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Metallurgy Division Publications - NISTIR 6797

Annual Report cover graphic

Program Overviews

Table of Contents

Forming of Lightweight Materials for Automotive Applications

Contact Information: Richard J. Fields

Automobile manufacturing is a materials intensive industry that involves about 10% of the US 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 ATP sponsored workshop (The Road Ahead, June 20-22, 2000, at U. S. Council for Automotive Research (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. Figure 1 shows an example of where the cost of tooling (dies) is the largest single cost in the production of parts for small cars. (This does not include assembly costs.)

Figure 1. Part cost breakdown for small cars.
(Kelkar et al., J. of Metals, pp 28-32, Aug 2001.)

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 project is meeting the industrial needs (see Table 2) by developing standard formability test methods, multiscale, physically-based constitutive laws, and models for consolidation of aluminum matrix composites. In the past year, we have established a sheet metal formability laboratory. A state-of-the-art formability testing machine equipped with an advanced surface displacement analysis system permits us to investigate industrially important measurement problems in formability and pursue standard test methods for formability. The facility provides test samples of biaxially 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 biaxially strained sheets to develop a surface roughening data base and a generic model which industry has identified as a high priority need.

Table 1. Industries needs being met by NIST solutions.

On a more fundamental level, we are using MSEL's advanced characterization capabilities such as transmission electron microscopy, synchrotron radiation, and neutron scattering at the NIST National Center for Neutron Research 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.

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Materials for Magnetic Data Storage

Contact Information: Robert D. Shull

For the magnetic data storage industry, the market potential is vast and growing, but global competition is intense, and the technical challenges extreme. Leading commercial magnetic disk drives today store about 25 gigabits of data per square inch. The National Storage Industry Consortium (NSIC) plans to demonstrate a recording density of 1 terabit per square inch—40 times today's level—by 2006.

New materials are needed that have smaller grain structures, can be produced as thin films, and can be deposited uniformly and economically. Recording heads must be designed to produce higher output signals and lower noise. Component dimensions must be made smaller, and the measurements more precise. New lubricants are needed to prevent wear as spacing between the disk and head becomes smaller than the mean free path of air molecules. New methods are needed to standardize components and increase yields.

The National Institute of Standards and Technology is working to achieve these goals. For the past century, NIST has been helping U.S. magnetic data storage industries invent and manufacture product with superior reliability. NIST offers state-of-the-art technology, measurement tools, and standards—many of which cannot be found elsewhere—as well as a reputation for technical excellence and neutrality. Staff expertise spans all fields relevant to magnetic data storage, including materials science, electrical engineering, physics, mathematics and modeling, manufacturing engineering, chemistry, metrology, and computer science. By addressing important measurement issues in magnetism, by bringing together the industrial and scientific communities through the organization of workshops and conferences in the area, and by the development and preparation of appropriate standards, NIST acts to accelerate the use of advanced magnetic data storage materials by the industrial sector, and to enable industry to take advantage of new discoveries and innovations. In addition, close linkage with NSIC increases the industrial relevance of our program and improves technology transfer. Additional collaborations with Xerox, General Motors, Hewlett Packard, IBM, Seagate, and Motorola Corporations, for example, enable NIST to leverage its activities with the much larger, but complementary, capabilities of other organizations.

In FY2001, the Program on Materials for Magnetic Data Storage in the Materials Science and Engineering Laboratory focused on the following projects that were continued from the previous year:

• Processing of magnetic multilayers for optimal giant magnetoresistance effect (Metallurgy Division)

• Magnetic domain imaging and micromagnetic modeling of magnetic domains for understanding magnetization statics and dynamics in recording heads and magnetic media (Metallurgy Division)

• Understanding the nanotribology of magnetic hard disks through the measurement of stiction, friction, and wear at the nanometer scale (Ceramics Division)

• Measuring nanoscale magnetic interactions and structure in multilayers, nanocomposites, and low dimensional systems, needed for understanding and applying materials physics at small scales (Metallurgy Division, NIST Center for Neutron Research)

• Measuring and understanding the origin of magnetic exchange bias in conventional and advanced magnetic structures and devices (Metallurgy Division, NIST Center for Neutron Research)

• Developing a measurement system for magnetic susceptibility of small samples at high frequencies (Metallurgy Division)

• Preparing magnetic measurement standard reference materials. (Metallurgy Division)

Two new projects were initiated in FY2001:

• Processing and measuring the properties of "spintronic" systems wherein spin-dependent magnetic devices are integrated directly onto semiconductor chips (DARPA-sponsored; Metallurgy Division)

• Developing measurements of magnetic damping (NIST Nanotechnology Initiative Funding with EEEL; Metallurgy and Materials Reliability Divisions.)

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Materials for Microelectronics

Contact Information: Frank W. Gayle

Today's U.S. microelectronics and supporting infrastructure industries are in fierce international competition to design and produce new smaller, lighter, faster, more functional, and more reliable electronics products more quickly and economically than ever before.

Recognizing this trend, in 1994 the NIST Materials Science and Engineering Laboratory (MSEL) began working very closely with the U.S. semiconductor, component and packaging, and assembly industries. These early 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 within new product technologies, as outlined within leading industry roadmaps. The vision that accompanies this program - to be the key resource within the Federal Government for materials metrology development for commercial microelectronics manufacturing - may be realized 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 microelectronics.

With these objectives in mind, the program presently consists of twenty separate projects that examine and inform industry on key materials-related issues, such as: electrical, thermal, microstructural, and mechanical characteristics of polymer, ceramic, and metal thin films; solders, solderability and solder joint design; photoresists, interfaces, adhesion and structural behavior; electrodeposition, electromigration and stress voiding; and the characterization of next generation interlevel and gate dielectrics. 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.

FY2001 Projects (and division leading project)

Lithography/Front End Processing

• Characterization of Ultrathin Dielectric Films (Ceramics)

• Lithographic Polymers (Polymers)

On-chip Interconnects

• Interconnect Materials and Reliability Metrology (Materials Reliability)

• Measurements and Modeling of Electrodeposited Interconnects (Metallurgy)

• Thin Film Metrology for Low K Dielectrics (Polymers)

Packaging and Assembly

• Packaging Reliability (Materials Reliability)

• Solder Interconnect Design (Metallurgy)

• Solders and Solderability Measurements for Microelectronics (Metallurgy)

• Tin Whisker Mechanisms (Metallurgy)

• Wafer Level Underfill Experiment and Modeling (Metallurgy)

• Wire Bonding to Cu/Low-K Semiconductor Devices (Metallurgy)

• X-ray Studies of Electronic Materials (Materials Reliability)

Crosscutting Measurements

• Dielectric Constant and Loss in Thin Films and Composites (Polymers)

• Electron Beam Moiré (Materials Reliability)

• Ferroelectric Domain Stability Measurements (Ceramics)

• Measurement of In-Plane Thermal Expansion and Modulus of Polymer Thin Films (Polymers)

• Mechanical Properties of Thin Films (Ceramics)

• Permittivity of Polymer Films in the Microwave Range (Polymers)

• Polymer Thin Films and Interfaces (Polymers)

• Texture Measurements in Thin Film Electronic Materials (Ceramics)

• Thermal Conductivity of Microelectronic Structures (Materials Reliability)

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Metals Characterization

Contact Information: Samuel R. Low, III

Engineering design depends on the specification of the properties of the materials that are used. Equally important, manufacturers and their suppliers need to agree on how these properties should be measured. The MSEL Metals Characterization Program, centered within the Metallurgy and the Materials Reliability Divisions, spans the measurement spectrum from the 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).

The NIST effort in metals 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 the mechanical properties of multilayered and nano-scaled materials.

The Metals Characterization Program is 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.

Hardness of Metallic Materials (Metallurgy Division): Hardness is the primary test measurement used to determine and specify the mechanical properties of metal products. The hardness standardization project is providing industry with primary transfer standards for the Rockwell hardness and Vickers and Knoop microhardness scales. These SRM test block standards are used for the periodic calibration of hardness testing machines.

Magnetic Properties (Metallurgy Division): The need for reliable magnetic measurements is becoming increasingly acute because of new technologies involving magnetic phenomena in data storage and microelectronics. Such measurements require calibration of magnetometers using certified magnetic standards in several different shapes and magnetic strengths, and with a wide range in magnetic character. These standards are now being produced under this program.

Coating Thickness (Metallurgy Division): Coating thickness standards are produced by electrodeposition and are widely used for calibration of coating-thickness measuring instruments. SRM coupons are produced with a wide range of thicknesses, and are bar coded to allow analysis of degradation and life expectancy when the standards are returned for verification.

Charpy Impact (Materials Reliability Division): The Charpy impact machine verification project provides rapid, accurate assessment of test data generated by our customers using SRM Charpy standards, and, where merited, certifies the conformance of Charpy impact test machines to ASTM Standard E 23. Participation in ISO Committee TC 164, assures that specimens and procedures are compatible with international standards.

In addition to the SRM activities above, NIST (Materials Reliability Division) provides assistance to the Bureau of Reclamation (BOR) on metallurgical issues that arise during maintenance, inspection, and failure assessment of dams and water conveyance infrastructure projects. NIST advice and data provide BOR engineers with an independent check of other input.

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Metals Processing

Contact Information: Stephen D. Ridder

The Metals Processing Program applies NIST expertise in a wide range of disciplines, including thermodynamics, electrochemistry, fluid mechanics, diffusion, x-ray, and thermal analysis, to understand the processing steps which will lead to products having the desired form and properties, at an acceptable cost. Working with industries ranging as widely as automotive, aerospace, coating, and microelectronics, several important processing problems are being addressed including melting and solidification of welds, castings of single crystals, powder production and consolidation, and coating production by thermal spray and electrodeposition.

The increasingly competitive manufacturing environment fuels the search for new metal alloys as well as efficient processing techniques to fully realize their potential. The processing cycle can include many steps, including a formation process such as casting or electrodeposition, a heat treatment process, a deformation process such as rolling or stamping, joining by welding, or coating to enhance surface properties. In each of these processes, the distribution of crystal phases, the grain structure, the alloy compositional segregation, and the defect structure are altered, with resulting changes in properties such as strength, ductility, corrosion resistance, and conductivity which form the basic rationale for the use of metals in industrial products. The following projects in the Metals Processing Program 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.

• Modeling of Solidification and Microstructure Development: (Metallurgy Division): Models of alloy solidification, crystal growth processes and heat treatment are being developed to aid industry in designing production systems that increase product yield and performance.

• Processing-Structure-Property Data For Thermal Spray Coatings (Metallurgy Division): Coating reproducibility and reliability are addressed by the development and calibration of advanced sensors, applying these measurement tools to the control and characterization of TS coatings, and working with the Thermal Spray (TS) community to establish a coating processing-microstructure-property database.

• Weld Process Sensing, Modeling and Control (Materials Reliability Division): Advanced instrumentation and data analysis techniques are used to develop a better understanding of the underlying physics governing the arc welding process.

• High-energy X-ray Diffraction Studies (Materials Reliability Division): Investigations are underway on the use of high-energy x-ray diffraction as an alternate, nondestructive option to the conventional destructive methods for measuring physical properties.

• Tailored Metallic Powders (Metallurgy Division): Measurement techniques for the characterization of microengineered powders are developed to advance our understanding of the relationships among properties, processing, and microstructure.

• Electrodeposition of Aluminum Alloys (Metallurgy Division): Guidelines for the electrodeposition of aluminum-based alloys from low-temperature, low-vapor pressure non-aqueous electrolytes are being developed as an inexpensive method for producing homogeneous and fine-grained aluminum-based thin films for corrosion protection.

• Electrochemical Processing of Nanostructural Materials (Metallurgy Division): Electrochemical methods for the synthesis and characterization of nanoscale magnetoresistive device architectures are being examined with an emphasis on the use of surfactants and segregation phenomena in controlling homo- and hetero-epitaxial film growth.

• Reaction Path Analysis in Multicomponent Systems (Metallurgy Division): Costly experimental investigations of bonding and reaction processes involving interdiffusion at interfaces between metals, oxides, and vapors are supplanted by models, based on thermodynamic data, that predict the formation of transient phases and rates of reaction in complex multicomponent systems.

Metals Processing projects with an especially strong focus on areas which are of special interest to MSEL have evolved to become part of other program areas such as Materials for Microelectronics and Forming of Lightweight Materials. Because processing plays such a basic role in determining the properties and performance of metals, we expect this program to continue providing a foundation for advanced metals technologies.

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Combinatorial Methods

Contact Information: Leonid A. Benderksy

The Combinatorial Methods Program develops new measurement techniques and experimental strategies needed for rapid acquisition and analysis of physical and chemical data of materials by industrial and research communities. A multi-disciplinary team from the NIST Laboratories participates to address key mission-driven objectives in this new field, including needed measurement infrastructure, expanded capability, standards and evaluated data.

Measurement tools and techniques are developed to prepare and characterize materials over a controlled range of physical and chemical properties on a miniaturized scale with a high degree of automation and parallelization. Combinatorial approaches are used to validate measurement methods and predictive models when applied to small sample sizes. All aspects of the combinatorial process, from sample "library" design and library preparation to high-throughput assay and analysis, are integrated through the combinatorial informatics cycle for iterative refinement of measurements. The applicability of combinatorial methods to new materials and research problems is demonstrated to provide scientific credibility for this new R&D paradigm. One anticipated measure of the success of the program would be more efficient output of traditional NIST products of standard reference materials and evaluated data.

Through a set of cross-NIST collaborations in current research areas, we are working to establish the infrastructure that will serve as a basis for a broader effort in combinatorial research. A Combinatorial Methods Working Group (CMWG) actively discusses technical progress within NIST on combinatorial methods through regular meetings. The technical areas and activities of the CMWG are available in a brochure "Combinatorial Methods at NIST" (NISTIR 6730). Within MSEL, novel methods for combinatorial library preparation of polymer coatings have been designed to encompass variations of diverse physical and chemical properties, such as composition, coating thickness, processing temperature, surface texture and patterning. Vast amounts of data are generated in a few hours that promote our understanding of how these variables affect material properties, such as coatings wettability or phase miscibility. Additional focus areas for both organic and inorganic materials include multiphase materials, electronic materials, magnetic materials, biomaterials assay, and materials structure and properties characterization. State of the art on-line data analysis tools, process control methodology, and data archival methods are being developed as part of the program.

In order to promote communication and technology transfer with a wide range of industrial partners, an industry-national laboratories-university combinatorial consortium, the NIST Combinatorial Methods Center (NCMC), is being organized by MSEL. The NCMC will facilitate direct interactions on combinatorial measurement problems of broad industrial interest and efficient transfer of the methods developed to U.S. industry.

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Data Evaluation and Delivery

Contact Information: Ursula R. Kattner

Materials data are critical to the rapid and decentralized design and manufacture of communication, transportation and other devices, which characterize 21st century life. The goal of the Data Evaluation and Delivery Program is to provide the producers and users of materials with the means of fulfilling their data requirements in the most efficient ways. This goal is accomplished by providing improved access to materials data, developing methods for transferring materials data across the World Wide Web, providing protocols for data evaluation, and enhancing the functionality of existing collections of evaluated data. Much of this research is based on information technology and includes: the development of a materials mark-up language (MatML), the linkage of digitized crystallographic information with full structure analysis in cooperation with the International

Center for Diffraction Data and Fachinformationszentrum (FIZ) Germany, and the production of phase diagrams through the NIST/American Ceramics Society Phase Equilibria Program. Other informatics available to the community are contained in the Ceramics WebBook at the Ceramics Division Website. The Ceramics WebBook provides links to other sources of ceramic data and manufacturer's information, selected evaluated data sets, structural ceramics and high temperature superconductor databases, glossaries, and tools for analysis of ceramic materials.

Databases for metals will be developed on web pages in the form of phase diagrams, deformation mechanism maps, and simple - but useful - interactive calculations of thermodynamic and mechanical properties. Annotation and interpretation will be conducted by the Metallurgy Division.

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