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Metallurgy Division Publications - NISTIR 6907

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Program Overviews

Table of Contents

Advanced Manufacturing Methods

Contact Information: Stephen D. Ridder

An increasingly competitive manufacturing environment drives the search for new materials and processing techniques to make them. In most cases, materials processing steps determine the microstructure and performance of the material while manufacturing costs determine price. Industry needs measurement methods, standards, and data that will help monitor, control, and improve processing methods. These tools are also needed to help understand materials processing and to develop new processing methods and materials with enhanced properties. This is as true for highly developed, well-established industries as it is for rapidly growing or emerging industries. It is also true for all types of materials, processes, and products. The industrial competitiveness of the United States depends on U.S. manufacturers' ability to use the measurement tools to develop and advance their manufacturing methods. In many cases, the needed tools are generic and their impact would be greatly enhanced if they became industry wide standards. Therefore, MSEL is working to develop measurement methods and standards to enable industry to achieve these goals. This work is often being conducted in close collaboration with industry through consortia and standards organizations. The close working relationship developed with industry through these organizations not only ensures the relevance of the research projects, but also promotes an efficient and timely transfer of research information to industry for implementation. Since different materials and industries frequently have similar measurements needs, and most industrial products have multiple materials components, this program covers the processing of ceramics, metals, and polymers.

Research in the Ceramics Division focuses on development of test methods for the assessment of contact damage and wear, development of test methods and predictive models for evaluation of mechanical properties at elevated temperatures, and development of models for prediction of coating properties and performance. One project focuses on low temperature co-fired ceramics (LTCC), a manufacturing method being developed largely for portable wireless modules because it promises to allow for a reduction in the size and cost of modules used in high-frequency applications while improving performance. Because dimensional tolerances are critical in this process, accurate measurements and predictive models of dimensional changes during sintering are necessary for the commercialization of LTCC modules. Measurement methods and predictive models for the overall shrinkage and the local variations in sintering near vias and interconnects are being developed.

Projects in the Metallurgy Division cover several processing and measurement methods. The performance of metallic components in products is strongly dependent on processing conditions that determine microstructural features, such as grain size and shape, texture, the distribution of crystalline phases, macro- and microsegregation, and defect structure and distribution. Expertise is applied from a wide range of disciplines, including thermodynamics, electrochemistry, fluid mechanics, diffusion, x-ray, and thermal analysis, to develop measurement methods and understand the influence of processing steps for industries as diverse as automotive, aerospace, coatings, and microelectronics. Rapidly growing and emerging industries such as biotechnology and nanotechnology are dependent upon the development of new advanced manufacturing methods that can produce metallic components with the desired characteristics and performance. Current projects focus on measurements and predictive models needed by industry to design improved processing methods, provide better process control, develop improved alloy and coating properties, and reduce costs. Important processing problems being addressed include melting and solidification of welds, solidification of single crystals, powder production and consolidation, and coating production by thermal spray and electrodeposition.

Polymeric materials have become ubiquitous in the modern economy because of their ease of processing. However, these materials can exhibit complex and sometimes catastrophic responses to the forces imposed during manufacturing, thereby limiting processing rates and the ability to predict ultimate properties. The focus of the Polymers Division is directed towards microscale processing, modeling of processing instabilities, and on-line process monitoring of polymeric materials. Our unique extrusion visualization facility combines in-line microscopy and light scattering for the study of polymer blends, extrusion instabilities, and the action of additives. Current applications focus on understanding and controlling the "sharkskin instability" in polymer extrusion and observation of the dielectric properties of polymer nanocomposites. Fluorescence techniques are developed to measure critical process parameters such as polymer temperature and orientation that were hitherto inaccessible. These measurements are carried out in close collaboration with interested industrial partners.

Contact: Stephen D. Ridder

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Combinatorial Methods

Contact Information: Leonid A. Bendersky

The Combinatorial Methods Program develops novel high-throughput measurement techniques and combinatorial experimental strategies specifically geared towards materials research. These tools enable the industrial and research communities to rapidly acquire and analyze physical and chemical data, thereby accelerating the pace of materials discovery and knowledge generation. By providing measurement infrastructure, standards, and protocols, and expanding existing capabilities relevant to combinatorial approaches, the Combinatorial Methods Program lowers barriers to the widespread industrial implementation of this new R&D paradigm.

The Combinatorial Methods Program has adopted a two-pronged strategy for meeting these goals. The first of these is an active research and development program designed to better tailor combinatorial methods for the materials sciences and extend the state of the art in combinatorial techniques. Measurement tools and techniques are developed to prepare and characterize combinatorial materials libraries, often by utilizing miniaturization, parallel experimentation, and a high degree of automation. A key concern in this effort is the validation of these new approaches with respect to traditional "one at a time" experimental strategies. Accordingly, demonstrations of the applicability of combinatorial methods to materials research problems provide the scientific credibility needed to engender wider acceptance of these techniques in the industrial and academic sectors. In addition, the successful adoption of the combinatorial approach involves a highly developed "workflow" scheme. All aspects of combinatorial research, from sample "library" design and library preparation to high-throughput assay and analysis, must be integrated through an informatics framework which enables iterative refinement of measurements and experimental aims. Combinatorial Methods Program research projects give illustrations of how these processes are implemented effectively in a research setting.

NIST-wide research collaborations, facilitated by the Combinatorial Methods Program, have produced a wide range of new proficiencies in combinatorial techniques which are detailed in a brochure, "Combinatorial Methods at NIST" (NISTIR 6730), and online at Within MSEL, novel methods for combinatorial library preparation are designed to encompass variations of diverse physical and chemical properties, such as composition, film thickness, processing temperature, surface energy, chemical functionality, UV-exposure, and topographic patterning of organic and inorganic materials ranging from polymers to nanocomposites to ceramics. In addition, new instrumentation and techniques enable the high-throughput measurements of adhesion, mechanical properties, and failure mechanisms, among others. The combinatorial effort extends to multiphase, electronic, and magnetic materials, including biomaterials assays. On-line data analysis tools, process control methodology, and data archival methods are also being developed as part of the Program's informatics effort.

The second aspect of the Combinatorial Methods Program is an outreach effort designed to facilitate technology transfer with institutions interested in acquiring combinatorial capabilities. The centerpiece of this effort is the NIST Combinatorial Methods Center (NCMC), an industry-university-government consortium organized by MSEL that became operational on January 23, 2002 via a kick-off meeting in San Diego. Although it is still in the growth stage, the impact of NCMC activities is readily apparent as 11 industrial partners and the Air Force Research Lab have already joined the NCMC membership program. The NCMC facilitates direct interaction between NIST staff and these industrial partners, and provides a conduit by which Combinatorial Methods Program research products, best practices and protocols, instrument schematics and specifications, and other combinatorialrelated information can be effectively disseminated. This outreach is mediated in large part by a series of tri-annual workshops for NCMC members. The first NCMC meeting, "Library Design and Calibration," was held on April 26, 2002 at NIST, and it provided information essential to starting a combinatorial research effort. The second meeting (October 2002) will concentrate on combinatorial approaches to adhesion and mechanical properties. Further information on NCMC can be found on the website at

Contact: Leonid A. Bendersky

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Data Evaluation and Delivery

Contact Information: Carlos R. Beauchamp

Accurate materials data are increasingly critical to the rapid design and manufacture of the cost-effective, reliable products that characterize 21st century life. The MSEL Data Evaluation and Delivery Program is working to facilitate the building of interoperable materials structure, phase, and property databases needed by the scientific and industrial communities, and to develop strategies for visualizing multi-dimensional datasets needed for materials selection in product design.

To this end, the FY2002 Projects in the MSEL Data Evaluation and Delivery Program were focused on:

• Improving materials data transfer between databases through development of a standard materials mark-up language (MatML);

• Developing a major compilation of elastic moduli data for polycrystalline oxide ceramics;

• Providing protocols for data evaluation to ensure that databases are populated with accurate data;

• Expanding the Ceramics WebBook which provides links to other sources of ceramic data and manufacturer's information, as well as selected data sets evaluated by NIST, including structural ceramics and high temperature superconductor databases, glossaries, and tools for analysis of ceramic materials;

• Completing the first release of a new Windows-based PC product for the Inorganic Crystal Structure Database in cooperation with Fachinformationszentrum (FIZ) Germany

• Producing phase diagrams through the NIST/ American Ceramic Society, Phase Equilibria Program;

• Developing approaches to viewing multidimensional mechanical property and phase diagram data for metals, through a series of simple - but useful - interactive calculations;

• Establishing a prototype site for linking NIST materials data with external datasets such as those developed and maintained by ASM International; and

• Developing a comprehensive database of critically evaluated properties of lead-free solders including multi-dimensional data from three national consortia, the National Center for Manufacturing Sciences (NCMS) Lead-Free Solder Project, the NCMS Fatigue Resistant Lead-Free Solder Project, and the National Electronics Manufacturing Initiative (NEMI) Lead-Free Assembly Project.

Contact: Carlos R. Beauchamp

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Forming of Lightweight Material for Automotive Applications

Contact Information: Lyle E. Levine

Automobile manufacturing is a materials intensive industry that involves about 10% of the U.S. workforce. In spite of the use of the most advanced, cost-effective technologies, this globally competitive industry still has productivity issues related to measurement science and data. Chief among these is the difficulty encountered in die manufacture for sheet metal forming. In a recent Advanced Technology Program-sponsored workshop (The Road Ahead, June 20-22, 2000, at USCAR Headquarters), the main obstacle to reducing the time between accepting a new design and actual production of parts was identified as producing working die sets. This problem exists even for traditional alloys with which the industry is familiar. To benefit from the weight saving advantages of high strength steel and aluminum alloys, a whole new level of formability measurement methods and data is needed, together with a better understanding of the physics behind metal deformation.

This program is meeting these industrial needs by developing: 1) standard formability test methods, 2) models for surface roughening and friction during stamping, 3) multiscale, physically-based constitutive laws, 4) models for anelasticity and springback prediction, and 5) measurements of texture and residual stress evolution. Our recently established sheet metal formability laboratory is now adding in situ X-ray equipment for measuring stress in sheet metal samples during multiaxial deformation. This laboratory permits us to investigate industrially important measurement problems in formability and pursue standard test methods for formability. The facility provides test samples of multiaxially deformed metal for other aspects of this program. For example, deformation-induced surface roughening of sheet metal is a poorly understood phenomenon that is highly relevant to industry. We are currently performing controlled experiments on multiaxially strained sheets to develop a surface roughening database and a generic model which industry has identified as a high priority need. The test methods and surface roughening projects were selected by the Industrial Liaison Office of NIST for a pilot survey aimed at obtaining comprehensive, non-biased feedback from industry. They received high scores on all aspects including industrial relevance and potential impact. On a more fundamental level, MSEL's advanced characterization capabilities (TEM, AFM, Synchrotron Radiation, NCNR) are being used to understand the basic dislocation patterning responsible for the observed behavior of metals. A predictive model based on percolation theory has been developed from the measurements and observations. All aspects of the research at NIST will impact our customers by improving the commercially available, finite element computer codes that are heavily used by this industry. A key element in the design of this program is that an insight or advancement gained in one area can be immediately used in a piecewise fashion in the design process, i.e., total success of the program is not required to have an impact. Other means of transferring this technology, such as through standardizing organizations and by direct interaction with industrial counterparts, are being pursued. While targeting the auto industry, our research will have extended applications to all other industries that employ metal forming in their production lines.

Contact: Lyle E. Levine

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Materials for Micro- and Optoelectronics

Contact Information: Frank W. Gayle

U.S. microelectronics and related industries are in fierce international competition to design and produce smaller, lighter, faster, more functional, and more reliable electronics products more quickly and economically than ever before. At the same time, there has been a revolution in recent years in new materials used in all aspects of microelectronics fabrication.

Since 1994, the NIST Materials Science and Engineering Laboratory (MSEL) has worked closely with the U.S. semiconductor, component, packaging, and assembly industries. These efforts led to the development of an interdivisional MSEL program committed to addressing industry's most pressing materials measurement and standards issues central to the development and utilization of advanced materials and material processes. The vision that accompanies this program - to be a key resource within the Federal Government for materials metrology development for commercial microelectronics manufacturing - is targeted through the following objectives:

• Develop and deliver standard measurements and data;

• Develop and apply in situ measurements on materials and material assemblies having micrometer- and submicrometer-scale dimensions;

• Quantify and document the divergence of material properties from their bulk values as dimensions are reduced and interfaces contribute strongly to properties;

• Develop models of small, complex structures to substitute for, or provide guidance for, experimental measurement techniques; and

• Develop fundamental understanding of materials needed in future micro- and opto-electronics and magnetic data storage.

With these objectives in mind, the program presently consists of projects led by the Metallurgy, Polymers, Materials Reliability, and Ceramics Divisions that examine and inform industry on key materials-related issues. These projects are conducted in concert with partners from industrial consortia, individual companies, academia, and other government agencies. The program is strongly coupled with other microelectronics programs within government and industry, including the National Semiconductor Metrology Program (NSMP) at NIST. Materials metrology needs are also identified through industry groups and roadmaps including the International Technology Roadmap for Semiconductors (ITRS), International SEMATECH, the IPC-Embedded Passive Devices Taskgroup, the IPC Lead-free Solder Roadmap, the National Electronics Manufacturing Initiative (NEMI) Roadmap, the Optoelectronics Industry Development Association (OIDA) roadmaps, and the National [Magnetic Data] Storage Industry Consortium (NSIC).

Although there is increasing integration within various branches of microelectronics and optoelectronics, the field can be considered to consist of three main areas. The first, microelectronics, includes needs ranging from integrated circuit fabrication to component packaging to final assembly. MSEL programs address materials metrology needs in each of these areas, including, for example, lithographic polymers and electrodeposition of interconnects, electrical, mechanical, and physical property measurement of dielectrics (interlevel, packaging, and wireless applications), and packaging and assembly processes (lead-free solders, solder interconnect design, thermal stress analysis, and co-fired ceramics).

The second major area is optoelectronics, which includes work that often crosses over into electronic and wireless applications. Projects currently address residual stress measurement in optoelectronic films, and wide bandgap semiconductors. Cross-laboratory collaborations with EEEL figure prominently in this work.

The third area is magnetic data storage, where the market potential is already large and growing and the technical challenges extreme. NSIC plans to demonstrate a recording density of 40 times today's level by 2006. To reach these goals, new materials are needed that have smaller grain structures, can be produced as thin films, and can be deposited uniformly and economically. New lubricants are needed to prevent wear as the spacing between the disk and head becomes smaller than the mean free path of air molecules. MSEL is working with the magnetic recording industry to develop measurement tools, modeling software, and magnetic standards to help achieve these goals. MSEL works in close collaboration with the Electronics and Electrical Engineering Laboratory, the Physics Laboratory, the Information Technology Laboratory, and the Manufacturing Engineering Laboratory as partners in this effort.

Contact: Frank W. Gayle

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Materials Property Measurement

Contact Information: Samuel R. Low, III

This program responds both to MSEL customer requests and to the DOC 2005 Strategic Goal of "providing the information and framework to enable the economy to operate efficiently and equitably." For example, manufacturers and their suppliers need to agree on how material properties should be measured. Equally important, engineering design depends on accurate property data for the materials that are used.

The MSEL Materials Property Measurement Program works toward solutions to measurement problems, on scales ranging from the macro to the nano, in four of the Laboratory's Divisions (Ceramics, Materials Reliability, Metallurgy, and Polymers). The scope of its activities goes from the development and innovative use of state-of-the-art measurement systems, to leadership in the development of standardized test procedures and traceability protocols, to the development and certification of Standard Reference Materials (SRMs). A wide range of materials is being studied, including polymers, ceramics, metals, and thin films (whose physical and mechanical properties differ widely from the handbook values for their bulk properties).

Projects are directed to innovative new measurement techniques. These include:

• Measurement of the elastic, electric, magnetic, and thermal properties of thin films and nanostructures (Materials Reliability Division);

• Alternative strength test methods for ceramics, including cylindrical flexure strength and diametral compression (Ceramics Division); and

• Coupling micromechanical test methods with failure behavior of full-scale polymer composites through the use of microstructure-based object-oriented finite element analysis (Polymer Division in collaboration with the Automotive Composites Consortium).

The MSEL Materials Property Measurement Program is also contributing to the development of test method standards through committee leadership roles in standards development organizations such as ASTM and ISO. In many cases, industry also depends on measurements that can be traced to NIST Standard Reference Materials (SRMs). This program generates the following SRMs for several quite different types of measurements.

• Charpy impact machine verification (Materials Reliability Division);

• Hardness standardization of metallic materials (Metallurgy Division);

• Hardness standardization and fracture toughness of ceramic materials (Ceramics Division); and

• Supporting the Materials Property Measurements Program is a modeling and simulation effort to connect microstructure with properties. The Object-Oriented Finite-Element (OOF) software developed at NIST is being used widely in diverse communities for material microstructural design and property analysis at the microstructural level.

In addition to the activities above, the Materials Reliability, Metallurgy, Ceramics, and Polymers Divisions provide assistance to various government agencies on homeland security and infrastructural issues. Projects include assessing the performance of structural steels as part of the NIST World Trade Center Investigation, advising the Bureau of Reclamation (BOR) on metallurgical issues involving a refurbishment of Folsom Dam, advising the Department of the Interior on the structural integrity of the U.S.S. Arizona Memorial, advising the U.S. Customs Service on materials specifications for ceramics, and advising the Architect of the Capitol on repair procedures for cracks in the outer skin of the Capitol Dome.

Contact: Samuel R. Low

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Materials Structure Characterization

Contact Information: John E. Bonevich

Materials science and engineering is the area of science concerned with understanding relationships between the composition, structure, and properties of materials and the application of this knowledge to the design and fabrication of products with a desired set of properties. Thus, measurement methods for the characterization of materials structure are a cornerstone of this field. MSEL supports a wide array of techniques and instrumentation for materials measurements. Facilities include optical and electron microscopy, optical and electron scattering and diffraction, and major x-ray facilities at the National Synchrotron Light Source (NSLS) at Brookhaven Laboratory, and at the Advanced Photon Source (APS) at Argonne National Laboratory.

Synchrotron radiation sources provide intense beams of x-rays enabling leading-edge research in a broad range of scientific disciplines. Materials characterization using x-rays from synchrotron sources forms a major part of the Materials Structure Characterization Program. This includes the development and operation of experimental stations at the NSLS and at the APS. At the NSLS, NIST operates a soft x-ray station in partnership with Dow and Brookhaven National Laboratory. At the APS, NIST is a partner with the University of Illinois at Urbana /Champaign, Oak Ridge National Laboratory, and UOP, in a collaboration called UNICAT. At both facilities, NIST scientists, and researchers from industry, universities, and government laboratories, perform state-of-the-art measurements on a wide range of advanced materials. Studies currently underway include: ceramic coatings; defect structures arising during deformation of metals, ceramics, and polymers; defect structures in semiconductors and single-crystal proteins; and atomic-scale and molecularscale structures at surfaces and interfaces in polymeric, catalytic, and metal /semiconductor systems.

Ceramic powders are precursors for over 80% of ceramic manufacturing. As a result, a major focus in the Ceramics Division is the accurate and reliable measurement of the physical and chemical properties of ceramic powders, including sub-micrometer and nanometer sized powders. These measurements are critical to ensuring processes and products of high quality, minimal defects, and consequent economic benefits. Another area of concern to ceramic manufacturing is powder dispersion in a fluid vehicle for shape forming and other uses. The chemical and physical characteristics of powders dispersed in liquids are evaluated to understand the influence of surface charge, dissolution, precipitation, adsorption, and other physicochemical processes on the dispersion behavior. In addition to these activities, standard reference materials for use as primary calibration standards and national /international standards for particle size and size distribution, pore volume, and particle dispersion measurements are being developed in collaboration with industrial partners, measurement laboratories, and academic institutions in the U.S., Europe, and Asia.

The NIST effort in materials characterization has a strong emphasis on electron microscopy, which is capable of revealing microstructures within modern nanoscale materials and atomic-resolution imaging and compositional mapping of complex crystal phases with novel electronic properties. The MSEL microscopy facility consists of two high-resolution transmission electron microscopes (TEM) and a high-resolution, field-emission scanning electron microscope (FE-SEM) capable of resolving features down to 1.5 nm. Novel experimental techniques using these instruments have been developed to study multilayer and nanometer-scale materials.

Through this MSEL Program, measurement methods, data, and standard reference materials (SRMs) needed by the U.S. polymers industry, research laboratories, and other federal agencies are provided to characterize the rheological and mechanical properties of polymers and to improve polymer processibility. In response to critical industry needs for in-situ measurement methodologies, a substantial effort is underway to develop optical, dielectric, and ultrasonic probes for characterizing polymer processing. Improved methods for determining molecular mass distribution of polymers are developed because of the dramatic effect it has on processibility and properties. Mechanical properties and performance are significantly affected by the solid-state structure formed during processing. Importantly, unlike many other common engineering materials, polymers exhibit mechanical properties with time dependent viscoelastic behaviors. As a result, techniques are being developed that measure the solidstate structure and rheological behavior of polymeric materials. Recent program activities exploit advances in mass spectrometry using matrix assisted laser desorption ionization (MALDI) to develop a primary tool for the determination of the molecular masses of synthetic polymers, with particular emphasis on commercially important polyolefins. The polymer industry and standards organizations assist in the identification of current needs for SRMs, and based on these needs, research on characterization methods and measurements is conducted leading to the certification of SRMs.

Contact: John E. Bonevich

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