An Assessment of the National Institute of Standards and Technology Materials Science and Engineering Laboratory: Fiscal Year 2008 (2008)

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Ceramics Division SUMMARY The Ceramics Division has programs that are well defined and focused on its mission; it has developed several state-of-the-art facilities, some of which are unique; it has a fine, productive staff; and it has an enthusiastic and effective leadership team that vigorously evaluates the technical performance of the staff. The MSEL-wide project evaluation process, while burdensome in its early implementation, has been effectively employed by the Ceramics Division to redefine its project portfolio. The division’s aggregated research capabilities support materials characterization, particularly in x-ray metrology and synchrotron-based methods, and those located in the state-of-the-art Advanced Measurements Laboratory (AML) that are among the best. Proactive performance evaluation has addressed personnel issues to enhance the capability of the Ceramics Division. The staff is very productive, as measured by publications in refereed journals and the delivery of many standard reference materials and phase-equilibrium diagrams. The programs integrate theory and modeling with experimental studies, where feasible, to create a balanced portfolio. The funds appropriated under the America COMPETES Act of 2007 have been effectively used to enhance the capability of the three NIST beam lines in the National Synchrotron Light Source, a U.S. Department of Energy (DOE) national user facility, at the Brookhaven National Laboratory in New York. Noteworthy accomplishments include fielding the most advanced synchrotron detectors and performing, for the first time, interfacial structure measurements on commercially important high-dielectric-constant gate oxides. Several industrial partners are involved in the research. The division has made good use of the exceptional capabilities in the AML, where it has 11 modules comprising two laboratories focused on nanomechanics (using atomic force microscopy [AFM], scanning tunneling microscopy [STM], and nanoindentation) and x-ray metrology, using a custom-built parallel beam diffractometer. Both require exceptional stability of the measurement environment. Other noteworthy accomplishments include the first combinatorial measurements of metal high-dielectric-constant oxide structures and the release of the first nanoparticle reference materials. There are also important, ongoing projects to provide a spectrum of standard reference materials, standard test methods, and standard reference databases. These projects may not appear in refereed publications, but they do appear in thousands of laboratories worldwide as essential elements of research and production activities. TECHNICAL MERIT RELATIVE TO STATE OF THE ART The staff of the Ceramics Division are experienced, knowledgeable, and recognized as leading authorities in their respective fields. Evidence of the quality of the research being designed, organized, and conducted by the staff in the division includes the large number (185) of peer-reviewed publications in the past 18 months; collaborative relationships, both long and short term, with outside organizations such as the American Ceramic Society, other government agencies, and the National Cancer Institute (NCI); and national and international awards (e.g., election as fellows in technical societies and members of the National Academy of Engineering) received by staff members for their outstanding research accomplishments. 5 

The division is engaged in a wide range of important research topics, including the analysis, compilation, and dissemination of crystallographic and phase-equilibrium databases that serve thousands of materials engineers and scientists throughout the world. These topics also include modern and timely research fields such as nanodevices for measurement and standards, nanoparticles for medical applications, and synchrotrons for measuring the nanoscale structure of solids. The fact that all three NIST synchrotron beam lines are being used to capacity is strong evidence of the usefulness, capability, and demand for these state-of-the-art facilities. No major weaknesses were detected in the overall research program. The division staff is effectively evaluating the research projects on a timely basis and eliminating struggling projects in favor of projects in areas where future growth is more likely to occur. ADEQUACY OF INFRASTRUCTURE The FY 2008 technical portfolio of the Ceramics Division totals $13,030,000, with $830,000 supporting NIST Fellows’ projects. Technical work is grouped in four topical areas: nanomechanical properties, structure determination methods, functional properties, and synchrotron methods. The capabilities of the Ceramics Division to characterize materials by x-ray and synchrotron radiation, scanning probe microscopy, and other analytical techniques are, in aggregate, state of the art, and in several cases they are unique. Eleven laboratory modules in the AML—a state-of-the-art facility with Class 10,000 to Class 100 air quality, temperature control ranging from 0.25 oC down to 0.01 oC, and exceptional vibration control—provide x-ray metrology and nanomechanics laboratories and facilities needed to prepare standards required by U.S. industry to develop materials and devices based on nanotechnology. The capabilities on the beam lines in the NSLS at the Brookhaven National Laboratory incorporate unique equipment designed by NIST to provide measurement capabilities used by NIST scientists as well as many industrial and university-based collaborators. These noteworthy measurement capabilities have been directly applied to fulfilling the mission of the Ceramics Division to develop analytical techniques and SRMs. The division has worked effectively within its budget to develop its experimental capabilities, but some of the equipment (e.g., furnaces and x-ray diffraction equipment used in phase-diagram studies) has exceeded what would generally be considered its useful life. The division has an effective approach to assessing its staff and taking appropriate actions to address performance issues. The staff who presented their work to the panel were enthusiastic and articulate in describing their generally outstanding work. The Ceramics Division should increase efforts to compete more effectively for NRC postdoctoral students, both for the immediate capability that they bring and for their potential as future permanent staff. The productivity of the staff is outstanding, as measured by publications in refereed journals with high Institute for Scientific Information impact factor ratings. Moreover, the demand for the SRMs supplied by the division, including new reference materials developed for the emerging nanotechnology field—such as for gold nanoparticles—is evidence of the impact of the staff’s productivity. Recognition in the form of an invited paper in Science5 and the 2006 5 S.J.L. Billinge and I. Levin, 2007, “The Problem with Determining Atomic Structure at the Nanoscale,” Science, Vol. 316 (April 27): pp. 561-565. 6 

Outstanding Paper Award in Measurement Science and Technology6 is noteworthy. The refereed publications were appropriately supplemented by practice guides, such as Fractography of Ceramics and Glasses.7 ACHIEVEMENT OF OBJECTIVES AND IMPACT The Ceramics Division is meeting the NIST mission, vision, core competencies, and many of its core values. The division has suffered from limited hiring. It needs to compete more effectively for postdoctoral students in the NRC-administered National Academies Research Associateship Program. Measurement science, rigorous traceability, and the development and use of standards are, taken together, a core competence of the Ceramics Division. The division demonstrates customer focus to promote U.S. innovation and industrial competitiveness. Nanomechanical Properties Group The Nanomechanical Properties Group conducts five projects, all initiated between 2006 and 2008. Two of these make effective use of NIST’s comprehensive collection of state-of-the- art atomic-resolution testing capabilities in the AML: two scanning probe microscopes with capabilities including STM and AFM, two instrumented indenters with unprecedentedly small noise and thermal drift, and an optical interferometer with 1-nanometer-depth resolution. One of the AML-related projects has resulted in a highly precise prototype microfabricated cantilever beam array for calibrating commercial atomic force microscopes. This array has been employed by five vendors of atomic force microscopes and by users of these microscopes in industry, academia, and government. The other AML-related project has focused on nanoindentation for measurements of fracture and viscoelastic properties of materials and structures—including fracture toughness measurement in thin, amorphous films. A large component of one exciting project, focused on nanoscale-particle property measurements and standards, was initiated at the request of the National Cancer Institute in 2006. The NCI is engaged in an initiative to make use of the special properties of nanoscale particles to radically change the way that cancer is diagnosed, treated, and prevented. The NIST contribution, which makes very effective use of NIST core measurement competence, involves the development of measurements and standards for the physical characterization (with respect to size, surface area, charge, agglomeration, stability, and purity) of nanoscale particles of interest to the NCI program. The Ceramics Division-led NIST team has so far completed the first reference materials for biomedical applications, released in January 2008. These reference materials are for particles of 10, 30, and 60 nanometer diameter. Computational approaches are also under development in the Ceramics Division for specific particle properties. Two very recently initiated projects—Mechanical Reliability Measurements for Microelectromechanical Systems (MEMS) and Piezospectroscopy Measurements and Standards—appear to be well planned and oriented toward important applications. The former employs the design of a macroscale test structure in a novel manner for microscale structures, and the latter addresses nanoscale stress mapping with a NIST-built Raman optical probe. 6 R.S. Gates and J.R. Pratt, 2007, “Prototype Cantilevers for SI-Traceable Nanonewton Force Calibration,” Measurement Science and Technology, Vol. 17, no. 10, pp. 2852-2860. 7 National Institute of Standards and Technology, 2007, NIST Recommended Practice Guide: Fractography of Ceramics and Glasses, Gaithersburg, Maryland. 7 

Structure Determination Methods Group The portfolio of the Structure Determination Methods Group contains a balanced set of projects that were initiated during three separate decades. The database work is among the best, and the diffraction metrology work and standards work are excellent. The group’s mission is focused on SRMs, SRDs, computational tools, and x-ray, electron, and neutron diffraction. Core competencies lie in x-ray metrology; x-ray, electron, and neutron-based structure measurements; structure determination computational tools; and phase- equilibrium and crystallography determination. Customer engagement is strong, as demonstrated by SRM distribution through vendors with instrumentation packages, SRD licensing and distribution agreements, workshops, and the collaborative partnership with the American Ceramic Society on phase-equilibrium diagrams. The community demands that NIST continually improve SRMs; some 700 are sold each year. NIST certified the amorphous fraction of a 50:50 mixture of silicon and SRM 676a (alumina powder) to an accuracy that is considered to be the best; this is a noteworthy accomplishment. X-ray reflectometry can be used to measure the thickness and interfacial roughness of thin films repeatably. Many semiconductor industry partners demand this degree of measurement. The new work on measuring local structure is an excellent new start, and that work has been published in Science.8 The long-term work on ceramic phase-equilibrium data and crystallographic databases is among the best. Functional Properties Group The focus of the Functional Properties Group is measurement science, standards, and technology pertaining to the functional properties of advanced materials and devices, including ceramics and nanomaterials. The Functional Properties Group is a leader in three areas: combinatorial measurement methods, nanocalorimetry measurements, and thermoelectric measurements and standards. Of the three projects in these areas, one is almost mature— Combinatorial Measurement Methods for Advanced Complementary Metal Oxide Semiconductor (CMOS) Devices, a project that started in 2004. There are only two or three combinatorial thin-film synthesis laboratory facilities in the United States and a similar number in Japan. The NIST facilities are among the best of these and will be further enhanced by an atomic-layer deposition tool destined for the Nanofabrication Facility (located in the AML). For example, the material currently used for the CMOS is reaching its fundamental materials limit, and thus new materials are required by the $750 billion semiconductor industry. Semiconductor customers (Semiconductor Manufacturing Technology Consortium [SEMATECH], Intel Corporation, Micron Technology, Qualcomm, NIMS Japan, and IMEC, Belgium) are partnering with NIST to address this matter. Beyond the qualification of partners, the impact of the projects is measured by public recognition (Science Watch), invited NIST presentations, awards, effective partnership with users, SRM sales, database royalties, customer surveys, technology transfer to users, and patents (to a lesser degree). Regularly scheduled internal and external assessments of the Ceramics Division project portfolio by independent evaluators and customers or potential customers 8 S.J.L. Billinge and I. Levin, 2007, “The Problem with Determining Atomic Structure at the Nanoscale,” Science, Vol. 316 (April 27): pp. 561-565. 8 

identified in the MSEL project management process are critical to authenticating projects’ impact. An excellent opportunity exists for the Functional Properties Group to develop novel, combinatorial-compatible measurement methods. This quality work should be continued in order to help address these types of materials issues within the semiconductor industry. Synchrotron Methods Group Three mature projects that began in 1993 are found in the Synchrotron Methods Group, and the impact from this effort is expected to continue to increase when new facilities are constructed within the next several years. Support for synchrotron-related work was enhanced by funding through the America COMPETES Act, as discussed in the chapter on this funding. CONCLUSIONS The Ceramics Division is conducting high-quality research on a broad range of topics that strongly support the mission and core interests of the MSEL and NIST. The staff is using the financial resources and equipment at its disposal in an efficient manner. The research is widely recognized as being of high quality and in many instances is judged to be among the best. 9