the efforts to build lightweight automobiles. In general, phase diagram modeling affects the fundamental understanding of materials processing issues and therefore should be focused in support of other programs within NIST. The efforts in hardness standardization are pertinent and greatly benefit U.S. industry. It is often difficult for U.S. companies to band together and adequately represent U.S. interests during discussion about standards within international forums, such as the International Organization for Standardization. The ability to have NIST represent U.S. industry at these international meetings is critical. The division 's efforts to reduce uncertainties in primary standard hardness materials through better understanding of test requirements are therefore timely and well directed. The division's general work on thermophysical property measurements and techniques has fulfilled key industrial needs and supported other projects throughout the division. However, the future direction of this program was not clear to the panel. The focus of this work did not seem to be well defined, and it was uncertain what personnel and equipment would be appropriate and necessary for future efforts. In TBC characterization and thin film measurements and standards, workshops with industrial participation could help develop and focus NIST's efforts in these fields. Such workshops serve as a basis to implement world-class activities and foster core competency development. Additionally, the thermal spray program continues to evolve. A clear connection of this work with the measurement and standards component of the mission has not yet occurred. Industrial involvement may help to focus and further define activities in this area.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 Impact of Programs Over the past year, the Metallurgy Division has improved the presentation of the results of its programs. The Annual Report is more readable and more succinct. The panel found the use of quad charts to display the progress and impact of individual programs to be outstanding. In general, the division communicates its results to industry through publications and membership in consortia. Although some of the software developed within the CTCMS is available through the Internet, the laboratory as a whole could be more proactive in addressing the shift in dissemination techniques from paper-based approaches to electronic-based media. Several examples demonstrate how the work in the Metallurgy Division has an impact on various industries. A project on solder jet printing for microelectronics applications has worked with a variety of companies through CRADAs and through an industrial consortium. A major accomplishment of this work was the identification of impurities that caused clogging in the solder jets. Adjustments made by the manufacturers in response to NIST analyses extended the useful life of the jets from 8 hours to 1 month and enabled the commercialization of newer, more robust jets by a private company. NIST work on giant magnetoresistive (GMR) materials continues. These efforts are in support of the U.S. magnetic data storage industry, and this year research done in the Metallurgy Division contributed to the technological advances that enabled IBM to offer a new disk drive in which data storage is based on GMR effects. This year, the division concluded a project that determined testing methods and properties for lead-free solders. This work, done in concert with the National Center for Manufacturing Sciences and an industrial consortium, was very successful and spawned the Solder Interconnect Design Team, which works on models for predicting behavior of small-scale solder joints. The software developed by the scientists in the Metallurgy Division and the CTCMS is distributed via the Internet and has been adapted by several industrial customers, including Motorola, to assist in the design and fabrication of circuit board assemblies. A common theme throughout the Metallurgy Division is the modeling work done in collaboration with the laboratory's CTCMS. The impact of these efforts is outstanding. Staff have focused on model development, and then NIST works with outside commercial firms on tasks such as writing interfaces, providing user support, and building ports to multiple platforms. This cooperation enables efficient, cost-effective commercialization of software based on work done at NIST.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 Division Resources Funding sources for the Metallurgy Division (in millions of dollars) are as follows:   Fiscal Year 1997 Fiscal Year 1998 (estimated) NIST-STRS, excluding Competence 7.9 7.9 ATP 0.9 0.8 Measurement Services (SRM production) 0.3 0.2 OA/NFG/CRADA 2.3 1.9 Other Reimbursable 0.2 0.1 Total 11.6 10.9 Staffing for the Metallurgy Division currently includes 53 full-time permanent positions, of which 48 are for technical professionals. There are also 11 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers. This division is involved with several projects that support ATP programs. Such activities are highly valuable, but, as noted in last year's assessment, these projects often are forced to use dated equipment. Work with ATP grantees is appropriate for this division, and establishing world-class instrumentation and measurement capabilities in the relevant areas would reflect the importance of these efforts. MAJOR OBSERVATIONS Major observations made by the panel are presented below. The panel continues to be impressed by the excellent technical merit of the MSEL programs, and the findings of the laboratory are held in the highest regard by technical personnel worldwide. An example of the admirable work currently occurring in the laboratory is the growing involvement of the Center for Theoretical Computational Materials Science in the experimental projects in various divisions, particularly in polymers and metallurgy. The thin films work being conducted in the Ceramics Division is very important, and although the program is fairly young, key results are already being produced. This area of research is complex and the industry that could be affected by NIST's work is diverse. Careful management, guidance, and interaction with external experts are vital to ensure the effectiveness of this program. Dissemination via the Internet plays a key role in how much value the laboratory can bring to its customers. The MSEL is perceived as the premier source of measurements and standards technology, and a strong presence on the Web is necessary to maintain that position. The laboratory Web sites have improved since the previous assessment, but the panel continues to stress that constant maintenance, updates, and development are necessary to make full use of

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 this powerful communication technique. The laboratory obviously recognizes the importance of these activities, but it was not clear to the panel what level of support existed at the NIST level. The panel looks forward to improvements in the facilities resulting from congressional appropriations for renovations and upgrades. Currently, the program in ceramic thin films is judged to be the only effort seriously impeded by facilities inadequacies. REVIEW OF NIST CENTER FOR NEUTRON RESEARCH This annual assessment of the activities of the NIST Center for Neutron Research (NCNR) of the MSEL is based on a meeting of the Subpanel for the NIST Center for Neutron Research at the National Institute of Standards and Technology on February 18–19, 1998, and on the document NIST Center for Neutron Research: Annual Report, October 1996 through September 1997. 2 Members of the subpanel included David L. Price, Argonne National Laboratory, Chair; Alice P. Gast, Stanford University; John B. Higgins, Air Products and Chemicals, Inc.; Allan H. MacDonald, Indiana University; Theodore R. Schmidt, Sandia National Laboratories; and Gen Shirane, Brookhaven National Laboratory. Mission According to NIST documentation, the vision of the NCNR is to ensure the availability of neutron measurement capabilities to meet the needs of U.S. researchers from industry, university, and other government agencies. To serve this vision, 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 techniques, to develop new applications of these techniques, 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. In the panel's opinion, the activities of the NCNR are in full conformance with the NIST mission. In this context, the recent elevation of this organization to the status of a center within the MSEL is timely and appropriate, according to its director, and confers a level of responsibility commensurate with the NCNR's status as a major national resource. Technical Merit and Appropriateness of Work The NIST research reactor, with its associated instrumentation and scientific and technical staff, is an outstanding and unique resource for the national and international research communities. It is the only U.S. research reactor currently operating with a cold neutron source, 2   U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, NIST Center for Neutron Research: Annual Report, October 1996 through September 1997, NISTIR 6112, National Institute of Standards and Technology, Gaithersburg, Md., 1998.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 and its instrumentation for cold neutron research is, in many cases, unique within the United States. The NIST reactor's importance to the national scientific scene is intensified by the recent shutdown and uncertain future of the high flux beam reactor at Brookhaven National Laboratory. Although the Department of Energy has recently announced the decision to construct the world's most powerful spallation neutron source (SNS) at Oak Ridge National Laboratory, this project in no way diminishes the importance of the NCNR to the nation's neutron science activities. Several national advisory panels have established that the types of instrumentation and, to some extent, the scientific applications of reactor and spallation sources are quite different. Although the SNS project cannot have a major impact until its construction is complete, approximately 10 years from now, the expected investment in the development of neutron instrumentation during the design and construction phase will present a unique opportunity for the neutron community nationwide to pool ideas and experience. The staff of the NCNR, with their unique expertise in cold neutron instrumentation, should play a vital role in these discussions. Reactor and Research Facility Operations. It has been 2 years since the extensive facility upgrade was completed, and the subpanel was impressed by the continuing high availability of the reactor and the cold source. The reactor met its goal of 250 days at full power with facility reliability greater than 98 percent and with the cold source reliability greater than 99 percent. Unscheduled facility outages were held to a minimum, and most such events were related to loss of site power. There were no reportable occurrences this past year, and the NRC inspection reports were highly satisfactory. This past year the Department of Commerce also recognized the exemplary operation of the reactor facility by awarding a Department of Commerce Gold Medal to the Reactor Operations and Engineering organization. The citation noted the excellent staff, the unrivaled record of safe operation, the productivity, and the cost-effectiveness. Continued vigilance is required to maintain this level of achievement. The condition of the physical plant was reviewed and found to be excellent due mainly to successful efforts by the staff to maintain, upgrade, and replace older equipment. Currently staff are systematically reviewing the entire reactor facility in order to identify potential upgrades. The cooling tower was upgraded this year, and a complete upgrade of the reactor's heat rejection system is nearly finished. The radiation area monitors will be replaced this year, and the reactor instrumentation upgrade is ongoing and long term. A computer-based maintenance management system was initiated that will eventually enhance the availability of all systems. These facility upgrades are absolutely essential for continued reliability in operations. Significant operations and safety improvements have also been made in the guide hall. The electrical distribution system was redesigned to centralize the service provided to each major experimental station, two local cranes were installed that are dedicated and sized to individual spectrometer stations, “light” curtain enclosures that can be interlocked to the beam shutters were installed around experiment stations, and an additional helium compressor was installed to provide redundancy for a portion of the cold neutron source system. A new cold neutron source has been designed that will result in a doubling of the intensity. The new features are based on the design of the current system that has been validated by 2 years of successful operation. The improved intensity will result primarily from changes in the

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 geometry of the cold source and the cooling jacket and from the evacuation of the interior of the source. The staff plans to install the new system in the year 2000. Another major accomplishment of this year was the first shipment of spent fuel from the facility since 1988. Over 4 years' worth of spent fuel was sent out in a total of three shipments. As a result, the inventory of fission product on site was significantly reduced and space in the fuel storage pool was freed up. A new control system was also developed for spent fuel movement. The independent safety review system is in place and functioning well. The Safety Audit Committee last year examined the maintenance program in depth and recommended some changes in procedures that have been made. The on-site safety review committee is composed of members with diverse technical backgrounds and is broadly responsible for the safety of the reactor as well as the experiments. The committee is to be commended for utilizing some performance-based evaluations of operational activities. The Radiation Protection Program continues to be highly effective. The replacement of the elastomer seals in the guide tubes near the reactor could have resulted in significant exposure for the staff, however, with adequate planning and execution of the task, the total dose received was less than 1 man-rem. Relicensing of the reactor facility by the NRC appears to be proceeding in an orderly fashion. The Safety Analysis Report is expected to be finished and reviewed internally by the end of the year. The license must be renewed by the year 2004, and such a renewal would extend legal operations through 2024. Appropriately, staff use this latter date as the planning horizon for reactor upgrades, fuel procurement, and reactor component replacements. The reactor vessel has been analyzed and deemed to be satisfactory through 2030. Instrumentation Development. The subpanel was impressed by the effective manner in which the NIST staff is developing a state-of-the-art complement of neutron scattering instrumentation. Existing instruments in both the guide hall and confinement building are continually upgraded and maintained. In particular, the two instruments3 constructed with support from the NSF under the auspices of the Center for High-Resolution Neutron Scattering (CHRNS) are performing excellently and serving vigorous user communities. The subpanel welcomes the addition of an ultrahigh-resolution small-angle neutron scattering (SANS) instrument, based on diffraction from perfect crystals, to the CHRNS repertoire. Excellent progress has been made on the three new high-resolution inelastic instruments in the guide hall, at least two of which should be in use for research within the coming year. In agreement with an observation made in last year's assessment, the center has made a good start on upgrading the thermal neutron instruments, particularly the triple axis spectrometers. New monochromator drums and beam-tube shutters have been fabricated, and specific improvements have been made to a number of instruments. The subpanel was informed about and is supportive of plans for two future instruments, a new subthermal triple-axis spectrometer and a versatile biological structure instrument. The latter would provide support for the proposed new competence in biological science discussed below. Neutron Condensed Matter Science. The maintenance of an in-house scientific staff performing cutting-edge science with state-of-the-art instrumentation is an essential component of any 3   These two instruments are a 30 m small-angle neutron scattering (SANS) instrument and a spin polarized inelastic neutron scattering (SPINS) spectrometer.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 successful national user facility. The subpanel is impressed by the high quality of research being performed by the NCNR staff over a broad range of scientific fields. The Chemical Physics of Materials Group is investigating the structure and dynamics of a wide variety of condensed systems of scientific and technological interest. The research on cubane, which has received international acclaim in the past year, is being extended to inelastic scattering and modeling studies of the vibrational spectra and rotational relaxation. This combination of approaches is also being applied to more complex systems such as ribonuclease, and such an activity could help provide a basis for the proposed new initiative in biological materials. This group is especially well positioned to exploit the three new high-resolution inelastic instruments in the guide hall when they come into operation. The Magnetism and Superconductivity Group conducts high-quality work in areas of current interest. One current project studies a Fe3O4/CoO single-crystal interface. The fact that CoO changes spin direction under a magnetic field was determined using polarized neutrons. This work is important because it will help scientists choose between competing theories of the exchange-biasing effect, which is expected to be important in future magnetic information storage technology. Other recent projects include theoretical models of spin structure in layer cuprate materials that are useful in understanding trends observed in RCuO4 materials. Studies of magnetic fluctuations in the colossal magnetoresistance material R(Sr/Ba)MnO3 have produced surprising results near the critical temperature, Tc. These observations may be important in clarifying pictures of the large increase in resistance of these perovskites at the ferromagnetic transition temperature. In addition, high-resolution studies of magnetic excitation spectra in spin-ladder (SrCuO2), high-Tc (La(Sr)CuO4), and spin Peierls (CuGe(Si)O3) using the SPINS spectrometer continue to gather attention and interest from the scientific community. The Crystallography and Diffraction Applications Group conducts commercially important research on the beam tube 1 (BT-1) powder diffractometer and the BT-8 double-axis, residual stress/single-crystal diffractometer (known as DARTS). The high-resolution BT-1 instrument was upgraded with a new germanium monochromator, beam collimation, and improved shielding which more than double the intensity and provide additional flexibility with respect to instrument resolution. A diverse group of industrial, academic, and government users collected over 1,000 data sets from 320 samples in fiscal year 1997. Crystallography Group research with significant impact included locating hydrogen atoms associated with catalytically active acid sites in a commercially important zeolite catalyst and the structural characterization of gas sorption sites in gas separation materials. Research on intermetallics, ceramic coatings, superconductors, and GMR oxides also provided structural data on a wide range of high-technology materials. Improvements in sample handling, instrument control, and data analysis have initiated routine utilization of the BT-8 DARTS for residual stress and texture studies. The recent addition of a sample stress rig allows measurement of elastic compliance and the study of plastic deformation under compressive loads. Residual stress measurement experiments with industrial and government collaborators examined helicopter and aircraft materials, welds, railroad rails, thermally sprayed coatings, and infrastructure components. Measurements on reference samples provided by the Versailles Project on Advanced Materials and Standards will be used to prepare a draft standard for neutron residual stress measurements. The Crystallography Group provides a valuable contribution by developing innovative software for data analysis including upgrades to existing refinement programs and new graphical-user-interface-based tools. Tests on different samples of a new drug candidate produced very

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 similar diffraction data, and yet scientists were able to successfully analyze the data and distinguish between the samples using a visual indexing tool developed within this group. The different samples comprise low-symmetry polymorphs that probably have different physiological characteristics. The NIST Crystallographic Data Center formed new collaborative ventures with the Gmelin Inorganic Crystal Structure Database and with the Toth Metals and Intermetallics Database. These collaborations will produce a PC software product with full structural crystallographic descriptions of inorganic materials. An updated version of the existing NIST Crystal Data and Electron Diffraction Databases was released to third parties for distribution. The Surface and Interfacial Science Group focuses on neutron reflectometry studies at NIST. This work has had broad impact in a variety of disciplines including fluid physics, polymer science, magnetism, and biological membranes. Excellent projects in biological membranes include studies of lipid layers supported on self-assembled monolayers and containing poreforming toxins. Advances in inorganic surfaces are aided by the development of a molecular beam epitaxy/ultrahigh-vacuum system for in situ or ex situ growth of films. The fine resolution of the cold neutron reflectometer with polarized beam option (located at NG-1) has allowed researchers to characterize diffuse scattering of magnetic domains in cobalt thin films and to observe the destruction of such domains by a magnetic field. Reflectometry studies of swollen polymer brushes indicate an intriguing wetting transition in solvent mixtures. The subpanel was concerned that the two reflectometers used for work in this field are highly oversubscribed (by a factor of approximately 3 to 1) and this crowding may be limiting the pursuit of high-risk, lengthy experiments. The Macromolecular and Microstructure Science Group is very productive and generates excellent work. While maintaining the premier small-angle scattering facility in the country and serving a diverse community of over 200 scientists, staff also pursue very high-quality research projects of their own. Highlights from the past year include a variety of studies of block copolymers under shear, a project on the effect of pressure on polymer phase transitions, aerosol and particle studies, and increased activity in biological systems. The huge demand for SANS beam time is a tribute to the NCNR staff: By creating a world-class, user-friendly facility, they have brought SANS into the forefront of polymer and complex fluid research. When the neutron spin-echo, time-of-flight, and back-scattering machines are commissioned, the study of macromolecular dynamics is likely to join the SANS work as an important element for the research community. User Community.The NIST neutron user community appears to be highly satisfied with their access to and the quality of the research instrumentation at NCNR. They also seem content with the experiment selection and scheduling procedures implemented by the Cold Neutron Research Facility (CNRF). The subpanel received letters from the chair of the CNRF Users' Group Executive Committee, and the chair of the CNRF Program Advisory Committee (PAC), both of whom commended the efforts of the NCNR management and staff. The heavy oversubscription of some instruments testifies to the quality of those instruments and the significance of the scientific opportunities they present. However, the large number of user applications is placing a burden on the in-house staff, PAC members, and external reviewers. It may be appropriate to consider alternative review mechanisms, such as allowing frequent users to submit a single

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 proposal for projects consisting of a series of experiments, while continuing to take the needs of individual users into account. Impact of Programs The NCNR provided the basis for over 350 papers submitted to or published in archival journals in fiscal year 1997. According to a NIST citation analysis of refereed publications with NIST authors, the average impact of a neutron paper is 1.6 times the average for comparable papers published in the same journals (where impact is defined to be equal to the number of citations divided by the number for a similar paper in the same field in the same journal). In addition, NCNR staff presented 75 invited talks during the year. The NCNR also conducted a workshop on high-resolution inelastic scattering during the summer which was attended by 24 students. During the past year, the CNRF served 151 participants from 57 different industrial organizations and provided value to many more companies indirectly through support of industrial research carried out at universities. During the design phase of the cold neutron facilities, NIST solicited monetary support from industry; and Exxon Research and Engineering Company, one of the earliest contributors, helped build the first 30 m SANS. Exxon continues to support operation of this instrument and to use it for long-term corporate research and development. When necessary, they also use it for proprietary research; in such cases, Exxon pays for the full cost of running the SANS during those experiments. Currently, Texaco and IBM also support long-term projects at the NCNR. A particular example of a unique NCNR activity of national importance is the research on polymers, which draws on an active user community as well as on the high levels of expertise in this field at the center and in NIST's Polymer Division. This activity is being extended into the area of biological membranes and protein-enzyme complexes. A group of university researchers has developed a grant proposal that seeks external funding to support a buildup in biological activities at the center. The subpanel fully supports this plan. Where appropriate, NCNR staff also exploit technical opportunities in the inorganic materials area as they arise out of basic condensed matter research. Notable examples this year include the studies of exchange biasing in ferro-/antiferromagnetic layers, which may have considerable impact on magnetic storage technology, and investigation of the kinetics of the setting and hardening of portland cement, research supported by the Department of Transportation. NCNR Resources Funding sources for the NIST Center for Neutron Research (in millions of dollars) 4 are as follows: 4   The totals for the reactor include only normal operation costs. Fuel cycle and upgrade costs, totaling approximately $5.7 million per year, are excluded.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998   Fiscal Year 1997 Fiscal Year 1998 (estimated) NIST-STRS, excluding Competence 13.7 12.9 Competence 0.1 0.1 ATP 0.2 0.2 OA/NFG/CRADA 1.5 1.6 Other Reimbursable 0.2 0.1 Total 15.7 14.9 The budget shown above includes reactor operations and engineering, research facility operations, and neutron condensed matter science research. It provides for routine supply and equipment purchases, as well as for staff salaries, and includes the National Science Foundation support for the Center for High-Resolution Neutron Scattering. The apparent drop in funding from fiscal year 1997 to fiscal year 1998 reflects the fact that in fiscal year 1997, there were funds carried over from fiscal year 1996, whereas no such funds were carried over from fiscal year 1997. Staffing for the NIST Center for Neutron Research currently includes 84 full-time permanent positions, of which 78 are for technical professionals. There are also 14 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers. For the past several years, the subpanel has expressed concerns about the potential loss of reactor operations personnel through retirements. This issue has been ameliorated by the hiring of three experienced reactor operators who are expected to be licensed as senior reactor operators by the summer of 1998. No loss of operating staff has occurred in the past year, and the overlap between new and retirement-eligible personnel provides a good training opportunity. The need for additional expertise in modeling and fundamental condensed matter theory was also highlighted in previous subpanel reports. The subpanel recognizes that steps have been taken to address this issue. Collaboration with a renowned materials modeling group at the University of Pennsylvania is likely to contribute to the effectiveness of the center's science program. However, the subpanel also notes that the current search for an in-house theorist could be used as an opportunity to address the need for expertise in fundamental condensed matter theory and encourages the center to devise strategies that foster collaborations with theorists within NIST and in the community at large. Finally, the need to plan for an orderly transition from the current leadership to the next generation remains a concern of this subpanel. The outstanding and harmonious administration performed over several decades by the administrative chief, the chief of reactor operations and engineering, and the leader of the Condensed Matter Science Group has been an essential element in the history of the NCNR. The issue of how to replace these three key people within the next decade is of paramount importance to the future of the center. The subpanel is satisfied that the current leadership is fully aware of this issue and is addressing it in a sensible and timely manner.

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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES Fiscal Year 1998 Major Observations of the Subpanel The subpanel presents the following major observations. The subpanel was impressed with the continued high performance of the reactor, cold source, and experimental facilities, which contributes to the excellent scientific research, high staff morale, and strong user satisfaction. The recent award of the Department of Commerce Gold Medal to the Reactor Operations and Engineering Group represents a deserved recognition of this high performance. The subpanel was pleased by the elevation of the reactor organization to the status of a center. This change accords the director of the reactor a level of responsibility commensurate with the center's status as a major national resource. The staff are to be commended for their vigilance in upgrading the reactor facilities. The subpanel encourages continued close attention to this aspect of the operation. Good progress has been made on the three new high-resolution spectrometers in the guide hall, and the beginning of the upgrades for the thermal neutron instruments is also commendable. The subpanel supports the planning that has been started on a new subthermal triple-axis spectrometer and on a versatile biological structure instrument, which would provide support for new competence in biological science. In view of the high oversubscription of the small-angle scattering and reflectivity instruments, it is appropriate to consider alternative review mechanisms while continuing to take the needs of individual users into account. The subpanel was encouraged by the decision to add an in-house theorist and by the effort in place to attract a broad-based scientist with good connections to the condensed-matter theory community nationwide. The subpanel recognized and supports the planning under way to ensure an orderly transition from the current leadership to the next generation.