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
www.nist.gov/combi.
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
www.nist.gov/combi.
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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