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Metallurgy Division Publications - NISTIR 7127

Annual Report cover graphic

Program Overviews


 

Table of Contents


 

Advanced Manufacturing Processes

Contact Information: Carol A. Handwerker

The competitiveness of U.S. manufacturers depends on their ability to create new product concepts and to speed the translation from concept to market while decreasing product cost. This is equally true for well-established “commodity” industries, such as automotive and aerospace, and rapidly growing or emerging industries, such as biotechnology and nanotechnology. For existing products, manufacturing is a critical step in reducing product cycle time. Rapid, low-cost development of manufacturing processes is needed to incorporate new materials into complex product shapes with higher performance at equivalent or lower cost as the competing, established materials and methods. For innovative product concepts, new materials with increasing functionality are needed to translate these concepts to reality.

To realize such improvements in materials and manufacturing, MSEL is developing robust measurement methods, models, standards, and materials and process data needed for design, monitoring, and control of manufacturing processes. A growing challenge is being able to design, monitor, and control such materials and manufacturing processes at size scales from nanometers to meters. The Advanced Manufacturing Processes Program focuses on the following high-impact areas:

  • Combinatorial, high-throughput methods for materialsranging from thin films and nanocomposites tomicro- and macroscale material structures;
  • Industry-targeted R&D centered on uniquemeasurement facilities in forming of lightweightmetals for automotive applications, polymerprocessing, and high-speed machining;
  • Innovative testbeds for emerging materials,including carbon nanotubes and fuel cells;
  • National traceable standards having a major impacton trade, such as hardness standards for metals and process standards for polymers; and
  • Innovative, physics-based process modeling tools.

Our research is often conducted in close collaboration with industrial consortia and standards organizations. These collaborations not only ensure the relevance of our research, but also promote rapid transfer of our research to industry for implementation. Three projects focused on Advanced Manufacturing Processes are highlighted below.

NIST Combinatorial Methods Center (NCMC)

The NCMC develops novel high-throughput measurement techniques and combinatorial experimental strategies specifically geared towards materials research.

These tools enable rapid acquisition and analysis of 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 NCMC lowers barriers to the widespread industrial implementation of this new R&D paradigm. MSEL uses a two-pronged strategy for accelerating the development and implementation of these approaches: an active intramural R&D program that demonstrates the ability of combinatorial methods to produce cutting-edge scientific research and an ambitious outreach activity; key to this effort is the validation of these approaches with respect to traditional “one at a time” experimental strategies.

Forming of Lightweight Metals

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 has major productivity issues related to measurement science and data. Chief among these is the difficulty of designing stamping dies for sheet metal forming. An ATP-sponsored workshop (“The Road Ahead,” June 20–22, 2000) identified production of working die sets as the main obstacle to reducing the time between accepting a new design and actual production of parts. This is also the largest single cost (besides labor) in car production. To benefit from weight savings enabled by new high-strength steels and aluminum alloys, a whole new level of formability measurement methods, models, and data is needed, together with a better understanding of the physics behind metal deformation. MSEL is working with U.S. automakers and their suppliers to fill this need.

Polymer Processing

Polymers have become ubiquitous in the modern economy because of their processability, high functionality, and low cost. 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 our polymer research is on microfluidics and microscale processing, modeling of processing instabilities, and on-line process monitoring of polymers. 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. These measurements are carried out in close collaboration with interested industrial partners.

Contact: Carol A. Handwerker (Metallurgy Division)

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Nanometrology

Contact Information: Gery R. Stafford or John E. Bonevich

The burgeoning field of nanomaterials extends across the full range of traditional material classes, including all forms of metals, polymers, and ceramics. No previous materials technology has shown so prodigiously a potential for concurrent advances in research and industry as does the field of nanomaterials in mechanical devices, electronic, magnetic, and optical components, quantum computing, tissue engineering and other biotechnologies, and as-yet unanticipated exploitations of as-yet undiscovered novel properties of nanoscale assemblies of particles. Already, there is growing excitement surrounding the ability of some molecules or particles to self-assemble at the nanoscale to form new materials with unusual properties. Nanometrology, i.e., the ability to conduct measurements at these dimensions, to characterize the materials, and to elucidate the structure and nature of these new and novel assemblies, is a requisite and fundamental cornerstone that must be established securely if this technology is to flourish.

NIST is uniquely positioned to lead the development of the measurement methods, instrumentation, standards, and reference materials that, together, will form the metrological infrastructure essential to the success of nanotechnology.

The MSEL Nanometrology Program incorporates basic measurement metrologies to determine material properties, process monitoring at the nanoscale, nanomanufacturing and fabrication techniques, and structural characterization and analysis techniques such as advanced imaging and multiscale modeling. The Program comprises 22 projects in the Ceramics, Materials Reliability, Metallurgy, and Polymers Divisions, and includes structural characterization using neutron scattering at the NIST Center for Neutron Research (NCNR). The projects cover a wide range of measurement and characterization methods grouped into the areas of mechanical property measurement, chemical and structural characterization and imaging, fabrication and monitoring of nanoprocesses and events, and modeling of nanoscale properties. In each area, we work to advance basic measurement capabilities and lead the intercomparison, standardization, and calibration of test methods. The newly completed Advanced Measurement Laboratory at the NIST Gaithersburg site provides an incomparable environment for accurate nanoscale metrology.

In the area of mechanical property measurement, we are developing and standardizing techniques for determining nanoscale elastic properties (elastic moduli, Poison’s ratio, and internal stress), plastic deformation, density, adhesion, friction, stiction, and tribological behavior. Work in nanoindentation, used extensively in determining mechanical properties of thin films and nanostructures, focuses on developing traceable calibration methodologies and standard test methods. We also use atomic force acoustic microscopy, surface acoustic wave spectroscopy, and Brillouin light scattering to measure the mechanical properties of thin films. In addition, we are developing micro- and nano-scale structures and test methods to measure strength and fracture behavior of interfaces and materials having very small volumes.

The chemical and structural characterization and imaging utilize neutron and x-ray beam lines at three facilities: the NCNR; the National Synchrotron Light Source at Brookhaven National Laboratory; and the Advanced Photon Source at Argonne National Laboratory. Innovative scattering and spectroscopy methods are advancing our ability to obtain a wide range of chemical and structural information at the nanoscale, including chemical bond identification and orientation, polyelectrolyte dynamics, and equilibrium structures. In collaboration with three other NIST laboratories, we are developing electron microscopy and spectroscopy instrumentation for quantitative, 3D chemical imaging at the nanoscale. Other characterization projects include work on gradient reference specimens for the calibration of advanced scanning probe microscopy, and the application of carbon nanotubes as physical probes of cell membranes.

Efforts in the fabrication and monitoring of nanoscale processes and events include the study of electrochemical and microfluidic methods for fabricating nanostructures, novel approaches to nanocalorimetry for the study of interfacial reactions, in situ observations of nanoparticle and nanotube dispersion and alignment, and advanced instrumentation for nanotribology experiments.

Finally, we have extensive efforts in the theory, modeling, and prediction of material properties and behavior extending from nanoscale to macroscale dimensions. Modeling efforts include large-scale finite element methods, multiscale Green’s function methods, classical atomistic simulations, first principles, and quantum mechanical calculations using density functional theory. Often, several modeling methods must be combined into one study to accurately describe the material behavior; thus, we pay great attention to the correct interfacing between models operating at different length scales, to ensure that our models properly capture the physics of both components and total systems.

Contact: Gery R. Stafford or John E. Bonevich (Metallurgy Division)

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Biomaterials

Contact Information: Eric J. Amis (Polymers Division) or Lyle E. Levine

New materials and devices are radically changing the treatment of injury and disease, yet it is clear that within this rapidly evolving segment of the materials industry, a basic measurement infrastructure does not exist. The Biomaterials Program develops measurement methods, standards, and fundamental scientific understanding at the interface between the materials and biological sciences. For the health care industry, we focus on dental and medical sectors that apply synthetic materials for replacement, restoration, and regeneration of damaged or diseased tissue. Three primary foci exist within this program: biocompatibility, biomaterials characterization, and materials measurements applied to biological systems.

Whether the medical issue involves implanting a hip- or knee-joint prosthesis, a synthetic bone graft, or a tissue engineering scaffold into the human body, one primary issue is biocompatibility. Using our expertise in materials science, we have developed suitable Reference Materials (RM) for investigating biocompatibility and implant suitability. Research has focused on measuring cellular response to powders and bulk materials that are candidates for implants; recently, we produced a realistic wear particle Standard Reference Material (SRM® 2880) for bioactivity testing.

Work on quantitative methods of biomaterials characterization includes assays for adhesion, viability, proliferation, and differentiation of bone cells, 3-dimensional structural/functional imaging of tissue in-growth, and biochemical assays to quantify inflammatory responses to synthetic materials. The focus of this effort is bridging the gap between fundamental knowledge and the product development needs in industry. For example, in collaboration with the Chemical Science and Technology Laboratory, we are developing measurement methodologies and reference materials to assess interactions in complex systems of living cells with synthetic materials. The expected outcome of this work includes reference substrates that induce specific cellular responses, and engineered DNA vectors to act as fluorescent reporters of cellular responses.

Another example of our effort to bridge this gap is our collaboration with the dental industry, which is primarily composed of small manufacturers with limited R&D capability. Collaborations with the American Dental Association Foundation (ADAF) develop improved materials and materials measurements techniques, patent and license these inventions, and, most importantly, provide a technical foundation. Research focuses on improved understanding of the synergistic interaction of the phases of polymer-based composites and the mechanisms of adhesion to dentin and enamel. This approach will ultimately lead to materials with improved durability, toughness, and adhesion to contiguous tooth structure. We also collaborate with the ADAF to develop metrology for the biocompatibility of synthetic bone grafts.

biomaterials

In this era of interdisciplinary research, we provide an added dimension. By taking a physical/mechanical approach to how cells function, respond, and remodel in interaction with synthetic materials, we provide skill sets typically absent in the biomedical community. Mechanical properties issues also arise when considering synthetic bone grafts and tissue engineering scaffolds. Complementing traditional bulk mechanical property measurements, combinatorial approaches are being developed to identify compositions and surface features that affect properties such as biocompatibility and mechanical durability.

Our mechanical property metrology extends further to biological systems that span the range from individual neurons and muscle cells to complete pulmonary arteries. This necessitates the development of unique mechanical testing platforms and application of a materials science approach to understanding integrated properties. Recently, we have developed a bioreactor capable of applying biaxial stresses and allowing monitoring of the stress and strain of a two-dimensional scaffold sheet during tissue growth.

Fundamental to the Biomaterials program is recognition of the need for an integrated systems approach. Collaborations among and between project teams are critical to progress against the ambitious goals of this program.

Contact: Eric J. Amis (Polymers Division), Lyle E. Levine (Metallurgy Division)

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Materials for Electronics

Contact Information: Martin L. Green (Ceramics Division), Eric K. Lin (Polymers Division), Daniel Josell

The U.S. electronics industry faces strong international competition in the manufacture of smaller, faster, more functional, and more reliable products. Many critical challenges facing the industry require the continual development of advanced materials and processes. The NIST Materials Science and Engineering Laboratory (MSEL) works closely with

U.S. industry covering a broad spectrum of sectorsincluding semiconductor manufacturing, device components, packaging, data storage, and assembly, as well as complementary and emerging areas such as optoelectronics and organic electronics. MSEL has a multidivisional approach, committed to addressing the most critical materials measurement and standards issues for electronic materials. Our vision is to be the key resource within the Federal Government for materials metrology development and will be realized through the following objectives:

  • Develop and deliver standard measurements and data;
  • Develop advanced measurement methods needed byindustry to address new problems that arise with thedevelopment of new materials;
  • Develop and apply in situ as well as real-time, factoryfloor measurements, for materials and devices havingmicrometer- to nanometer-scale dimensions;
  • Develop combinatorial material methodologies forthe rapid optimization of industrially importantelectronic materials;
  • Provide the fundamental understanding of thedivergence of thin film and nanoscale materialproperties from their bulk values;
  • Provide the fundamental understanding of materialsneeded for future nanoelectronic devices, includingfirst principles modeling of such materials.

The NIST/MSEL program consists of projects led by the Metallurgy, Polymers, Materials Reliability, and Ceramics Divisions. These projects are conducted in collaboration with partners from industrial consortia (e.g., International SEMATECH), individual companies, academia, and other government agencies. The program is strongly coupled with other microelectronics programs within the government such as the National Semiconductor Metrology Program (NSMP). Materials metrology needs are also identified through the International Technology Roadmap for Semiconductors (ITRS), the IPC Lead-free Solder Roadmap, the National Electronics Manufacturing Initiative (NEMI) Roadmap, the Optoelectronics Industry Development Association (OIDA) Roadmap, IPC (the International Packaging Consortium), and the National [Magnetic Data] Storage Industry Consortium (NSIC) Roadmap.

In each of these areas, MSEL researchers have made substantial contributions to the most pressing technical challenges facing industry, from new fabrication methods and advanced materials in the semiconductor industry, to advanced packaging materials, to magnetic data storage. Below are just a few examples of MSEL contributionsover the past year.

Advanced Gate Dielectrics

To enable further device scaling, the capacitive equivalent thickness (CET) of the gate stack thickness must be 0.5 nm to 1.0 nm. This is not achievable with existing SiO2/polcrystalline Si gate stacks. Given the large number of possible choices for these new layers, the only feasible approach to understanding the complex materials interactions that result at the gate dielectric/ substrate and gate dielectric/metal gate electrode interfaces is through the application of combinatorial methodologies. This same methodology and apparatus are applicable to a wide variety of problems in the electronic materials field.

Sub-100 nm Nanofabrication

The continual decrease in feature size has been the driving force for advances in the semiconductor industry. Current structures have 90 nm dimensions with plannednodes at 65 nm and 35 nm structures. Advanced measurements of the patterning materials (photoresists),are needed to enable future large scale manufacturing ofsmaller devices. MSEL utilizes advanced x-ray andneutron tools to provide insight into the feasibilityand optimization of these important processes.

Advanced Metallization

Electrodeposited copper is rapidly replacing aluminumfor on-chip “wiring” because of its lower electricalresistivity, superior electromigration behavior, and the ability to fill fine features without the formation of seamsor voids. As feature dimensions go below 100 nm,difficulties in maintaining performance are anticipated.These issues are addressed through a combination ofmodeling and experimental efforts.

Test Methods for Embedded Passive Devices

Significant advantages arise if passive devices areintegrated directly into the circuit board as embeddedpassive devices rather than discretely attached withautomated assembly. New metrology methods weredeveloped to address the needs of the electronic industry. Two test methods were completed and have receivedwide acceptance by industry as new methods to acceleratethe development of embedded passive device technology.

Contact: Martin L. Green (Ceramics Division), Eric K. Lin (Polymers Division), Daniel Josell (Metallurgy Division)

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Safety and Reliability

Contact Information: Frank W. Gayle

While various structural failures have captured national attention over the years, the events of September 11, 2001 generated a greatly increased awareness of vulnerabilities in our national infrastructure. The extent of these vulnerabilities depends to a large degree on the performance of materials in situations outside of the original design considerations. It is now recognized that a critical and urgent national need exists to establish the behavior of materials under such extreme loadings, and to disseminate guidance and tools to assess and reduce future vulnerabilities.

The goal of providing a technical basis for cost-effective changes to national practices and standards, coupled with a need for an integrated effort drawing on capabilities and expertise of a broad collaborative team, has lead to the development of the Safety and Reliability Program within MSEL. This program draws on the expertise of several divisions in MSEL and across NIST.

Project selection is guided by an identification and assessment of the particular vulnerabilities within our materials-based infrastructure, and focusing on those issues which would benefit strongly by improved measurements, standards, and materials data. Ultimately, we intend to moderate the effects of acts of terrorism, natural disasters, or other emergencies, all through improved use of materials.

Our vision is to be the key resource within the Federal Government for materials metrology development as realized through the following objectives:

  • Identify and address vulnerabilities and needed improvements in U.S. infrastructure;
  • Develop and deliver standard measurements and data;
  • Develop advanced measurement methods needed by industry to address new problems that arise with the development of new materials;
  • Support other agency needs for materials expertise.

This program responds both to customer requests (primarily other government agencies) and to the Department of Commerce 2005 Strategic Goal of “providing the information and framework to enable the economy to operate efficiently and equitably.” For example, engineering design can produce safe and reliable structures only when the property data for the materials is available and accurate. Equally important, manufacturers and their suppliers need to agree on how material properties should be measured.

The Safety and Reliability Program works toward solutions to measurement problems on scales ranging from the macro to the micro, in three of the Laboratory’s Divisions (Materials Reliability, Metallurgy, and Polymers). The scope of activities includes the development and innovative use of state-of-the-art measurement systems; leadership in the development of standardized test procedures and traceability protocols; development of an understanding of materials in novel conditions; and development and certification of Standard Reference Materials (SRMs). Many of the tests involve extreme conditions, such as high rates of loading, high temperatures, or unusual environments (e.g., deep underwater). These extreme conditions often produce physical and mechanical properties that differ significantly from the handbook values for their bulk properties under traditional conditions. These objectives will be realized through innovative materials, property measurement and modeling.

safety fig

The MSEL Safety and Reliability Program is also contributing to the development of test method standards through committee leadership roles in standards development organizations such as the ASTM International and the International Standards Organization (ISO). In many cases, industry also depends on measurements that can be traced to NIST Standard Reference Materials (SRM®).

In addition to the activities above, all three 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 on metallurgical issues involving pipelines and dams, advising the Department of the Interior on the structural integrity of the U.S.S. Arizona Memorial, and collaborating with both the Department of Transportation and the Department of Energy on pipeline safety issues.

Contact: Frank W. Gayle (Metallurgy Division)

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