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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 7 Materials Science and Engineering Laboratory INTRODUCTION The mission of the Materials Science and Engineering Laboratory (MSEL) is to work with industry, standards bodies, universities, and other government laboratories to improve the nation’s measurements and standards infrastructure for materials. The laboratory is organized in four divisions, as shown in Appendix A: Ceramics Division, Materials Reliability Division, Polymers Division, and Metallurgy Division. The MSEL also includes the NIST Center for Neutron Research (NCNR). Because of the special reporting needs of the center, the findings on NCNR are presented separately in this chapter. Nevertheless, the Board interacted with the NCNR review team during this assessment cycle and found the cross-fertilization of findings to be valuable to all. Appendix A also presents the staffing trends for the laboratory (see Figure A.7). MAJOR OBSERVATIONS The Board presents the following major observations with respect to the Materials Science and Engineering Laboratory: The MSEL has impressive programs of very high quality and technical merit as well being both relevant and effective. There are emerging programs that have high potential for future benefit.
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 The MSEL staff have shown their excellence through receipt of external awards and recognition, including an impressive number of staff with membership in the National Academies. The MSEL fulfills its NIST mission well, and effectively disseminates information through the production of Standard Reference Materials (SRMs), Recommended Practice Guides, and databases. The laboratory uses the World Wide Web well in making information available to its customers. The publication record of the laboratory is exemplary. Three of its researchers are listed by Thomson-ISI as being among the most highly cited researchers in the world in materials science. The laboratory is recognized by industry for its contributions to technology, technology transfer, standards, and metrology. The new Advanced Measurement Laboratory (AML) has the potential to benefit MSEL through the use of significant new equipment such as high-resolution X-ray diffractometry. The NCNR facility is of enormous value to the laboratory, to NIST researchers, and to the worldwide user community. It continues to operate with a level of technical excellence that reflects very positively on the laboratory and NIST. TECHNICAL QUALITY AND MERIT The technical quality and merit of MSEL continue to be very high relative to the state of the art for most programs. The overall quality of the research is laudably high. To illustrate this point further, some examples of excellent research are cited below. This list is by no means all-inclusive, providing only illustrative examples. Following that is a discussion of some of the challenges and opportunities that the laboratory faces. Examples of programs with outstanding technical quality and merit include the following: The program on Synchrotron Materials Science in the Ceramics Division has particular technical merit. This program includes mapping surface chemistry and molecular orientation with combinatorial Near-Edge X-ray Absorption Fine Structure spectroscopy and chemistry and structure of nanomaterials. The tools at the user facilities at both the Advanced Photon Source at Argonne National Laboratory and the National Synchrotron Light Source at the Brookhaven National Laboratory offer one-of-a-kind, NIST-like measurements. One researcher in this program was presented with the Department of Commerce Gold Medal for his pioneering development of a first-in-the-world national facility for soft X-ray absorption spectroscopy. There is special merit to the classical metallurgy and reliability work done in support of the World Trade Center (WTC) investigation. The work was performed collaboratively between the Metallurgy and the Materials Reliability Divisions. NIST became the lead agency in the investigation of the WTC Twin Towers collapse. Over the 2 years of this review, the NIST team has, in an effective and timely way, generated the structural data, particularly on the steel structure, needed for modeling the collapse. In particular, the team evaluated the properties of the many (more than 29) structural steels involved, at high temperatures and at high stress rates. To do so they needed to create new measurement techniques, especially concerning the yield strengths at high temperatures. The measured parameters allow meaningful modeling of the collapse of these buildings. The measurement techniques developed for the parameter determination are a permanent legacy of this project. Standardized test methods are being developed to quantitatively evaluate and compare the resistance of structural steels to high-temperature deformation and failure. This project is a demonstration of the core competencies that exist and that must be preserved in order for NIST to respond properly to this kind of failure analysis in the future.
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 Within the Polymers Division, the programs involved with organic electronic materials are particularly impressive. These programs include Characterization of Porous Low-k Dielectric Constant Thin Films, Polymer Photoresists for Next-Generation Nanolithography, Organic Electronics, and Nanoimprint Lithography. Initiatives in next-generation lithography are aggressively addressing several critical issues as the surfaces and interfaces begin to dominate in nanoelectronic devices (sub-100 nm design rules). The progress in developing fundamental parameters for dissolution behavior and line-edge roughness of the image is impressive. The nanoimprint technology is but one of many contenders for future lithography, but the work is cutting edge and clearly has relevance to issues in 30 nm design rules. The vision of nanoimprint lithography as an enabler to carry out leading-edge measurement science in a variety of areas is appropriate. The program on Quantitative Nanomechanical Properties in the Materials Reliability Division is particularly worthy of praise. This program focuses on atomic force microscopy (AFM)-based metrology for the rapid, nondestructive measurement of mechanical properties with true nanoscale spatial resolution. It employs atomic force acoustic microscopy (AFAM) involving the vibrational resonance of an atomic force microscope cantilever when its tip is in contact with a sample. The work has matured to the point of making innovative strides in improving the data collection rates and understanding issues such as tip wear to improve the validity of data. The project on Mechanical Metrology for Small-Scale Structures in the Ceramics Division is impressive. This project seeks to measure the mechanical properties of industrial and biological micro-structures that cannot be fabricated as bulk samples. The multifaceted project includes a combination of finite-element analysis (characterization and optimization of test configurations), specimen fabrication, and experiment (nanomechanical testing, fractography, and length/force metrology). This work represents an elegant measurement solution to important practical problems. It fits well into the NIST metrology vision. It provides a path to standards for small-scale mechanical measurements; opportunities to use this technique abound, including biomedical opportunities. Within the Metallurgy Division, the collective work in a number of magnetic programs is exemplary. These programs include High Coercivity FePt Alloys for Future Perpendicular Magnetic Data Storage, Electrodeposited Pt1–x (Fe,Co,Ni)x Alloys, and Novel Magnetic Materials for Sensors and Ultra-High Density Data Storage. These programs pave the way for measurement metrics in the future magnetic-storage industry. Very importantly, resources have been concentrated on the development of ultrasoft magnetic thin films for very high sensitivity spin valves. Though the primary application for such high-sensitivity sensors is not obvious, it is exceedingly likely that a number of applications will be generated in a number of fields, including memory and medical applications, if such a sensor is available. This is a high-risk project with considerable payoff potential. In related work on magnetic materials, the work on ballistic magnetoresistance is commendable. The group carrying out this work has proven unambiguously that the huge magnetoresistance values reported for very small contacts were purely artifactual, resulting from mechanical alterations at the contact due to magnetostriction or particle accumulation in the presence of a field. This negative result has saved a number of companies in the hard-disk business seeking a high-sensitivity detector from pursuing a false lead. The work in biomaterials within the Polymers and the Materials Reliability Divisions is praise-worthy. The work in dental applications is moving from its history in dental materials to metrology at the interface between cells and scaffolds, working on standardized scaffolds and references with the American Society for Testing and Materials (ASTM). The biomaterials groups have established robust efforts in metrology at the interface between materials science and cell biology, both in the definition of relevant quantitative parameters and in the development of appropriate methodologies. Excellent
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 progress has been made in the development of a reference scaffold, with a particular emphasis on the definition and quantification of porosity in tissue scaffolds. The Metrology for Nanoscale Properties: Brillouin Light Scattering program within the Materials Reliability Division has exceptional technical excellence. After many years of work on the instrumentation, this program is now ready for data collection. The Brillouin capability is unique, since all other groups in this field are focused on magnetics rather than on elastic properties, and the team is collecting very useful hardware validation of models of elasticity as a function of size. By using Brillouin scattering as the “gold” reference, the AFAM work becomes a practical secondary technique for mapping elastic properties across a nanoscale surface. Challenges and opportunities with respect to technical quality and merit at MSEL include the following: For the very impressive Ceramics Division program on Mechanical Metrology for Small-Scale Structures, MSEL should find collaborators from universities that can help sustain this work. The work on metals and reliability for the WTC investigation is coming to a close. The skills and expertise required for that effort have continuing value, and the researchers can apply these to other projects such as pipeline failure. The Materials Reliability Division has a history of providing leadership in the areas of welding and Sharpe Impact testing, and it has many satisfied customers. However, this expertise has been on the wane; while the existing talent was crucial to the WTC investigation and work on standards for fire-resistant steels, the expertise seems to be constantly under threat of extinction. In fact, the Infrastructure program has received new funding from the Department of Transportation to look at measurements and standards for high-strength pipeline steels. While this is an effective use of the Materials Reliability Division talents, the overall program would benefit from increased focus, direction, and proactive efforts on funding. The scientists involved with the reliability efforts on microelectronics have done very good work. They have developed a microtensile testing facility, but it is useful primarily for calibration. This team is searching for its identity. It is doing very clever work in nanoscale reliability stress/response methodology, but it needs to connect that work to a future vision of usable metrology. It appears that the group is not well connected to its customers, and the impact of this program remains to be seen. In the magnetic materials research, magnetic nanoparticles are now broadly made and have been shown to have very different properties. It is not certain whether these differing properties are due to material differences or to measurement methods. There is need for Standard Reference Materials in this new field. RELEVANCE AND EFFECTIVENESS The MSEL scores high for choosing programs that are both relevant and effective. The programs are relevant in supporting the mission of the laboratory and of NIST. The work is effective in that the laboratory is diligent in disseminating the results of its work through many venues. The MSEL is largely very customer-focused and makes effective use of workshops and customer consortia. Illustrative examples are presented below, followed by examples of new programs that have potential for relevance and effectiveness. Finally, some comments are offered in the nature of challenges and opportunities that the laboratory faces in this arena. Table 7.1 illustrates some of the statistical information on the output of MSEL as it pertains to relevance and effectiveness.
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 TABLE 7.1 Materials Science and Engineering Laboratory (MSEL): Fiscal Year 2004 Output Performance Data Performance Criterion Total, Measurement and Standards Laboratories (MSLs) Total MSELa Total MSEL as Percentage of Total, MSLs Total expenditures $444.7 million $47.7 million 11 Publications 1,612 502 30 Invited talks 376 SRMs sold, total (units) 25,820 2,928 11 SRMs sold, total ($ thousand) 7,315 1,056 14 Patents pending 39 4 10 Patents issued 11 0 0 CRADAs active during FY 2004 52 5 10 Total CRADAs signed, FY 1988-2004 1,017 243 24 CRADAs (new) 16 0 0 Standards committee memberships 1,197 123 10 Standards committees chaired 138 10 7 Staff participation in standards committees 369 29 8 Guest researchers, in United States 933 207 22 Guest researchers, total 1,533 389 25 aMaterials Science and Engineering Laboratory (excluding NIST Center for Neutron Research reactor operations). NOTE: SRM, Standard Reference Material; CRADA, cooperative research and development agreement. Examples of high relevance and effectiveness include the following: The program on Synchrotron Materials Science in the Ceramics Division used Small Business Innovative Research (SBIR) funding to connect with industry by using these funds to build instruments for novel applications. This approach is effective; the Synchrotron team could teach techniques for leveraging SBIR funding to other NIST staff. The Sheet Metal Forming Project is MSEL’s “poster child” in the customer-service domain. Its output is highly prized by the automotive industry in particular. The forming group has been focusing on developing standard tests and data for characterizing advanced sheet material formability for the automotive community. Its most recent achievements are the introduction of a springback cup test (or the Demeri Cup Test) to the ASTM at its national meeting to explore the standardization of this test, and improvements in the new X-ray stress measuring system for the direct in situ characterization of the stress in a given direction while the sheet is under multiaxial stretching. The group has made significant progress in mapping the multiaxial stress-strain behaviors for three aluminum sheet alloys. This system enables the accurate measurement of the effect of strain paths on the evolution of the yield surface. Within the Polymers Division, the NIST Combinatorial Methods Center (NCMC) continues to serve as an excellent example of work with both relevance and effectiveness. This program develops combinatorial and high-throughput synthetic and measurement methodologies for the materials sciences. Key to (and a result of) its success has been the ability of the center to attract a significant industrial customer base. The center provides an important national strategic service in giving access to U.S. companies that might otherwise be unable or unwilling to make the investment needed to gain
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 access to combinatorial and high-throughput screening methodologies. The involvement of Food and Drug Administration (FDA) researchers in the center suggests that NCMC is also providing valuable intragovernmental service. Throughout the past 2 years, the center has continued to grow and build new devices to measure properties. The future impact of this program could be compared with that of the Phase Diagram Program, with NIST at the forefront. The program is enabling small companies with tools, methods, and a cooperative public domain approach that moves the field forward. The program encompasses the NIST missions of metrology and technology transfer. The Biomaterials Metrology Program in the Materials Reliability Division has been successful in its mechanical measurements. This program is commendable on many levels. It has demonstrated high-quality technical work and is an excellent example of applying NIST expertise to an important area of research that was outside a traditional area of expertise for the group. Also, the program is very well connected to the local health research community and is a best-practice example of bringing in external advisers and using external review boards to keep programs on target and to open up new conduits for technology transfer. Examples of emerging MSEL programs with potential for high relevance and effectiveness include the following: The emerging thrusts in nanocalorimetry are seen as promising, with an increasing need for calorimetric measurements on very small samples. It is anticipated that the work will lead to impressive precision for measurements on such small samples that it will be relevant to U.S. industrial needs. The efforts on providing cantilever standards for AFM are applauded. If successful, this work will impact many U.S. technological programs and is perfectly in keeping with the NIST mission. Researchers previously working on lead-free materials and superconformal metal deposition are beginning to work on using these materials and processes at smaller dimensions for future interconnection technology. The Board will await the outcome from this shift of emphasis but does not offer judgment at this time. Challenges and opportunities with respect to the relevance and effectiveness of MSEL programs include the following: The NIST Combinatorial Methods Center could be of even more usefulness to its customers if its resources and staff were further expanded. The NCMC can serve as a good model as MSEL expands other programs to add more direct value to the nation’s industrial base. The MSEL demonstrated interesting efforts in the development of gradient libraries in an effort to delineate the relationship between materials parameters and cellular responses. The Board strongly supports the thrust of the Polymers Division into the biomaterials area, but it remains concerned by the lack of vision and progress in identifying and developing relationships with a customer base. One could argue that, unlike the electronics and NCMC efforts, the industrial customer base for the output of the biological efforts is less well defined at this point. The potential industrial customers may be younger companies and the critical metrology problems less well defined, but these factors make an outreach effort all the more critical. The Board encourages the organization of workshops and conferences to reach out to the industrial base and to build collaborative programs so that MSEL can lead rather than follow the development of metrology. The work on nanotribology has resulted in good tools, but it is not clear to the Board what the
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 purpose or vision is. The investigators would benefit from a broad understanding of the project motivations. The Board finds it difficult to gauge the relevance of this work. The growth of semiconductor nanowires embodied some very elegant materials science with respect to gold seed particles and epitaxial ZnO growth. It is not apparent, however, that the resulting structures allow any electronic or electro-optic devices that cannot be synthesized at least as well by existing planar photolithographic techniques. The conformed electrodeposition program has historically made significant contributions to the semiconductor industry. The present interconnect project represents a positive addition to that accomplishment, but it is worth considering whether or not the superconformal project has its most valuable contributions behind it. The deposition of the ruthenium seed layer for both a barrier and a conductive layer is a significant increment, but this is a project whose future should be carefully considered before further effort is committed. With the generation of new materials and a proper analysis of magnetic hysteresis properties, magnetic refrigeration has been extended from the sub 1 degree K range to the tens of degrees (K) range. A space-viable magnetic refrigerator is being constructed by the National Aeronautics and Space Administration, but it is hard to see how magnetic refrigeration, with its limited caloric pumping capability, will replace conventional thermoelectric cooling devices in the foreseeable future. Spin-density waves have been established to exist in the ferromagnetic alloy Fe3Al. Spin-density waves have previously been found only in antiferromagnets. This is an elegant piece of physics, but its relation to NIST’s mission is not clear. The work in the laboratory on mass spectrometry of polymers (matrix-assisted laser desorption-ionization mass spectrometry [MALDI-MS]) has been very relevant. It is now time to consider whether the “low-hanging fruit has been picked.” The laboratory may wish to consider whether the most effective use of resources is to continue these programs at their current levels. The premise of the work in organic electronics is valid: there is great deal of interest in this growing and technologically important field, and U.S. competitiveness is critical. There is wide variation in properties of materials prepared in different laboratories, and NIST can play an important role here in defining and developing characterization methodology and metrology, giving an edge to U.S. efforts in this field. The initial testing of materials from different leading research and development molecular electronics laboratories and their correlation to device behavior will serve as a good vehicle of technology transfer for the developed metrology. The vision for the program needs to be better defined. The collaboration with Intel provides an important avenue for MSEL technology to impact a critical industry, but it was not clear to the Board what resources (intellectual, infrastructure, financial) Intel was bringing to the table other than relevance. The mission and management structure of the Materials Reliability Division at the Boulder campus are very unclear. This lack of clarity is affecting both morale and progress by the excellent scientists in that location. Further delay in reorganizing or naming leaders will be counterproductive. RESOURCES For many review cycles, the Board has advised that years of flat or declining budgets for the Materials Science and Engineering Laboratory are eroding its ability to continue the high-quality and needed work in many existing programs and potential new programs. Despite this concern, the laboratory experienced severe cuts in FY 2004, necessitating a reduction-in-force (RIF) plan. This plan was suspended pending expected increases for FY 2005. These increases were realized at least in part, and the RIF was avoided.
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 Nevertheless, the budget trend over a decade, whether monotonic or sawtooth, shows clearly that the laboratory had no choice but to reduce its permanent staff to compensate for budget shortfalls and inflation of staff salaries and equipment costs. An understandable response by the laboratory has been to rely more heavily on temporary staff. An increasing reliance on temporary staff erodes the core competencies of the laboratory. The Board continues to advise that this laboratory is underresourced considering its need and competency, but is concerned that this advice will fall on deaf ears. During the 2005 review, there were fewer comments than there had been in the past from researchers on the inability to purchase needed sophisticated equipment. This may be a shock response to the aborted RIF program (researchers may be pleased merely to have their jobs). It may also reflect the equipment now available in the Advanced Measurement Laboratory. NIST CENTER FOR NEUTRON RESEARCH Major Observations The NIST Center for Neutron Research has a mission to ensure the availability of neutron measurement capabilities in order to meet the needs of U.S. researchers from industry, universities, and other government agencies. The center is executing this mission well. As an overview, the Board finds the following: The internal science program covers an impressive range with excellent depth. Good topics are pursued with highly visible results, and many problems addressed have technological interest. Nonetheless, there must be steady critical review of the technical relevance and scientific novelty of the internal work. It makes no sense not to install the already-constructed 10 m small-angle neutron scattering (SANS) instrument and make it available to users through the National Science Foundation (NSF)-supported Center for High Resolution Neutron Scattering in order to relieve the large user pressure for SANS beam time. The integration of theory into NCNR programs is improved and should continue. The NCNR should vigorously explore collaborations with universities, government agencies, and other NIST units in order to further involve theorists. The reactor license renewal application was submitted to the Nuclear Regulatory Commission in a commendable way. There should be enhanced support for neutron reflectometry with a careful selection of appropriate problems and consideration of complementary X-ray techniques. There is excellent synergy between NCNR and the Spallation Neutron Source (SNS) (at the Oak Ridge National Laboratory) in instrument and program development. This exemplary cooperation might well be extended to the international arena. Technical Quality and Merit The number of users accommodated by NCNR and the strength of its internal research program are at outstanding levels. Quantitative measures, while only approximate, show that NCNR services users in an economical way when compared with similar national and international centers with the same mission. Excellent technical quality is evidenced by the staff’s many publications in high-quality journals, with many of those publications in journals that have exceptionally high impact factors. NCNR
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 staff members have been recognized by numerous awards both from the Department of Commerce and from external organizations. Facility users have also been honored for scientific advances enabled by the use of NCNR instruments. The organization is competitive in its efforts to bring excellent young researchers to NCNR. The NCNR leadership is well integrated into the U.S. neutron scattering organizations, and staff members are recognized as leaders in their technical areas of neutron science. There is a particularly free exchange of information about the development of the Spallation Neutron Source at the Oak Ridge National Laboratory, and there is a clear understanding of the future synergy between the two facilities when SNS comes online. The NCNR has in place an extensive planning process for new instruments that balances user needs with investments in new instruments and techniques. The reactor and its associated safety and security systems have in place a portfolio of timely actions designed to ensure continued levels of high availability through the entire 20-year period of relicensure. Relevance and Effectiveness The NCNR provides the principal source for neutron scattering experiments in the United States. As such, it is readily available and is of exceptional value to its users. Users include universities, corporations, and other governmental entities. The scope of research projects at NCNR ranges from basic sciences, to applied sciences and engineering applications, and to propriety research in support of new commercial applications. In addition to disseminating results through technical publications, the staff actively participate in summer schools, both at NCNR and elsewhere, to teach neutron scattering techniques to scientists in other fields. New Web-based applications to help experimentalists with experimental planning, data analysis, and fitting are being used effectively. Resources The facilities, equipment, and human resources of NCNR currently are adequate for the volume of high-quality work being carried out internally, but they are not sufficient to meet the higher volume of projects proposed by users. Thus, NCNR is staffed at or below the minimum level needed to meet its objectives. The requests for user access dramatically exceed availability, so that in some cases as few as 47 percent of the proposals can be approved, and, over the same period, the number of days approved is only 30 percent of the total number of days requested. Moreover, the lack of an adequate number of staff members limits facility development, and it also limits the professional and career development of the staffers themselves. The staff display remarkable morale and esprit de corps, but they clearly are taxed to provide the service needed. Additional permanent staffing is required to maintain and enhance the user program; any losses would harm the program. Provisions for reactor maintenance and operation in the future have been made in a timely way. The NCNR has an exemplary safety record, and the staff understand and support the need for safe operations. Nonetheless, care must be taken to maintain continuous training and improvement and to avoid complacency. Configuration management control needs to be improved, and systems need to be developed for instruments, support facilities, and documents; these needs will probably require a dedicated champion on the staff. Coordination and new joint programs with other reactor-fuel users should be explored to enhance and ensure a stable supply of fuel for the long term. The available equipment and facilities at NCNR are adequate at present, but additional instruments are needed to meet user demand now. Further instrument development should be done in concert with
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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 other facilities. It is significant that NCNR has managed to decommission instruments (i.e., NG-1 and the 8 m SANS) while bringing impressive new instruments online. The staff has an impressive range of ideas for instruments and sample environments that should be developed. With respect to new instrumentation, the installation of the already-constructed 10 m SANS instrument is a high priority. Its inclusion in the Center for High Resolution Neutron Scattering will substantially relieve the large user pressure for SANS beam time. Further, there should be additional support for neutron reflectometry, which also has a substantial user base. Overarching theoretical work as well as analysis tools should be developed in parallel with instruments and with sample environments. Space issues may also become a concern, especially as the total number of instruments grows and replacement instruments increase in size and complexity.
Representative terms from entire chapter: