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

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Programs Funded Under the America COMPETES Act SUMMARY The funding under the America COMPETES Act started in FY 2007, so it is early to assess its impact. The projects benefiting from the funding are well conceived, and the first results are positive. The Ceramics Division is responsible for enhancing the NIST capability in the National Synchrotron Light Source at the Brookhaven National Laboratory. It is effectively applying the funding to attain new capability such as interfacial structure measurements on high- dielectric-constant gate oxides. The enhanced research capability is significant enough that it should be managed in a way that brings broader participation from NIST in establishing priorities for the portion of beam time that NIST controls. The Metallurgy and the Materials Reliability Divisions share in executing a program to develop standards and test protocols related to the hydrogen economy—specifically, to the safety of pipelines to transport hydrogen under high pressure. A flexible research and test facility is under construction at the NIST facility in Boulder that promises to greatly enhance the capability of NIST to study this complex problem. A related project to measure hydrogen content rapidly in order to assess materials compatibility is solid but small. The project to build the first broadband coherent anti-Stokes Raman scattering microscope is off to a good start in the Polymers Division. CERAMICS DIVISION A strong core competence of the Ceramics Division is in the area of x-ray measurements on materials, in which the use of a synchrotron as the x-ray source represents a very important class of measurement technique. Synchrotrons provide a source of x-ray radiation that is intense, bright, collimated, tunable, and polarized—all characteristics not available from laboratory x-ray sources. This technique offers uniquely accurate subnanometer-resolution measurements of the electronic, chemical, and spatial structure of advanced materials, including semiconductor electronic materials, polymeric materials, nanotubes, catalysts, and biomaterials. The Synchrotron Methods Group within the Ceramics Division focuses on three important technical areas: the development of synchrotron measurement methods, material structural determination using synchrotron measurements, and synchrotron beam-line operations at the National Synchrotron Light Source, a DOE national user facility at the Brookhaven National Laboratory in New York. NIST’s Synchrotron Methods Group operates three beam lines (experiment stations) that have x-ray wavelengths appropriate for measurements on materials spanning the entire Periodic Table of the Elements. The NIST group is widely recognized as a pioneer and leader in the development and application of synchrotron-based techniques, and opportunities to use the NIST beam lines are in high demand. Although the facility operates full 24-hour days, industry and academia applicants seeking facility measurement opportunities exceed capacity by nearly 2 to 1. The expertise of the NIST team lies principally in the area of specialized detectors. The funding under the America COMPETES Act has been directed toward several specific capability upgrades: • A state-of-the-art analyzer and multi-element detector for near-edge x-ray absorption spectroscopy (NEXAFS) capability was installed in 2007 on beam line U7A. In 23 

addition, funding has been committed to the NIST Electronics and Electrical Engineering Laboratory in Boulder, Colorado, for the development of a detector to provide unprecedented NEXAFS sensitivity and selectivity. This work is in progress and slated for completion in December 2009. The application of this capability is in the surface chemistry and molecular structure of materials, including self-assembled monolayers, deoxyribonucleic acid (DNA), proteins, other biological materials, organic and molecular electronics, polymer surfaces and interfaces, catalysts, and nanotubes. • A new detector for extended x-ray absorption fine structure capability was installed in 2007 on beam line X23A2. The application of this capability is in measuring local atomic and electronic structures from nanolayer thin films to bulk materials and from crystalline to highly disordered materials of higher molecular weight (beginning with titanium on the Periodic Table). • A new, high-throughput endstation for x-ray standing wave spectroscopy capability was installed in 2007 on beam line X24A. This line is used for the lower- and middle-molecular-weight materials. • A major project, in excess of $1 million capital, was begun in partnership with Sandia National Laboratories to implement a new variable kinetic energy x-ray photoelectron spectroscopy (VKE-XPS) capability on beam line X24A for high- spatial-resolution measurements. The new surface measurement capability will be completed in 2008, and enhanced depth measurements, to less than 1 nanometer, will be completed in 2009. A scientific program using the high-throughput VKE- XPS was initiated with SEMATECH to study next-generation transistor gate layer structures. • A novel three-dimensional VKE-XPS chemical microscope is under development, also for beam line X24A. This capability will provide strategic chemical and structural insights in nanotechnology applications such as transistor gate-stacks, organic electronics, MEMS lubrication, self-assembled-monolayer templates, and catalysts. The project is a Phase II SBIR collaboration slated for delivery in the summer of 2009. • Owing to the unexpected flat funding under the America COMPETES Act in 2008, two projects were put on hold: the Synchrotron Enhanced Scanning Tunneling Microscopy project and the Modernized High-Resolution Diffraction Beamline project. An exciting and very timely development is the DOE announcement that a new, billion- dollar beam line—NSLS II—will be built on the Brookhaven site, with groundbreaking in 2009 and occupancy starting in 2012. The x-ray radiation source will be 10,000 times brighter than the current NSLS, with the potential for major enhancements in measurement capabilities. The existence of the NIST ACI Synchrotron project enables NIST to plan construction of two new state-of-the-art beam lines in the new facility. The NIST team has already begun responding to this exciting and unique opportunity to maintain leadership in synchrotron-based materials measurements. The capability emerging from the enhanced funding is broadly applicable to NIST programs; therefore, it may be desirable to establish a formal process for prioritizing the projects that are performed during the time that the facility is under NIST control. (The DOE user- 24 

facility process that competitively selects projects determines who uses the beam lines the remainder of the time.) MATERIALS RELIABILITY DIVISION The hydrogen pipeline safety project is part of a coordinated NIST program to develop the infrastructure for a hydrogen economy. The Metallurgy Division is focusing on research and development test methods to look at issues such as developing hydrogen-resistant alloys and looking at supersaturation effects on alloys. The Materials Reliability Division has taken responsibility for measuring the mechanical properties, in the presence of hydrogen, of existing and new high-strength pipeline steels. The purpose is to ascertain whether, and at what pressures, existing gas or petroleum pipelines in the United States could be used for shipping hydrogen around the country in preparation for a possible hydrogen fuel economy. This is an essential material property measurement activity for which the Materials Reliability Division is well equipped based on its past and present experience in bulk material property mechanical testing and pipeline testing. The facility that the division needs for extending its capabilities to testing in hydrogen is under construction and will give NIST at Boulder an unrivaled facility for testing pipeline steels under realistic hydrogen transportation conditions. METALLURGY DIVISION One project in the Metallurgy Division modestly funded through the America COMPETES Act is focused on competitiveness relative to the hydrogen economy. Since the project is at an early stage, an assessment of it may be premature; however, in general it is off to a good start. It is the Hydrogen Distribution (hydrogen embrittlement of steels) project, which has a sound technical approach and is a worthwhile activity. NIST has the required expertise to meet the project’s objectives. The level of coordination between MSEL divisions on this project is excellent. The tie between this project and increasing American competitiveness is somewhat tenuous, but the transportation of gaseous hydrogen is clearly important to the success of the hydrogen economy. A second project receiving funding through the America COMPETES Act is an effort to develop a rapid high-throughput measurement of hydrogen content for assessing novel materials for hydrogen storage. This Hydrogen Storage project is technically sound and has demonstrated the feasibility of a new measurement approach (infrared emissivity) for attacking this problem. The magnitude of the effort may be too small to make a major impact. If successful, when the hydrogen economy becomes a reality, this project could assist in spawning new industries, thus improving U.S. competitiveness. POLYMERS DIVISION The Bioimaging Program and efforts in optical coherence microscopy, broadband coherent anti-Stokes Raman scattering (CARS) microcopy, and the associated technology efforts fit the mission of ACI. The Optical Coherence Microscopy Program is on its pathway to commercialization with an SBIR Phase III program. CARS technology is unique because of its ability to image cells with three-dimensional spatial resolution, non-invasively and without using labels. Using contrast in vibrational spectra, CARS microscopy can provide physical and 25 

chemical information from the cells to characterize their response to different materials as well as determine differences in spatial heterogeneities between normal and diseased cells. The Bioimaging Program built the first broadband CARS instrument in 2004, has more recently developed time-resolved detection methods to reduce nonresonant background, and has developed algorithms for faster and flexible spectral recovery. 26