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Ceramics Division

SUMMARY

The mission of the Ceramics Division is to promote U.S. innovation and industrial competitiveness in the development and use of materials by advancing measurement science, standards, and technology in ways that enhance economic security and improve our quality of life. The Ceramics Division has 22 NIST permanent technical staff, 3 NRC postdoctoral researchers, 4 term employees/students, 31.3 research associates (see footnote 1), and 6 administrative and support staff. Approximately 50 percent of the staff is physicists. The total budget in FY 2009 was $14.5 million, with $271,000 coming from other agencies. The division is organized into four groups: Nanomechanical Properties; Functional Properties; Synchrotron Methods; and Structure Determination Methods.

The chief of the Ceramics Division presented for the division review team a comprehensive overview, including as topics the mission, organization, staffing, budget, facilities, equipment, and core competencies. The overview was followed by presentations from the group leaders and tours of three laboratories.

The format of the review worked well. The presentations were nicely focused, and the laboratory tours provided a good impression of the excellent facilities. The staff discussions helped the panel members understand the work environment.

TECHNICAL MERIT RELATIVE TO STATE OF THE ART

The staff of the Ceramics Division are knowledgeable and recognized as leaders in their respective fields. Their output was 147 refereed journal publications over the past 2 years, not counting open-software and reference materials. There also has been a concerted effort in the division to publish in high-impact journals, which was effectively demonstrated in the breakdown of publications relative to journal impact factor. There were 3 NIST publications or reports, 24 referred conference proceedings, and 13 review articles or book chapters. Several division scientists received important awards, career and early-career awards, and competitive NIST awards. The staff is also well engaged in professional society activities, which demonstrates good technical leadership.

The division’s programs continue to address critical scientific and technical issues in their respective fields, guided by the well-defined mission of NIST to advance measurement science, standards, and technology. There is no organization with a comparable focus in the United States, so a direct comparison with the performance of other government laboratories is not feasible. Nevertheless, judged by the standards of the scientific community, the quality of research performed in this division ranks with the best in the world.



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2 Ceramics Division SUMMARY The mission of the Ceramics Division is to promote U.S. innovation and industrial competitiveness in the development and use of materials by advancing measurement science, standards, and technology in ways that enhance economic security and improve our quality of life. The Ceramics Division has 22 NIST permanent technical staff, 3 NRC postdoctoral researchers, 4 term employees/students, 31.3 research associates (see footnote 1), and 6 administrative and support staff. Approximately 50 percent of the staff is physicists. The total budget in FY 2009 was $14.5 million, with $271,000 coming from other agencies. The division is organized into four groups: Nanomechanical Properties; Functional Properties; Synchrotron Methods; and Structure Determination Methods. The chief of the Ceramics Division presented for the division review team a comprehensive overview, including as topics the mission, organization, staffing, budget, facilities, equipment, and core competencies. The overview was followed by presentations from the group leaders and tours of three laboratories. The format of the review worked well. The presentations were nicely focused, and the laboratory tours provided a good impression of the excellent facilities. The staff discussions helped the panel members understand the work environment. TECHNICAL MERIT RELATIVE TO STATE OF THE ART The staff of the Ceramics Division are knowledgeable and recognized as leaders in their respective fields. Their output was 147 refereed journal publications over the past 2 years, not counting open-software and reference materials. There also has been a concerted effort in the division to publish in high-impact journals, which was effectively demonstrated in the breakdown of publications relative to journal impact factor. There were 3 NIST publications or reports, 24 referred conference proceedings, and 13 review articles or book chapters. Several division scientists received important awards, career and early-career awards, and competitive NIST awards. The staff is also well engaged in professional society activities, which demonstrates good technical leadership. The division’s programs continue to address critical scientific and technical issues in their respective fields, guided by the well-defined mission of NIST to advance measurement science, standards, and technology. There is no organization with a comparable focus in the United States, so a direct comparison with the performance of other government laboratories is not feasible. Nevertheless, judged by the standards of the scientific community, the quality of research performed in this division ranks with the best in the world. 7

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ADEQUACY OF BUDGETS, FACILITIES, AND HUMAN RESOURCES Other than the occurrence of a budget spike in FY 2007, the budgets have been stable over the past 5 years. State-of-the-art facilities for measurement science have long been a feature of the NIST organization. The division’s facilities are top-notch, and all of the laboratories examined are in good shape. In particular, the Nanomechanics Cleanroom Facility in the Advanced Measurement Laboratory represents an outstanding capability. Group leaders and staff are generally satisfied with the breadth and quality of the equipment, which includes equipment that is among the best in the world and some that is unique. There was also heavy infrastructure investment in FY 2009. Highlights include the American Recovery and Reinvestment Act of 2009 (ARRA; Public Law 111-5) funding of an equipment investment of $1.9 million to the Synchrotron Methods Group for the near edge x-ray absorption fine structure (NEXAFS) Microscope Endstation at the National Synchrotron Light Source (NSLS)-I and -II and $1 million for the Nanomechanical Properties Group for the Imaging X-ray Photoelectron Spectroscopy System (for the nanomaterial environmental, health, and safety [EHS], Nano-EHS Program). Since the 2008 review, several excellent new staff hires have occurred to backfill for recent retirements. The division has demonstrated that it can hire new staff expeditiously. Newly hired staff are thriving in this laboratory environment through a combination of mentorship, freedom to pursue their work, and good leadership. Active leadership development is helping to reinvigorate the workforce. In addition, two NRC postdoctoral researchers are expected in the summer of 2010. Bringing in additional NRC postdoctoral researchers is an opportunity for this division, which has the fewest of them in the MSEL. The technical staff of NIST is well known worldwide for their collective expertise in all aspects of measurement science and standards. In addition, the Ceramics Division chief is the designated lead of the NIST Nano-EHS Program and has demonstrated strong institutional leadership on this topic. The division is now shifting emphasis into vitally important areas, such as health and safety, structural and functional nanomaterials, advanced synchrotron technologies, and sustainable and renewable energy materials. As a part of these new technical thrusts, the division is making strategic investments in human resources. As a prestigious institution with a well-recognized track record, NIST is attracting high-caliber new staff. In particular, the impressive early- career staff and postdoctoral researchers are receiving excellent mentoring, they are excited by the projects on which they are working, and they are already formulating a vision of what needs to be done to maintain a leadership position in their research areas. Box 2.1 illustrates how professional leadership has produced an important new research project. ACHIEVEMENT OF OBJECTIVES AND DESIRED IMPACT The Ceramics Division has met its objective of developing and disseminating measurement science, standards, and technology relevant to mechanical properties, functional properties, structure determination, and synchrotron methods for the development and use of advanced materials. Personal interaction and organized 8

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BOX 2.1 Professional Leadership Produces Important New Research Project The Materials Science and Engineering Laboratory encourages the participation of its staff and managers in professional organizations to help disseminate its accomplishments, attract staff and postdoctoral candidates, and promote professional growth, and to help define research projects. The latter is well illustrated by a growing project that resulted from a group leader’s having the honor of being elected to chair a Gordon Conference in 2006. This MSEL staff member chose a topical area that excited participants who were facing a common technical problem of determining “local structure” from x-ray diffraction analyses. The results include the distinction of having an invited article by MSEL authors in Science magazine (an honor), a new project (Local Structure Determination), a workshop hosted by NIST, and 14 publications, the most recent being selected as an Editor’s Choice in Physical Review B. workshops account for good customer engagement. For example, six major workshops have been hosted since October 2008—all of which have contributed to a sharpening of the focus of existing and potentially new programs. The production of SRMs, documentary standards, SRDs, and data analysis software continues to provide an invaluable service to the entire materials community worldwide. TECHNICAL PROGRAM REVIEW Nanomechanical Properties Group The Nanomechanical Properties Group consists of 5 NIST permanent technical staff, 2 NRC postdoctoral associates, 3 term employees or students, 18.1 NIST associates (see footnote 1), and 1 administrative staff member. The stated objectives of the group are to develop mechanical measurement science, standards, and technology needed by U.S. industry to apply materials and components in nanomechanical applications. This group continues to perform high-quality research in scanning probe microscopy, nanoparticle metrology, and nanoscale stress and strength measurements. Its budget in FY 2009 was $4.3 million. This group is mature, understands the unique mission of the laboratory, and has acted accordingly. Looking beyond that, it has recognized the importance of having control of the materials that it is measuring. In a few cases, notably theta-section fabrication and laser ablation of films, the group has already taken a step in this direction. Improvements in scanning probe microscopy measurement techniques are needed by the broad materials community, and researchers in this group are providing leadership on this topic. The achievements to date are impressive. In particular, the progress in the development of an electromechanical coupling measurement method for extremely thin films and elastic modulus measurements of nanowires and nanotubes are noteworthy. The nanoparticle metrology project team has assembled excellent capabilities to investigate laser light scattering, optical spectroscopy, and field-flow fractionation. Advances in confocal Raman microscopy, strain measurement by electron diffraction, 9

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and related areas are significant and continue to make an impact in the scientific literature. Nanoscale stress and strength measurements show significant progress on all fronts. A highlight of this research is the optimization of a photolithographically formed “theta” device for micro-tensile strength measurements. The device is robust, reliable, and versatile. Nanoindentation-based elastic, plastic, viscous, and fracture measurements continue to be a productive area of research, with numerous publications to the group’s credit in archival journals. The Nanomechanics Cleanroom Facility is impressive. It surely will provide unmatched capabilities for conducting atomic force microscopy, scanning tunneling microscopy, and nanoindentation measurements without being compromised by concerns with respect to sample contamination. This facility will likely assume even greater importance as device technology advances progressively into the nanoscale domain. Working closely with nanodevice manufacturers should be a rewarding activity. Opportunity areas for further research include the design, fabrication, and testing of nanoscale sensors and electromechanical devices to monitor and assess the reliability of large-scale engineered structures. Another opportunity area is that of self-healing nanostructured coatings to replace chromate-based protective coatings for diverse applications. The panel’s findings and recommendations with respect to the Ceramics Division’s Nanomechanical Properties Group are as follows: Finding: The electromechanical measurement method for thin films has potential for broader use. Recommendation: As a new initiative, this technology should be applied to nanocrystalline (one phase) and nanocomposite (two or more phases) ceramics where there is a need to determine changes in hardness, stiffness, and wear properties across nanograin and nanophase boundaries. In addition, precise measurements on high-density ceramics to determine unequivocally the dependence of hardness on grain size extending from micro- to nanoscale dimensions would be beneficial. Finding: The theta test device is a powerful tool for exploring mechanical properties of materials. Recommendation: The “gapped-theta” design for determining the strength and stiffness of micro- and nanofibers of materials should be evaluated. Beyond that, there are opportunities to modify the device further to perform microscale and nanoscale measurements of (1) temperature dependence of tensile strength and fracture behavior, (2) low- and high-cycle fatigue properties, and (3) susceptibility to stress-corrosion cracking. The ability to carry out these tests on carbon fibers would also be invaluable, now that carbon-fiber-reinforced composites are being used in commercial and military aircraft. 10

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Finding: Knowing the details of a material synthesis process is often essential to understanding its properties, but existing capabilities are limited. Recommendation: The “nanofabrication” capabilities should be upgraded to provide high-quality materials for property and performance measurements, as well as for in-depth materials characterization. Finding: The nanoindentation work merits expansion. Recommendation: The nanoindentation effort should be expanded to include nanowear, nanoscratch, and nanoimpact tests. For example, scratching experiments performed at ramped loads could enable the measurement of the critical load at which failure occurs in bulk materials, or at which decohesion occurs for coatings. High-cycle fatigue tests could be performed by oscillating the sample, causing the diamond probe to impact the surface repetitively at high frequency until failure occurred. These are significant challenges, but well within the capabilities of the Nanomechanical Properties Group’s personnel. Functional Properties Group The Functional Properties Group consists of four NIST permanent technical staff, one NRC postdoctoral researcher, and 4.2 NIST associates (see footnote 1). The stated mission of the Functional Properties Group is to (1) develop and disseminate measurement science, standards, and technology pertaining to functional properties of advanced materials and devices; and (2) determine and disseminate key data needed to establish the relationships between structure, properties, and performance of functional materials for advanced applications in energy, sustainability, and microelectronics. The stated mission is broad, but the group is focused on four technical areas: (1) energy conversion materials, (2) carbon mitigation, (3) nanocalorimetry, and (4) combinatorial measurement methods. This group is relatively new and, from the perspective of its $2.6 million budget, is the smallest of the four groups in the Ceramics Division. This group is in the process of getting fully established, which is consistent with the number of early-career group members. The group has some excellent external collaboration with industry and academia, including good international collaborations with top institutions (e.g., the Interuniversity Microelectronics Center [IMEC] in Belgium and the National Institute for Materials Science [NIMS] in Japan). In the area of energy conversion materials, this group has and is developing a comprehensive suite of characterization capabilities for thermoelectric materials. The intent is to develop standard reference materials and determine the best measurement techniques and protocols for characterizing thermoelectric performance. Standard test methods and unique test systems developed by NIST are being effectively used to address the stated goals of the group, which has also developed a range of good partners (industrial and academic) on this topic. NIST has also established a combinatorial materials effort focused on characterization methods, which has been effectively applied to determining work function in gate electrode systems. Interactions with Micron Corporation, SEMATECH, IMEC, and NIMS on this topic are noteworthy. The group is 11

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now appropriately looking for ways to take further advantage of this combinatorial materials effort by applying it to thermoelectric materials in combination with their other technique development on thermoelectrics. In terms of establishing new, leading-edge capabilities, the effort to develop a chip-based nanocalorimetry capability seems quite novel. This relatively new work has some good, early accomplishments and, if successful, should provide a new capability that can be applied broadly. Noteworthy here is that Micron Corporation is supporting a student intern at NIST to increase its engagement with this effort. Also valuable are additional collaborations on this topic with the NIST Nanofab facility in the NIST Center for Nanoscale Science and Technology, with the University of Illinois at Urbana- Champaign, and with the Johns Hopkins University. A new effort on measurement needs related to carbon mitigation has been initiated. Measurement challenges have been identified, but it is too early to evaluate the focus or progress of this project. Two noteworthy accomplishments were achieved by the group this year. The first was the development and certification of a Bi2Te3 Seebeck coefficient SRM for the calibration of measurement apparatus. In addition, a NIST Bronze Medal was awarded to one of the staff for exceptional programmatic leadership over an extended period. The panel’s finding and recommendation with respect to the Functional Properties Group are as follows: Finding: There is substantial room for the Functional Properties Group to expand technically, especially in the area of energy conversion materials, where batteries and capacitors were identified as an appropriate growth area. Recommendation: The Functional Properties Group should continue to hold workshops, such as the upcoming workshop on carbon mitigation planned for 2011, to determine how NIST can best contribute to broad and fast-moving fields from the perspective of measurement science and technology. Synchrotron Methods Group The Synchrotron Methods Group consists of three NIST permanent technical staff members and four associates. The mission of the Synchrotron Methods Group is measurement science and technology that pertains to chemical and electronic structure of advanced materials and devices by synchrotron methods. The group is meeting its objectives by developing state-of-the-art methods and making them available to NIST users and other collaborators. The suite of spectroscopy beam lines at the National Synchrotron Light Source impressively spans the entire Periodic Table and served 110 users with 90 experiments over the past year. Funding for the Synchrotron Methods Group has increased appropriately, from $2.5 million to $3.0 million over the past 2 years. Capability upgrades have been realized through ARRA and Small Business Innovative Research (SBIR) III funding. The group is also appropriately focused on working with the Brookhaven National Laboratory on the NSLS-II project, which is a billion-dollar facility that will have x-ray beams with improved coherence and tunability and increased brightness (by 10,000 times) in comparison with the current NSLS facility. The NIST group at 12

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Brookhaven appears to be an important stakeholder in the planning of this new national facility, which is expected to start construction in 2010, with start of operations in 2015. The x-ray absorption fine structure spectroscopy (XAFS) at beam line X23A2 demonstrated a major accomplishment of revealing ferroelectric functionality of SrTiO3 thin films on Si by means of piezo-force microscopy.5 A cryostat sample holder will be added to this capability next year. In addition, the group works well with the Polymers Division, which led to determining the molecular structure-function relationship of a mixture of polymer-fullerenes using NEXAFS beam line U7A at NSLS. The hard x-ray photoelectron spectroscopy (HAXPES) beam line X24A has been an important part of a SEMATECH collaboration on semiconductor gate stacks. The x-ray photoelectron spectroscopy (XPS) three-dimensional chemical microscope, which is under development at beam line U4A at NSLS, appears to be an excellent capability that ranks among the best in the world. In addition, excellent work continues with the Ultra-Small Angle X-ray Scattering (USAXS) facility at the Advanced Photon Source, Argonne National Laboratory. One good example was the certification of gold nanoparticle size for NIST reference materials: 8011, 8012, and 8013. The Synchrotron Methods Group has many good outreach activities to meet customer needs, including partnerships, Cooperative Research and Development Agreements (CRADAs), board service, Memorandums of Understanding (MOUs), industry coalitions, and international workshops. The group leader of the Synchrotron Methods Group was recognized with a Bronze Medal (a NIST award) for significantly advancing NEXAFS spectroscopy methods to quantify the interfacial molecular orientation of organic semiconductor materials that are being developed for flexible low- cost electronics. The group is at the state of the art in the development and application of synchrotron methods, has established a very mature capability that continues to produce significant accomplishments, and has clearly met its stated mission objectives. The panel’s findings and recommendations with respect to the Synchrotron Methods Group are as follows: Finding: The group is at the state-of-the-art level in the development and application of synchrotron methods. The group has established a very mature capability that clearly meets stated mission objectives through significant accomplishments. Recommendation: The upcoming transition to the National Synchrotron Light Source-II project should be used to build and upgrade facilities and equipment. Finding: No patents were awarded during the past 2 years. Recommendation: Appropriate developments should be patented. 5 M.P. Warusawithana, C. Cen, C.R. Sleasman, J. Woicik, Y. Li, J. Kluga, L.F. Kourkoutis, H. Li, L.P. Wang, M. Bedzyk, D.A. Muller, L.Q. Chen, J. Levy, D.G. Schlom, “A Ferroelectric Oxide Directly on Silicon,” Science 324:367, 2009. 13

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Structure Determination Methods Group The Structure Determination Methods Group consists of nine permanent technical staff members, one term employee/student, nine associates, and one administrative staff member, with a budget of $4.2 million. The stated mission of the group is to develop and disseminate measurement science, standards, and technology for the determination of the structure of advanced materials by improving: x-ray, electron, and neutron diffraction; and computational tools and providing SRMs and SRDs. The x-ray metrology and USAXS facilities have demonstrated outstanding performance. In particular, their newly commissioned divergent beam diffractometer achieves ±20 femtometers precision in lattice parameter measurements. This group is the premier source for crystallographic data for non-organic compounds; its SRDs are packaged with instruments marketed by several major vendors, and its SRMs comprise 4 to 5 percent of NIST’s total sales volume. The group highlighted three projects: X-ray Metrology and Standards, Measurement and Prediction of Local Structure, and Crystallographic and Phase Equilibrium Data. The X-ray Metrology and Standards project develops SRMs and quantitative, reproducible measurement methods and protocols for powder diffraction, high-resolution diffraction, and x-ray reflectometry to enable the accurate and precise determination of material structure at the x-ray wavelength scale. Among other notable accomplishments, this project has achieved order-of-magnitude improvements in accuracy and precision in lattice parameter determination with its new divergent beam diffractometer. The Measurement and Prediction of Local Structure project develops theoretical predictions and data-analysis methods for the quantitative determination of local atomic structure, based on inputs from multiple experimental techniques and first-principle calculations. The project lists several recent publications on a variety of materials systems, including the determination of the local structure origin of dielectric properties in AgNbO3-based ceramics, which received an Editor’s Choice award. The Crystallographic and Phase Equilibrium Data project provides critically evaluated, comprehensive crystal-structure SRDs in formats that are readily incorporated into x-ray, neutron, and electron diffraction instrumentation. Its Inorganic Crystal Structure Database has been expanded to include calculated (non-experimental) atomic coordinate information, in addition to experimentally derived information. This project has achieved excellent results in determining, compiling, evaluating, and disseminating phase-equilibrium data, which are now published electronically and cover the literature. This group is meeting the needs of its customer base, particularly in the production of SRDs and SRMs, which are in heavy demand. The development of software capable of combining multiple types of experimental data for the determination of local structure will be a valuable tool, particularly for the nanomaterials community. With respect to the Structure Determination Methods Group, the panel makes the following recommendation: Recommendation: The Structure Determination Methods Group should continue to look for new, high-impact structure determination work and novel methods for the dissemination of information to build on its excellent current performance. 14

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OVERALL FINDINGS AND RECOMMENDATION Finding: There has been a strong leadership commitment to bringing in new staff to reinvigorate the Ceramics Division. Finding: The Ceramics Division has a small amount of external funding relative to other divisions in MSEL. Finding: The name “Ceramics” Division may no longer be appropriate as a description of the primary work being done by this division. Recommendation: Opportunities for bringing in additional funding should be explored. Other-agency funding can be used to expand staffing and capabilities and helps to sharpen people’s focus, as developing external funding is a very competitive process. 15