On the Cover: 

From the front cover and continuing on to the back, the images shown are, 

respectively: 

Fig 1 - 3-D model of binary eutectic systems under various solidification 

conditions. (Dan Lewis) 

Fig 2 - Color representation of one normal mode of magnetization vibration 

calculated for a 50 nm thick film of Permalloy with 20 nm defects. 

Fig 3 - Magneto-optical image of domain patterns in a new “synthetic 

antiferromagnet” Co/Ru/Co trilayer showing two different types of 

domains separated by novel non-180 degree walls. Similar trilayers 

are used in high density recording media. 

Fig 4 - Combinatorial pattern of Au/Ni metallization on gallium nitride. 
National Institute of 

Standards and Technology 

Arden L. Bement, Jr. 

Director 

Technology 

Administration 

Phillip J. Bond 

Undersecretary of 

Commerce for Technology 

U.S. Department 

of Commerce 

Donald L. Evans Materials Science and Secretary Engineering Laboratory 

FY 2002 Programs and

Accomplishments 

Metallurgy

Division 

Carol A. Handwerker, Chief 

Frank W. Gayle, Deputy 

NISTIR 6907 

September 2002 
Certain commercial entities, equipment, or materials may be identified in this document 

in order to describe an experimental procedure or concept adequately. Such identification 

is not intended to imply recommendation or endorsement by the National Institute of 

Standards and Technology, nor is it intended to imply that the entities, materials, or 

equipment are necessarily the best available for the purpose. 
Table of Contents


Table of Contents


Executive Summary ......................................................................................................... 1


Technical Highlights ......................................................................................................... 5


Magnetization Dynamics in Films with Nanometer Scale Microstructure ........................ 6


Ballistic Magnetoresistance:


A New Phenomenon with Great Potential for Magnetic Sensors ................................... 8


Advanced Metallizations for Sub-100 Nanometer Electronics ..................................... 10


Performance-Limiting Defects in GaN ...................................................................... 12


Responding to the Auto Industry’s Research Needs in Materials:


Forming of Lightweight Materials .............................................................................. 14


Thermodynamic Database for Multicomponent Alloys ................................................ 16


Advanced Manufacturing Methods .................................................................................. 18


Modeling Solidification and Microstructure Evolution .................................................. 19


High Speed Machining ............................................................................................. 20


Metal Powder Processing ......................................................................................... 21


Electrochemical Processing of Nanoscale Materials .................................................... 22


Instrumented Consolidation of Amorphous Powders .................................................. 23


Combinatorial Methods .................................................................................................. 24


Combinatorial Materials Research:


Interconnects to Optoelectronic Materials .................................................................. 25


Combinatorial Methods for Thin Films ...................................................................... 26


Data Evaluation and Delivery ......................................................................................... 27


Reaction Path Analysis in Multicomponent Systems .................................................... 28


Thermodynamic Databases for Industrial Processes .................................................. 29


Mechanical Properties of Metals and Alloys on the Internet ........................................ 30


Electrodeposited Coating Thickness Standards ......................................................... 31


iii 
Table of Contents


Forming of Lightweight Material for Automotive Applications ............................................ 32


Plasticity, Fabrication Processes, and Performance ..................................................... 33


Standard Test Method Development for Sheet Metal Formability ............................... 34


Microstructural Origins of Surface Roughening and Strain Localizations ...................... 35


Underlying Processes of Plastic Deformation ............................................................. 36


Anelasticity and Springback Predictability .................................................................. 37


Materials for Micro- and Optoelectronics ........................................................................ 38


Mechanism of Sn Whisker Growth from Electrodeposits ............................................ 39


Superconformal Film Growth: Measurements and Modeling ..................................... 40


Solder and Solderability Measurements for Microelectronics ...................................... 41


Magnetic Properties and Standard Reference Materials ............................................. 42


Magnetic Properties of Nanostructured Materials ...................................................... 43


Nanomagnetodynamics ............................................................................................ 44


New Materials for Ultra-High Density Data Storage .................................................. 45


Materials Property Measurements .................................................................................. 46


Hardness Standardization: Rockwell, Vickers, Knoop ............................................... 47


Deformation Mechanisms and Constitutive Laws in Thin Film Superlattices ................ 48


Analysis of Structural Steel in the World Trade Center Investigation ............................ 49


Materials Structure Characterization ............................................................................... 50


Nanoscale Characterization: Electron Microscopy ..................................................... 51


Metallurgy Division FY02 Annual Report Publication List ................................................. 53


Metallurgy Division ........................................................................................................ 63


Research Staff .............................................................................................................. 64


Organizational Charts .................................................................................................... 67


iv 
Executive Summary


Executive Summary 

This report describes the major technical activities, 

accomplishments, and areas of scientific expertise in 

the Metallurgy Division of the NIST Materials Science 

and Engineering Laboratory in FY2002 (October 2001 

through September 2002). In this report, we have tried 

to provide insight into how our research programs meet 

the needs of our customers, how the capabilities of the 

Metallurgy Division are being used to solve problems 

important to the national economy and the materials 

metrology infrastructure, and how we interact with our 

customers to establish new priorities and programs. 

We welcome feedback and suggestions on how we can 

better serve the needs of our customers and encourage 

increasing collaboration to this end. 

Mission 

Our mission is to provide critical leadership in the 

development of measurement methods and standards, 

as well as fundamental understanding of materials 

behavior needed by U.S. materials users and producers 

to become or remain competitive in the changing global 

marketplace. As an essential part of this mission, we are 

responsible not only for developing new measurement 

methods with broad applicability across materials classes 

and industries, but also for working with individual 

industry groups to develop and integrate measurements, 

standards, software tools, and evaluated data for 

specific, technologically important applications. 

Establishing Priorities 

As part of the development of our technical program, 

we examine a wide range of research opportunities and 

make choices for our research portfolio based on several 

criteria: the match to the NIST mission, the magnitude 

and immediacy of industrial need, the degree to which 

NIST’s contribution is critical for success, the anticipated 

impact relative to our investment, our ability to respond 

in a timely fashion with high-quality output, and the 

opportunity to advance mission science. This requires 

that we establish our research priorities through 

extensive consultation and collaboration with our 

customers in U.S. industry and with our counterparts 

in the international metrology community, using a 

variety of methods including industrial roadmapping 

activities, workshops, technical meetings, standards 

committee participation, and individual consultation 

with our customers. 

Within the context of industrial relevance and 

potential impact of our research, technology trends 

strongly influence the technical directions addressed by 

NIST. We prefer to work in rapidly evolving technologies, 

where advances in measurement science are needed 

to understand the limitations on system behavior and, 

therefore, where our contributions are likely to have 

an impact on the course of technology. For NIST as a 

whole and the Metallurgy Division in particular, we are 

committed to having an impact on the measurement and 

standards infrastructure for the NIST strategic Focus 

Areas: nanotechnology, health care, homeland security, 

and information technology/knowledge management. 

Nanotechnology and information technology/knowledge 

management are not industry sectors themselves, but 

are technologies that will have an impact on virtually 

all present and future industrial enterprises. We have 

major projects in nanotechnology and homeland security 

in 2002; additional Division projects will begin in 

nanotechnology and health care in 2003 and in 

nanotechnology and information technology/knowledge 

management in 2004. 

Research Portfolio 

Our 2002 research portfolio focuses on fulfilling 

specific measurement needs of the industrial sectors: 

the magnetic data storage, microelectronics packaging, 

automotive, aerospace, and optoelectronics industries, 

and on establishing national traceable hardness 

standards needed for international trade. Our output 

consists of a variety of forms, from a fundamental 

understanding of materials behavior to measurement 

techniques conveyed through the scientific literature 

and oral presentations, standard reference materials, 

evaluated data and online databases, software tools, 

and sensors for on-line process control. 

■ Magnetic Data Storage: In 2001 we started two 

new major projects within this program. As part of the 

National Nanotechnology Initiative, a major collaboration 

among MSEL, the Information Technology Laboratory 

(ITL), and the Electronics and Electrical Engineering 

Laboratory (EEEL) is developing new measurement 

methods and models for magnetic damping, needed by 

the magnetic recording industry in the next 3–5 years 

to improve switching speed. Significant progress has 

been made in 2002 in modeling and measuring 

fundamental damping mechanisms through 

ferromagnetic resonance measurements. In 2002, 

our long-term project on GMR thin films was 

refocused into Spintronics, the use of spin-polarized 

electrons for new devices and magnetic imaging. 

Through an extensive network of university and 

industrial collaborators, we are using the process 

measurement and control capabilities of the MSEL 

Magnetic Engineering Research Facility to develop 

an understanding of the materials structure and 

processing issues in the creation and transfer of 

spin-polarized electrons. 

■ Microelectronics Packaging: In the MSEL Program 

on Materials for Microelectronics, we are providing 

1 
Executive Summary


tools for producing improved metal interconnects, 

from copper on-chip interconnects at the nanometer 

scale to lead-free solder joints on printed wiring 

boards. Our project on measurements and modeling 

of electrodeposited copper for nanometer scale chip 

interconnection technology continues to produce 

significant value to the microelectronics community. 

In the three years since beginning the project, we 

have developed a measurement technique, a theory for 

control of interface dynamics, and modeling software 

for predicting quantitatively the ability of complex 

electrolytes to fill vias and trenches for on-chip 

interconnects, and have transferred all of these to 

the appropriate industrial customers. During the last 

year, we have demonstrated, in collaboration with 

International Sematech and Motorola, the generality 

and versatility of the NIST theory for electrodeposited 

metals other than copper, and for chemical vapor 

deposition. In the area of electronics assembly, we 

continue to play a major role in the NEMI Lead-Free 

Solder Task Force, with the goal of preparing the U.S. 

microelectronics industry to assemble products with 

lead-free solders as required for international trade. 

In FY2002, the NEMI Lead-free Task Force and 

NIST have worked together to respond to the needs 

for critically evaluated data for modeling the reliability 

of lead-free solder alloys. 

■ Automotive: Within the expanding program on the 

Forming of Lightweight Materials, we are developing 

standard test methods for sheet metal forming, 

measurements of surface roughness, and physically 

based constitutive laws — and measurement tools 

needed to reveal them. In FY2002, we have made 

a major breakthrough in bridging the length scale 

between dislocation level modeling and macroscopic 

deformation. This statistical physics approach to 

propagation of dislocations through dislocation cell 

walls, and the local accumulation of deformation till slip 

bands form provides the underpinning for developing 

physically-based constitutive laws as a function of alloy 

composition. All of our projects in the Forming of 

Lightweight Materials Program are done in close 

collaboration with the automotive industry through 

formal partnerships, such as USCAR and the Freedom 

Car, and are designed to help accelerate the design of 

forming operations for lightweight materials such as 

aluminum that will ultimately improve fuel economy. 

■ Aerospace and Power Generation: Within the 

Metals Processing Program, we continue to help U.S. 

aerospace and power generation industries improve 

responsiveness and competitiveness by accelerating the 

design of manufacturing processes for turbine engines. 

Our development of composition-dependent diffusion 

mobility databases for superalloy systems provides an 

efficient method to store a wealth of diffusion 

data and the means to extrapolate the available 

data to higher order systems of importance to these 

industries. NIST collaborates on a DARPA project 

with General Electric and Howmet Corporation using 

this approach to accelerate process development for 

the Ni-Al-Cr-Co-Fe-Hf-Mo-Nb-Re-Ta-Ti-W system. 

■ Optoelectronics: As a result of a growing 

collaboration between EEEL and MSEL, a Program 

on Wide Band Gap Semiconductors was established at 

the end of FY2001 and continued through FY2002. 

Building on the existing projects on metal interconnects 

for GaN (Metallurgy Division) and on interface and 

bulk defects in GaN (Ceramics Division), the EEELMSEL program is developing a comprehensive suite 

of measurement methods for characterizing interface 

and bulk defects limiting the application of GaN and 

related materials. 

■ National Hardness Standards: In addition to 

industry-specific goals, national and international 

standardization activities are a continuing responsibility. 

As part of our core NIST mission, we provide national 

and international leadership in the standardization of 

Rockwell hardness, the primary test measurement used 

to determine and specify the mechanical properties of 

metal products. Our responsibility requires us not only 

to develop the U.S. national standards with traceability 

from NIST through NVLAP to secondary standards 

labs and U.S. metals producers and users, but also to 

provide leadership to ASTM Standards Committees, 

the U.S. delegation to ISO, BIPM, and OIML. 

Division Structure and Expertise 

The Division is composed of 39 scientists, 

supported by 6 technicians, 6 administrative staff 

members, and more than 80 guest scientists, and 

organized into five groups that represent the 

Division’s core expertise in Metallurgical Processing, 

Electrochemical Processing, Magnetic Materials, 

Materials Structure and Characterization, and Materials 

Performance. However, by virtue of the interdisciplinary 

nature of materials problems in the industrial and 

metrology sectors that we serve, program teams are 

assembled across group, division and laboratory 

boundaries to best meet our project goals. We are 

committed to assembling the expertise and resources 

to fulfill our technical goals with the speed and quality 

necessary to have the desired impact. 

Recognition for Division Staff 

We are proud of the accomplishments of the 

Metallurgy Division staff in delivering the measurements, 

standards, data, and modeling tools needed by our 

customers. In FY2002, Division members were 

2 
Executive Summary


recognized for the impact and quality of their work 

by a wide range of organizations, including internally 

at NIST. 

■ John Cahn was awarded the 2002 Bower Prize 

for Achievement in Science for “his unprecedented 

contributions to the understanding of thermodynamics 

and kinetics of phase transformations in materials.” 

The award consists of a gold medal and $250,000. 

■ Daniel Josell, Tom Moffat, and Gery Stafford were 

awarded the Department of Commerce Gold Medal, 

the highest honor conferred by the Department, for 

their pioneering achievements in developing measurement 

and modeling techniques for controlling copper 

metallization processes for use in on-chip interconnects. 

Within two years, they provided the measurement and 

modeling tools necessary to extend the technology 

to below 60 nm line width, smaller than the target 

line width for 2008 according to the 1999 SIA 

International Technology Roadmap for Semiconductors. 

■ Ursula Kattner was awarded the NIST Bronze Medal 

and the ASM George Kimball Burgess Memorial Award 

for her outstanding achievement in thermodynamics and 

the application of phase diagrams to important industrial 

metallurgical processes. 

■ Bill Boettinger became a NIST Fellow, the highest 

scientific and technical position at NIST. 

■ Tom Moffat was awarded the William Blum Award from 

the National Capital Section of the Electrochemical 

Society for his research on electrodeposition at the 

nanoscale and his application of this research to 

on-chip interconnection. 

■ Bob Shull was elected as a Senior Member of IEEE. 

■ Ursula Kattner and Albert Davydov were awarded the 

2002 Alloy Phase Diagram International Committee 

(APDIC) Best Paper award for the best critical review 

of phase diagram data published in the three years 

preceding the award. 

■ Steve Banovic was given the Society of Automotive 

Engineers Best Paper Award for Wrought Aluminum 

Alloys for his paper on the effect of microstructural 

variables on surface roughening in aluminum alloys. 

■ Chris Johnson was given the International 

Microelectronics and Packaging Society (IMAPS) 

Best Paper Award with George Harman of ITL for 

their paper on “Wire Bonding to Advanced CopperLow-K Integrated Circuit, the Metal/Dielectric 

Stacks, and Materials Considerations.” 

■ Jonathan Guyer was awarded the Best Poster Award 

from the Materials Research Society, 2002 Spring 

Meeting for his poster on stress-induced instabilities 

in thin films. 

■ Carol Handwerker was awarded the SolderTek 

Award for Lead-Free Solders in recognition of her 

contributions to lead-free soldering technology in the 

NCMS Lead-Free Solder Project and in the current 

NEMI Lead-Free Assembly Project. 

Carol A. Handwerker 

Chief, Metallurgy Division 

3 

Technical Highlights


Technical Highlights 

The following Technical Highlights section includes 

expanded descriptions of research projects that have 

broad applicability and impact. These projects generally 

continue for several years. The results are the product 

of the efforts of several individuals. The Technical 

Highlights include: 

■ Magnetization Dynamics in Films with Nanometer 

Scale Microstructure 

■ Ballistic Magnetoresistance: A New Phenomenon 

with Great Potential for Magnetic Sensors 

■ Advanced Metallizations for Sub-100 Nanometer 

Electronics 

■ Performance-Limiting Defects in GaN 

■ Responding to the Auto Industry’s Research Needs 

in Materials: Forming of Lightweight Materials 

■ Thermodynamic Databases for Multicomponent Alloys 

5 
Technical Highlights


Magnetization Dynamics in Films with Nanometer Scale Microstructure


Magnetization damping is essential for data storage 

and retrieval at GHz data rates in disk drives, MRAM 

chips and other magnetoelectronic devices. In disk 

drives, the write head materials, media and read head 

must all be able to perform well on nanosecond time 

scales. For measurement of magnetic damping 

parameters, ferromagnetic resonance (FMR) is the 

dominant technique, but the raw linewidth data is 

often clouded by the presence of inhomogeneities. 

Our modeling of ferromagnetic resonance spectra in 

inhomogeneous thin films takes a novel approach to a 

problem that for several decades has been solved only 

for weak inhomogeneities. Our new model involves 

solving for the normal modes of an inhomogeneous film 

and calculating the absorption spectrum from all of the 

modes. This model provides the theoretical basis for 

studying the intrinsic damping processes through FMR 

linewidth measurements, and ultimately for delivering 

the needed data on magnetic damping to industry. 

Magnetic data storage has become the most 

prevalent form of data storage in the world, far 

surpassing paper documents in worldwide capacity. 

Annual hard drive storage capacity shipped is 

approximately 1 × 1019 bytes with a 60% per year 

growth rate. To handle anticipated storage at GHz 

data rates, it is important to understand and control 

magnetization damping, the process that allows 

magnetization to come to equilibrium by dissipating heat. 

To develop high-data-rate hard drives, it will be important 

to understand and control damping in the magnetic 

materials used in write heads, media and in read heads. 

For magnetic random access memory (MRAM) chips, 

damping is a limiting factor for the speed of these chips 

because reliable switching of the magnetic “bit” requires 

waiting for the magnetization to come to equilibrium 

before the next switching event. 

The Nanomagnetodynamics Project is a cooperative 

project between the Metallurgy Division in MSEL and 

the Magnetic Technology Division in EEEL. The work 

is designed to address magnetization dynamics, and 

magnetization damping in particular, and to deliver to 

industry the data and metrology needed to develop 

high-data-rate magnetic devices. This highlight describes 

a recent theoretical breakthrough by MSEL staff that 

will enable reliable magnetization damping metrology. 

The primary measurement used to determine the damping 

properties of magnetic materials is ferromagnetic resonance 

(FMR) linewidth. Ferromagnetic resonance, like electron 

spin resonance (ESR) and nuclear magnetic resonance 

(NMR) involves precession of the magnetization around 

an equilibrium direction at a frequency that depends on 

the applied field. The damping rate is determined from 

6 

the width of the susceptibility peak corresponding to 

the magnetization precession frequency as illustrated in 

Figure 1. 

Figure 1. a) Magnetization precession. Damping causes 

the magnetization to come to equilibrium as shown by the 

red spiral. b) A typical FMR signal, taken at 2.5 GHz in a 

10 nm thick film of Permalloy. Damping is measured through 

the line width ∆H. 

Measurements of damping in ferromagnetic materials 

are complicated by the fact that in addition to damping, 

inhomogeneity contributes to the FMR linewidth. 

Reliable interpretation of FMR linewidth data therefore 

requires separation of the linewidth into components 

arising from damping and inhomogeneity. 

Unlike ESR and NMR in paramagnetic materials, the 

spins in ferromagnetic materials are strongly coupled by 

short-range exchange interactions and long range dipolar 

interactions. To account for magnetic interactions, it is 

convenient to describe the vibrations of the magnetization 

in terms of spin waves, or in quantum mechanical language, 

“magnons.” Spin waves (magnons) are the collective 

vibrational normal modes of the magnetization in a uniform 

film just as sound waves (phonons) are the collective normal 

modes of a uniform crystal lattice. The analogy with sound 

waves is useful in describing the interaction of spin waves 

with defects. If a sound wave encounters a defect where 

the elastic properties are different, a portion of the incoming 

sound energy will be scattered into sound waves traveling 

in different directions, but with the same frequency. For 

spin waves, the uniform precession that is driven by a 

microwave field in an FMR experiment can be scattered 

into short-wavelength spin waves with the same precession 

frequency as the uniform mode. The quantum mechanical 

Hamiltonian describing a system with defects can be written 

† † * † H = h∑ωk ak ak + h∑(Ak,k'

ak ak' + Ak,k'ak ak')

k k

where αk

† and αk are the magnon (or phonon) creation 

operators for waves at frequency ωk and Ak,k is a 

coefficient describing the strength of the defect that 

produces scattering. 
Technical Highlights


The “two-magnon” model was first derived in the 

1950’s to describe the effects of defects on linewidth 

measurements in bulk ferrite materials. Until the 

present work, it was the most sophisticated model of 

inhomogeneities in FMR. 

The physical picture presented by the two magnon 

model is that inhomogeneities cause energy to be 

transferred from the k = 0 uniform precession mode to 

other k ≠ 0 spin wave modes having the same frequency. 

The two-magnon model is expected to be valid when the 

spin wave amplitudes are small compared to the uniform 

precession amplitude, so scattering from spin wave 

modes back to the uniform precession mode is weak 

and spin wave–spin wave interactions are not important. 

Our approach to the problem of ferromagnetic 

resonance in inhomogeneous thin films treats the very 

common case where the Ak,k coefficients are too large 

for the two-magnon model to be valid. To do this, we 

start with the Hamiltonian for films with inhomogeneities 

given above and find the eigenmodes and eigenvalues 

directly. This process involves constructing a model 

microstructure of the film, calculating the Ak,k ́ 

coefficients, limiting the Hamiltonian to approximately 

1000 spin wave modes and computationally diagonalizing 

the Hamiltonian matrix having elements Ak,k + ωkδk,k ́. 

The resulting eigenmodes of the inhomogeneous film 

are mixtures of the spin waves and the uniform, k = 0

precession mode. Each eigenmode has a finite coupling 

to a uniform driving field that depends on the amount of 

the k = 0 mode that it contains. Figure 2 shows the 

eigenmode spectrum and an eigenmode for a typical 

calculation. 

Figure 2: Eigenmode spectrum of an inhomogeneous 

thin film. Each eigenmode couples directly to the uniform 

FMR driving field to give the simulated FMR spectrum 

shown. The background image is the magnetization pattern 

corresponding to one of the eigenmodes. The image width 

is 5 mm and the defect size is 20 nm. 

The physical picture presented by this model is 

very different from that of the two-magnon model. 

Inhomogeneities do not merely couple the spin wave 

modes, they cause mixing of the spin wave modes into 

a new set of eigenmodes, each of which is observable 

in an FMR experiment. In this picture, it is clear that the 

linewidth caused by inhomogeneities is due to a spreading 

of the FMR intensity in frequency, not to any additional 

damping process. 

Figure 3 shows a comparison between our 

eigenmode calculation, the two-magnon model and 

experimental linewidth measurements for a 20 nm film of 

Permalloy deposited on polycrystalline NiO. The coupling 

to antiferromagnetic NiO produces an inhomogeneous 

“exchange bias” field and a uniaxial anisotropy field 

that varies in strength and direction from grain to grain. 

These intentionally created “defects” are turned off by 

deposition of a thin layer of Ta on the NiO, decoupling it 

from the Permalloy. 

Figure 3: Comparison of the two-magnon model and the 

eigenmode model of FMR line width with Permalloy films: 

one made inhomogeneous by NiO and a control sample. 

The development of this new model of FMR in 

inhomogeneous films is important in several respects. 

■ It gives a clear physical picture of the magnetization 

dynamics in inhomogeneous thin films. 

■ It clarifies that the linewidth due to inhomogeneities 

does not constitute a different kind of damping. 

■ It provides the theoretical basis for interpreting FMR 

linewidth that will allow us to study the intrinsic 

damping processes and, ultimately, to deliver the 

necessary data to industry. 

For More Information on this Topic 

For further information on magnetization dynamics, 

damping and ferromagnetic resonance, please contact 

R.D. McMichael. 

Andrew Kunz and R.D. McMichael, “Normal Mode 

Mixing and Ferromagnetic Resonance Linewidth.” IEEE 

Trans. MAG, (in press). 

7 
Technical Highlights


Ballistic Magnetoresistance:


A New Phenomenon with Great Potential for Magnetic Sensors


Magnetic sensors play a central role in many important 

technologies ranging from data storage to health care 

to homeland security. A common need among these 

technologies is higher sensitivity and smaller size. 

One possible route to higher sensitivity and smaller size 

is the introduction of the Ballistic Magnetoresistance 

(BMR) effect as a method of sensing magnetic fields. 

Although BMR is, at present, a poorly understood and 

poorly characterized effect, it has shown very large 

magnetoresistance values in nanoscale devices and 

could potentially lead to dramatic improvements in 

magnetic sensors. NIST has initiated a program aimed 

at clarifying, controlling, and utilizing BMR for advanced 

magnetic sensor applications. 

Magnetic sensors play a central role in many 

important technologies. To name just a few, 

computer hard disk drives use magnetic sensors to read 

stored data, magneto-encephalography uses magnetic 

sensors to image brain wave activity, and bio-hazard 

detectors use magnetic sensors to detect magnetic 

beads that are bio-tagged for biological agents such as 

anthrax, botulism, and cholera. 

Figure 1: Computer hard disk drives use a magnetic 

sensor to read data. 

A common need among these technologies is 

sensors with higher sensitivity and smaller size. With 

higher sensitivity and smaller size, more data could be 

stored on a hard disk, higher resolution imaging of 

brain activity would be possible, and earlier warnings 

of bio-contamination could be given. 

The recent discovery of the Ballistic Magnetoresistance 

effect (BMR) holds the promise of both greatly increased 

sensitivity and greatly reduced size for magnetic sensors. 

Figure 3 illustrates how a typical sample is fabricated. 

Magneto-encephalography: Imaging Brain Activity 

An array of 37 magnetic sensors: An image of epileptic activity: 

Figure 2: Magnetic sensors are the only technology 

available for real-time imaging of brain activity. Current 

sensors are bulky and provide low resolution. Advanced 

sensors could provide much higher resolution and provide 

improved surgical guidance. 

A sharp Ni wire is placed about 20 μm from a flat Ni 

substrate. In an electrochemical cell, an electrodeposition 

potential is applied between the wire and substrate. A fine 

column of Ni grows out from the wire until it meets the 

substrate. When electrical contact is made between the 

column and the substrate the electrodeposition potential 

drops immediately to zero and the electrodeposition stops. 

At the point of contact with the substrate, the column has 

a diameter of ~10 nm. When the wire and substrate 

are magnetized in parallel, electrical current easily flows 

through the nanocontact. However, when the magnetization 

is antiparallel, as illustrated in Figure 3, electrons tend 

to be reflected at the nanocontact because they have 

the wrong spin to pass easily through this region, and 

a sharp increase in electrical resistance is observed. 

This effect is known as magnetoresistance, and values 

as large as 700% have been observed in this type of 

magnetic nanocontact. 

Figure 3: An illustration of magnetic nanocontacts formed 

by electrodeposition that exhibit very large values of 

magnetoresistance (N. García, et. al., 2001). 

8 
Technical Highlights


To put this result in context, the sensors that read data 

from hard disk drives currently have a magnetoresistance 

of only about 15%, almost 50 times smaller. Moreover, 

the size of the nanocontact in BMR samples is ~ 50 

times smaller than the hard disk drive sensors. Thus, 

the BMR effect holds the potential for magnetic sensors 

of greatly increased sensitivity and greatly reduced size. 

The term “ballistic” means that the nanocontact is 

too small for electrons to flip their spin in transit, as 

they would in a macroscopic Ni sample. 

Unfortunately, it often takes many years to go from 

laboratory demonstration of a concept to a commercially 

successful device. While BMR looks promising, it is 

certainly at an early stage of development. The samples 

investigated so far have poor reproducibility, poor stability, 

and poor reliability. The techniques of fabrication are 

poorly understood, and there is no theory that can 

explain the magnitude of the BMR effect. 

Fortunately, there is the precedent of the Giant 

Magnetoresistance (GMR) effect to serve as a model. 

When GMR was discovered in 1989, it was subject 

to very similar shortcomings. Many experts thought it 

would never be a commercially successful technology. 

However, the technical community, assisted by a strong 

effort at NIST, began to address the issues, and 

gradually the problems were solved. The result is that, 

today, every hard disk drive produced in the world uses 

GMR technology in the read head. 

Clearly, the sample geometry illustrated in Figure 3 is 

not suitable for fabrication of hard disk read heads. The 

industry’s manufacturing practices require lithographic 

processing on wafers, and a fundamentally different 

approach would be prohibitively expensive. In light of 

this need, initial work at NIST has focused on techniques 

for achieving BMR in planar geometries on wafers. 

Our first attempt is illustrated in Figure 4. Although 

the geometry looks ideal, the BMR achieved so far is 

only 14%. We believe the problem lies in the method of 

pinhole formation. Consequently, we are exploring novel 

approaches to controlling pinhole size, such as the use 

of the Coulomb explosion that occurs when a highly 

charged ion like Xe44+ contacts a surface. By varying 

Figure 4: A planer geometry for BMR. Pinholes are 

created by dielectric breakdown at thin spots in an Al2O3 

film when the electrodeposition potential is applied. 

the charge on the ion, the size of the pinhole can be 

finely tuned. 

A different and much more successful planar 

geometry on a wafer is illustrated in Figure 5. In this work, 

a Ni film ~10 nm thick is deposited on an insulating 

wafer and patterned into the form of a nano or micro 

gap. Electrodeposition is used to bridge the gap with a 

Ni nanocontact. In such samples, we have been able to 

achieve a much higher BMR value of 350%. However, 

problems with reproducibility, stability, and reliability 

remain. We are investigating these shortcomings with 

scanning electron microscopy (SEM) with polarization 

analysis, transmission electron microscopy (TEM), 

Lorentz microscopy, and scanning tunneling microscopy 

(STEM). The field of BMR is so new that very little 

microscopy has been carried out to date. 

Figure 5: An illustration of Ni films with lithographically 

patterned gaps for electrodeposition of magnetic 

nanocontacts on wafers. 

We believe that with these studies, it is likely that 

the shortcomings of BMR materials can be addressed, 

and BMR technology can move towards a new 

generation of ultrasensitive nanoscale magnetic sensors 

that will have wide-ranging impact on many important 

technologies. 

“The technical challenges facing the data storage 

industry in the next 10 years are so broad and so deep 

that the industry cannot do it alone. We need 

researchers like you here at NIST to help us.” 

Dr. Sining Mao 

Director, Read-Head Research


Seagate Technology


June 14, 2002


For More Information on this Topic 

Contact: W.F. Egelhoff, Jr. 

M. Muñoz, G.G. Qian, N. Karar, H. Cheng, 

I.G. Saveliev, N. García, T.P. Moffat, P.J. Chen, L. Gan, 

and W.F. Egelhoff, “Ballistic Magnetoresistance in a 

Nanocontact between a Ni Cluster and a Magnetic Thin 

Film.” Appl. Phys. Lett., 79, p. 2946, (2001). 

9 
Technical Highlights


Advanced Metallizations for Sub-100 Nanometer Electronics


Electrodeposited copper is rapidly replacing aluminum 

in device interconnect technology because of its lower 

electrical resistivity, superior electromigration behavior, 

and the ability to fill fine features without the formation 

of seams or voids. As feature dimensions go below 

100 nm difficulties in maintaining performance are 

anticipated. In FY2002 we have pushed the quantitative 

limits of the Curvature Enhanced Accelerator Coverage 

(CEAC) mechanism developed in the Metallurgy 

Division of NIST. Exploring the mechanism has 

yielded new electrochemical processing routes for 

improved metallization and is guiding the development 

of advanced metallizations beyond copper as well as 

new processing routes such as surfactant catalyzed 

chemical vapor deposition. 

This Metallurgy Division project is meeting the 

microelectronics industry’s need for improved 

device metallization by exploring advanced materials 

and processes for superconformal film growth. 

In FY2002 we have: 

■ Established the generality of the CEAC model for 

superfilling by electrodeposited silver and other metals; 

■ Developed a new processing method for eliminating the 

delay time for superfill to begin during electrodeposition, 

thereby increasing the aspect ratio and decreasing the 

width of trenches that can be superfilled; and 

■ Extended the CEAC mechanism to quantitatively 

predict superfill during chemical vapor deposition. 

Our current measurement and modeling effort is 

focused on copper and silver metallizations, the latter 

metal having the lowest resistivity of any element, thus 

having potential on-chip applications. Superconformal 

Figure 1: Superconformal filling of vias during silver (left) 

and copper (right) electrodeposition (NIST Metallurgy 

Division, using patterned wafers from International SeMaTech). 

silver deposition was demonstrated this year in 

the Metallurgy Division and is the first example of 

superconformal feature filling with a metal other than 

copper. “Superfilling” is characterized by bottom-up 

deposition as shown in Figure 1. 

Filling of trenches and vias with silver and copper 

is quantitatively explained by the Curvature Enhanced 

Accelerator Coverage Mechanism (CEAC) developed 

at NIST. Electrochemical and surface analytical 

measurements on planar substrates were used in 

FY2002 to establish a one-to-one correlation between 

catalyst coverage and the metal deposition rate. 

In the case of silver deposition, adsorbed selenium 

was found to catalyze the deposition rate. For the 

thiol /disulfide-polyether-halide additives used in copper 

superfilling, the sulfonate-end group of the thiol or 

group of the thiol or disulfide molecules was found to 

destabilize the passivating polyether surface film thereby 

accelerating the local metal deposition rate. 

The insight provided by uncovering the CEAC 

mechanism has enabled the development of a new 

two-step process for superconformal film growth; 

in contrast to standard electrodeposition techniques, 

the catalyst is deposited on the substrate prior to the 

metallization. Specifically, the patterned substrate is first 

Figure 2: Time evolution of trench filling after different 

“derivitization” steps. The concentration of SPS or MPSA 

catalyst used for the 30 s surface derivitization steps are 

indicated. All specimens were transferred to a catalyst-free 

electrolyte for copper deposition. 

10 
Technical Highlights


“derivitized” or “dosed” with a submonolayer coverage 

of catalyst and then transferred for electroplating 

in an electrolyte that does not contain the catalyst. 

For an optimum catalyst coverage, superconformal 

filling of trenches and vias occurs as shown in 

Figure 2 (50 μmol/L SPS). If the catalyst coverage 

is too low or high, conformal or subconformal 

deposition occurs, resulting in void formation during 

feature filling (0.5, 500 μmol/L SPS, 1mmol/L 

MPSA). The filling behavior is completely analogous 

to that obtained using a single (conventional) 

electrolyte containing both catalytic and inhibiting 

species. The new process provides unambiguous 

verification of the CEAC mechanism of superconformal 

film growth. Restricting the catalyst to the surface prior 

to metal deposition also enables the rate differentiation 

provided by the CEAC mechanism to be increased 

relative to the conventional process. From a technical 

perspective, the two-step process offers an interesting 

solution to the difficult control issues associated with 

catalyst destruction and related aging effects which are 

known to occur in the “conventional” single-electrolyte 

superfilling process currently used in industry. 

The generality of the CEAC mechanism has now been 

extended to include the first quantitative prediction of 

superconformal chemical vapor deposition (CVD). More 

recently, this work has enabled a direct comparison of the 

CEAC mechanism with detailed experiment results on iodine 

catalyzed copper CVD as shown in Figure 3. 

Project results from FY2002 have firmly established 

the generality of the Curvature Enhanced Accelerator 

Coverage (CEAC) mechanism, which we developed in 

FY2001 to explain superconformal electrodeposition of 

copper. The output also clearly demonstrates the predictive 

power of the CEAC formalism. 

Three different electrode-shape change algorithms 

have been developed. They show excellent agreement 

with experimental results. 

These algorithms, in the form of software, are 

available from the Metallurgy Division website and 

are currently being examined by Texas Instruments 

and IMEC. In addition, Motorola (B. Melnick and 

M. Freeman), International SeMaTech (C. Witt) and 

Figure 3: Superconformal filling of vias during iodine 

catalyzed chemical vapor deposition. Experimental via 

results are from Hynix Semiconductor, and model predictions 

for a trench are from the Metallurgy Division of NIST. 

Hynix Semiconductor (S.G. Pyo) are now active 

collaborators in our experimental and modeling efforts. 

The first two provide patterned wafers for NIST 

electrodeposition studies; the last provides results from 

iodine catalyzed chemical vapor deposition experiments 

for NIST modeling. 

Selected Project Publications for FY2002 

D. Wheeler, D. Josell and T.P. Moffat, Modeling 

Superconformal Electrodeposition Using the Level Set 

Method, J. Electrochem. Soc., submitted July 2002. 

T.P. Moffat, D. Wheeler, C. Witt and D. Josell, 

Superconformal Electrodeposition Using Derivitized 

Substrates, Electrochemical and Solid-State Letters, 

submitted May 2002. 

D. Josell, S. Kim, D. Wheeler, T.P. Moffat, S.G. Pyo, 

Superconformal Deposition by Iodine-Catalyzed 

Chemical Vapor Deposition, J. Electrochem Soc., 

submitted May 2002. 

B.C. Baker, M. Freeman, B. Melnick, D. Wheeler, 

D. Josell, T.P. Moffat, Superconformal Electrodeposition 

of Silver from a KAg(CN)2-KCN-KseCN Electrolyte, 

J. Electrochem. Soc., in press. 

D. Josell, B. Baker, C. Witt, D. Wheeler and 

T.P. Moffat, Via Filling by Electrodeposition: 

Superconformal Silver and Copper and Conformal 

Nickel, J. Electrochem. Soc., in press. 

T.P. Moffat, B. Baker, D. Wheeler, J.E. Bonevich, 

M. Edelstein, D.R. Kelly, L. Gan, G.R. Stafford, 

P.J. Chen, W.F. Egelhoff, and D. Josell, Superconformal 

Electrodeposition of Silver in Submicron Features, 

J. Electrochem. Soc. 149, C423 (2002). 

D. Josell, D. Wheeler and T.P. Moffat, Superconformal 

Electrodeposition in Vias, Electrochemical and Solid-State 

Letters 5, C49 (2002). 

D. Josell, D. Wheeler and T.P. Moffat, Superconformal 

Deposition by Surfactant-Catalyzed Chemical Vapor 

Deposition, Electrochemical and Solid-State Letters 5, 

C44 (2002). 

D. Josell, D. Wheeler, W.H. Huber, J.E. Bonevich 

and T.P. Moffat, A Simple Equation for Predicting 

Superconformal Electrodeposition, J. Electrochem. 

Soc. 148, (12) C767 (2001). 

Our findings have also been conveyed to U.S. 

industry, academia and other national laboratories 

through more than ten external presentations in the 

last year. 

For More Information on this Topic 

D. Josell, D. Wheeler, B. Baker, T.P. Moffat 

11 
Technical Highlights


Performance-Limiting Defects in GaN


The III-V nitrides and GaN, in particular, are 

emerging new semiconductors for electronic devices, 

including light-emitting diodes (LED) and laser 

diodes in the blue-green and UV wavelengths, UV 

detectors and ultrahigh power switches. The main 

challenges in this technology are optimization of 

optical output efficiency and stability of metal contacts. 

One objective of the MSEL project on GaN is to 

quantify the effect of GaN defects, in particular 

of threading dislocations, on these properties. In 

FY2002 a mechanism for the degradation of electrical 

contacts through threading dislocation-mediated phase 

transformations was determined through detailed 

characterization using transmission electron microscopy. 

Doping methods to disable the mechanism may lead to 

greatly improved stability, reliability, and performance 

of commercial GaN devices. 

Direct bandgap GaN and its alloys with AlN and InN are receiving considerable attention as 

promising semiconductors for electronic devices 

operating at high temperatures, high frequency and 

high power and for optoelectronics applications in the 

blue-green and UV wavelengths. Therefore, electrical 

contacts to the nitrides (ohmic contacts and Schottky 

barriers) which are stable at elevated temperatures are 

needed. 

As bulk crystals of these materials are not available, 

GaN is epitaxially grown on a substrate, usually on 

(0001) sapphire or (0001) 6H-SiC. Because of a large 

lattice mismatch between the substrates and GaN, high 

densities of various crystallographic defects are present 

in the active GaN layers. Among the defects that can 

cross the epitaxial GaN layer and reach a surface are 

threading dislocations, inversion domains, nanopipes 

and prismatic planar defects. 

In order to achieve desirable characteristics of ohmic 

contacts, different combinations of different metal layers 

have been studied. For example, the commonly accepted 

contact to p-type GaN is Ni /Au which gives good 

electrical characteristics after annealing at 400-600°C. 

For higher temperatures, the electrical characteristics 

worsen and severe degradation of contact morphology 

is observed. Degradation of such electrical contacts are 

associated with dislocations in GaN, island formation 

in the contact layers, and decomposition of GaN. In 

FY2002, NIST developed a mechanism for contact 

degradation that is based on heterogenerous nucleation 

of GaN decomposition at threading dislocations/metal 

interface, followed by wetting of the threading 

dislocation by liquid Ga. The morphology of the metal/ 

GaN interface is an important issue: if the Ga metal 

were to penetrate through a thin GaN layer and reach an 

underlying layer in a device, the device could be rendered 

inoperable. Furthermore, the stability of interfacial 

morphology is a general concern for contacts to all 

semiconductors. 

Reaction and interdiffusion in the Au/Ni/GaN 

system as a function of annealing temperature from 

400 to 900°C has been investigated by several groups, 

mostly using Rutherford backscattering (RBS), Auger 

spectroscopy and x-ray scattering. Only rarely has 

this microstructural evolution been directly observed 

using transmission electron microscopy (TEM). 

In collaboration with researchers from the Electrical 

Engineering Department at Howard University, we 

investigated electrical and microstructural behavior of 

Ni/Au bilayers as a function of annealing temperature, 

with emphasis on structural evolution at a TEM level. 

The as-deposited layers consisted of 50 nm of Ni and 

35 nm of Au, with Ni in contact to n-type GaN. Ohmic 

contacts with a specific contact resistivity, ρs, as low as 

6.9 × 10-6 Ω-cm2 for a doping level of 5.0 × 1017 cm-3 

were obtained after annealing the sample for 10 s at 

800°C. Two very important conclusions were achieved 

from the TEM investigation: 

1. A strong reaction between the metal contact layer 

and the threading dislocations core structure leads 

to decomposition of GaN along dislocation lines. 

Such behavior will be a major factor limiting annealing 

temperature and operation temperature/time of devices. 

2. Interdiffusion between Ni and Au results in reversal 

of Au and Ni phases across the metal film. Thus, 

after annealing the phase primarily responsible for 

the formation of the energy barrier of the contact 

between GaN and metal contact is Au-based. 

Figure 1: SEM image of Au/Ni/GaN/sapphire annealed 

at 600 and 800°C for 10 sec. 

Figure 1 shows a SEM image of Au/Ni/GaN 

annealed at 600 and 800°C for 10 sec. For the 

imaging, we used a cross-sectional ion milled TEM 

specimen where two differently annealed specimens 

were glued face to face. Whereas at 600°C the metal 

film is continuous, at 800°C severe degradation of 

the metal contact occurred. In many places the film is 

12 
Technical Highlights


separated from GaN, and deep V-shaped pits can be 

found penetrating GaN. Such pits are detrimental to 

the near-surface electrical performance of devices. 

TEM analysis of these specimens showed that 

the V-shaped pits are always associated with the 

threading dislocations. Figure 2 shows bright and dark 

field images of the 600°C-annealed specimen. The pits 

are clearly seen in the bright field image and marked 

by triangles. The weak beam imaging using different 

g-vectors established that each pit is connected to a 

place where a threading dislocation exits GaN. The 

threading dislocations vary in character (e - edge, 

s - screw and m - mixed). 

Figure 2: Bright field (upper) and weak-beam dark field 

(bottom) images of the 600°C-annealed specimen. 

Bright and dark field images of the 800°C-annealed 

specimen are shown in Figure 3. The pits associated 

with the threading dislocations in the specimen are 

significantly deeper and wider. The metal film in some 

places is lifted from the GaN surface, and in other 

places, the surface of GaN is exposed. It appears that 

the surface of GaN, between the dislocations, was not 

degraded and remained flat (see arrows in Figure 3). 

This phenomenon, the elevated temperature chemical 

instability of GaN defects exposed to either metal films 

or free surfaces, is very general in nature and has 

importance for GaN-based device design. Bulk GaN 

has the following decomposition reaction above 800°C: 

GaN 6 Ga(l)+N2(g). Nevertheless, GaN films can 

survive higher temperatures due to the high stability of 

the (0001) surface. In addition, the reaction is sluggish 

due to kinetic difficulties recombining nitrogen atoms 

into N2 molecules on the GaN surface. At locations 

where a dislocation exits GaN, the atomic arrangement 

is of lower stability and therefore triggers the 

decomposition of GaN (Figure 4). Nitrogen atoms 

may diffuse into the metal, recombine into molecules 

and form N2 gas. Such gas accumulates under the 

metal film and exerts enough pressure to cause metal 

film de-cohesion (see Figure 3). 

Figure 3: Bright field (upper) and weak-beam dark field 

(bottom) images of the 800°C-annealed specimen. 

Figure 4: Schematic drawing illustrating decomposition of 

GaN along a dislocation line and resulting in the formation 

of N2. 

For More Information on this Topic 

L.A. Bendersky, A.V. Davydov, W.J. Boettinger 

13 
Technical Highlights


Responding to the Auto Industry’s Research Needs in Materials: 

Forming of Lightweight Materials 

In response to a recommendation by the NIST Visiting 

Committee on Advanced Technology, the Industrial 

Liaison Office (ILO) was established to address the 

desire of NIST Senior Management for NIST to “close 

the loop with industry.” In particular, although NIST 

receives excellent recognition for its work from industrial 

project leaders and bench level scientists and engineers, 

at higher levels of industrial R&D management, 

the impact of NIST’s work is frequently unknown. 

Since the automotive industry, one of NIST’s largest 

“customers,” was chosen as a targeted sector, several 

projects within the MSEL Program on Forming of 

Lightweight Materials for Automotive Applications were 

selected to test the industry feedback process and 

answer the question: “Are we meeting industry’s needs?” 

The feedback results were overwhelmingly positive. 

The NIST Industrial Liaison Office (ILO) chose three 

projects within the Metallurgy Division to assess the 

impact of NIST Laboratory Programs on the auto industry: 

■ Standard Test Method Development for Sheet Metal 

Forming 

■ Microstructural Origins of Surface Roughening and 

Strain Localization 

■ Process Models for Metal–Matrix Composites 

Detailed descriptions of the first two projects are 

contained in this annual report. The project on Process 

Models for MMCs was completed last year and was 

described in the FY01 annual report. 

The ILO process began with the development 

of surveys that were targeted for a cross-section of 

researchers, managers, and directors in the automotive 

and associated industries. The surveys contained brief 

descriptions of the projects and provided web sites 

with more detailed project results. At this point, the 

respondents were queried as to their familiarity with the 

projects and whether the intended outputs were useful 

to their companies. A series of questions was designed 

to assess the impact of the projects on the automotive 

industry. Finally, the survey sought feedback as to 

whether some modifications to the projects or any 

other research would be more valuable than the 

current projects. 

A list of potential industrial contacts was made for 

each project consisting of researchers, managers, and 

executive level staff from the appropriate companies. 

The ILO manager then contacted these individuals and 

requested their participation in the survey. The surveys 

were sent out only to those who agreed in advance to 

provide feedback to NIST. The ILO manager again 

contacted each individual to go over the survey. For the 

three projects mentioned, more than 50 surveys and 

interviews were completed. 

Figure 1: A transmission fluid pump component showing 

centerline porosity (light band) predicted using process 

modeling shown in Figure 2. 

Figure 2: Predicted density of the powder part which is 

shown in Figure 1. Note low density regions in the middle. 

Results of Surveys 

Standard Test Method Development 

for Sheet Metal Forming 

Objective: Enable the production of more accurate 

dies for auto body parts. 

Approach: Produce, measure, and analyze 

multi-axially strained sheet samples. 

Product: New standard tests and metrology to 

accurately determine sheet metal mechanical response 

under forming conditions. 

Relevance: Enables use of lighter, high strength 

materials required to meet fuel efficiency goals. 

Industry Response: The survey revealed that this 

project is already known and appreciated by a significant 

portion of the appropriate people in the auto industry. 

Its uniformly high scores for impact, value of output, and 

importance indicate that it would be mutually beneficial to 

extend this awareness to an even greater portion of the 

industry. The reviewers provided a list of potential new 

14 
Technical Highlights


contacts. The addition of these new contacts to future 

communications by NIST researchers with the automotive 

industry will help expand the visibility of this project. 

Impact of Survey on NIST: Following these surveys, 

the results were reviewed with the NIST researchers, 

the Group Leader, the Metallurgy Division Chief, and 

the MSEL Director. As a result of the survey, the 

NIST research team has been able to: (1) validate 

their priorities for materials to be tested, (2) reinforce 

the current priorities, (3) identify 13 new contacts, 

(4) learn of the desired form of communicating project 

results, (5) learn more about types of standard testing 

that already exist in industry, and (6) identify important 

future directions. 

Figure 3: A pre-standard cup test specimen used at 

NIST to measure formability and constitutive behavior under 

equibiaxial strain conditions. 

Microstructural Origins of Surface 

Roughening and Strain Localization 

Objective: Develop measurement methods, models, 

and data that enable industry to predict the behavior of 

sheet metal in dies. 

Approach: Explore the origins of inhomogeneous 

deformation and its quantification and behavior 

prediction for use in finite element codes. 

Product: Microstructural and formability databases 

for aluminum and steel. 

Relevance: By better understanding the interplay of 

the material and the stress states encountered within the 

die, the die tryout period can be reduced and significant 

cost savings realized. 

Industry Response: The response was extremely 

positive. About 2/3 of the respondents were already 

aware of the project. Those who were not previously 

aware of this work became interested as they learned 

about it. The expected outputs were all considered to 

be useful and valuable. The window of opportunity was 

thought to be 12 months. Respondents felt the work 

was important and that NIST’s assessment of its impact 

was valid. Only minor modifications were suggested. In 

particular, high-strength steel and advanced high-strength 

steel were mentioned as additional alloys of industrial 

interest. They are eager to establish communications 

with NIST to follow the progress of this project. 

The respondents supplied a number of new contacts. 

Impact of Survey on NIST: The NIST research 

team will include several new steel alloys in the project. 

They also intend to communicate their results directly 

to the 13 new contacts identified during this process. 

Process Models for Metal–Matrix Composites 

Objective: Provide process models for the USAMP 

project “Low Cost Powder Metallurgy Technology for 

Particle Reinforced Aluminum (PRA)” to accelerate the 

introduction of PRA into auto parts and to capture the 

knowledge generated by the USAMP project in a readily 

usable form. 

Approach: Provide models for lightweight metal 

consolidation, measurements and data for model 

validation, software that readily transfers the models, 

and data required to implement the models. 

Product: Models and input data for commercial 

software. 

Relevance: Enables use of lighter, high-strength 

materials required to meet fuel efficiency goals. 

Industry Response: A limited number of responses 

were received, perhaps due to the fact that this project 

was already completed. “Expected outputs” were rated 

4.3 out of 5, indicating high value. Three-quarters of 

the respondents agreed with NIST’s assessment of the 

project’s impacts and importance. Additional impacts 

were identified by the respondents. No modifications 

were suggested, but suggestions for future related 

projects with details were made. 

Impact of Survey on NIST: An interesting issue 

was raised by the survey. A respondent who knew and 

approved of NIST’s work did not understand that the 

modeling software developed by NIST and its partners 

is broadly applicable to powder consolidation of a wide 

range of alloys and conditions, not just those of direct 

interest to the USAMP project. Scientists sometimes 

assume that the generality of their work is understood; 

this is a communication issue that must be addressed 

in order to ensure the greatest impact and application 

of technical developments. 

For More Information on this Topic 

Standard Test Method Development for Sheet 

Metal Forming and Microstructural Origins of Surface 

Roughening and Strain Localization: T. Foecke, 

S. Banovic; Process Models for Metal Matrix 

Composites: R. Fields; NIST Industrial Liaison 

Office and the impact of these projects on industry: 

C. Allocca 

15 
Technical Highlights


Thermodynamic Database for Multicomponent Alloys


Commercial alloys rarely consist of only two elements 

and some contain up to 10 elements. Thermodynamic 

modeling allows the prediction of phase equilibria in 

multicomponent alloys from the extrapolation of the 

thermodynamic descriptions of the constituent binary 

and ternary systems. Different properties of a 

system, such as phase boundaries and enthalpies 

are described with one set of functions resulting in 

a consistent description of phase properties. The 

approach gives reasonable predictions for complex 

alloys, thereby providing a powerful tool for alloy 

design, and provides a compact storage method 

for large amounts of phase diagram and other 

thermodynamic data. 

During the last decade, researchers from the 

Metallurgy Division have collaborated with 

scientists from universities and industry on several 

projects with emphasis on modeling tools for the 

design and manufacture of multicomponent alloys. 

The traditional approach for development of a new alloy 

relies on the knowledge and experience of the engineer, 

which can be costly due to the significant amount of 

testing required to obtain the correct properties. 

Structural parts made from Ni-base superalloys not 

only must withstand extended periods of service at high 

temperatures, but also must tolerate severe environmental 

conditions, such as the highly corrosive environment of 

a jet engine. Higher operating temperatures result in 

increased performance demands for both aerospace 

applications, as well as land-based energy applications. 

For a number of projects, including the NISTsponsored Consortium on Casting of Aerospace Alloys, 

the DARPA sponsored Investment Casting Cooperative 

Arrangement, and the General Electric-lead DARPA 

project for Accelerated Insertion of Metallic Structural 

Materials (AIM), the Metallurgy Division has constructed 

a thermodynamic database for Ni-base alloys. The 

NIST Ni-superalloy thermodynamic database includes 

10 elements, Ni-Al-Co-Cr-Hf-Mo-Re-Ta-Ti-W, and is 

based on critically-evaluated literature and NIST work. 

Phase equilibria can be calculated from this database. 

Since the immediate goal for the application of this 

database was for the modeling of single crystal alloys, 

the final refinement of the description in the database 

was restricted to the liquid, fcc-γ and L12- γ ́ phases. 

Figure 1 shows the comparison of experimental liquidus, 

solidus and solvus temperatures and those predicted 

from the calculation for a series of commercial superalloys. 

Experimental and calculated phase boundary data for 

the γ-γ ́ two-phase region are compared in Figure 2. 

As a result of this work, detailed solidification 

behavior for Ni-base superalloys can be predicted. 

This improved the quality of solidification simulations 

for investment castings by providing more reliable 

predictions of casting defects allowing industry to 

eliminate the need for extensive testing of a series of 

castings to reach an acceptable design. 

In addition to a dependence on the multicomponent 

thermodynamics, a wide variety of Ni-base superalloy 

applications are controlled by diffusion processes 

including solidification, homogenization, γ ́ precipitation, 

bonding and repairing processes, and protective bond 

coats. Many of these industrial problems can be 

addressed using a diffusion simulation code that combines 

composition-dependent diffusivities with multicomponent 

thermodynamics. The thermodynamic database was 

used for the development of a diffusion mobility database 

for Ni-base superalloys. The NIST mobility database 

can be used in conjunction with the NIST Ni-superalloy 

thermodynamic database, as well as with other commercial 

thermodynamic databases. 

Electronic versions of the NIST databases have 

been distributed to various industries, universities, and 

national laboratories. 

Most databases that are currently available to scientists, 

engineers and students need to be expanded and 

improved. A workshop on “Databases for Computational 

Thermodynamics and Diffusion Modeling” was held at 

NIST Gaithersburg, March 21–22, 2001. The workshop 

format was a series of invited talks given to the group as 

a whole followed by general discussions of needs and 

benefits. The workshop was attended by 39 registered 

participants of which 16 were from industry. Of the 

17 oral presentations given, 8 were from industry, 

Figure 1: Comparison of experimental and calculated 

liquidus, solidus and solvus temperatures of superalloys. 

16 
Technical Highlights


Figure 2: Comparison of experimental and calculated phase boundary data for the γ-γ ́ two phase region. 

emphasizing the applicability of the modeling approach 

to industrial processes. Extensive discussions followed 

the presentations. 

The participants at the workshop agreed that, by the 

year 2010, it is highly likely that all Materials Science 

and Engineering students will learn to solve real world 

materials problems using modeling and simulation tools. 

The national benefits of providing materials engineers 

with software and databases for modeling materials and 

processing are savings in costs, energy and natural 

resources via optimization studies, as well as improved 

materials properties and development times. The primary 

deliverables of the workshop were, first, to identify the 

database and information delivery tool needs of industry 

and, second, to propose a roadmap for how these needs 

can be met. 

Expanded collaborative efforts are needed in areas 

of materials education, basic research, and database 

development within the next decade to meet these needs. 

Working groups will be formed for each of these areas in 

FY2003. The primary objective for materials education 

identified at the workshop is to interest faculty and 

students in applied thermodynamics and kinetics by 

preparing a collection of applied problems. The current 

NSF program at Penn State University on computational 

thermodynamics and kinetics will serve as a model for 

improving abilities of students in these research areas. 

Basic research was identified to be of crucial importance 

to generate experimental, as well as calculated data from 

first-principles calculations. This requires a broad 

initiative to rebuild the thermodynamic and kinetic 

measurement infrastructure and to encourage theoretical 

a priori studies. The action items identified for public 

databases include encouragement of journal policies to 

require publication of parameters in assessment papers, 

recommendation and publication of a data format designed 

for portability of the thermodynamic parameters and 

fostering industrial user groups to identify software needs. 

The second major activity for FY2002 was 

developing a relationship with SGTE (Scientific Group 

Thermodata Europe), one of the leaders in the world 

effort to develop thermodynamic databases for inorganic 

and metallurgical systems and their applications to 

practical, industrial problems. SGTE was originally a 

consortium founded by European centers active in 

database development. Today membership in SGTE 

is no longer limited to European organization and the 

NIST is being welcomed into the now international 

group. The aims of SGTE are the critical assessment 

and compilation of self-consistent thermodynamic data 

for both pure substances and solutions of all types. 

SGTE has pioneered the development of multicomponent 

databases. This includes compilation of the Gibbs 

energies of the pure elements, published by SGTE in 

1991, thermodynamic properties of stoichiometric 

inorganic compounds in 1999 to 2001 and the 

planned publication of databases for binary systems. 

The self-consistency of the SGTE databases has made 

the thermodynamic quantities and model descriptions 

de facto standards for the construction of databases 

for multicomponent systems. Joining SGTE will enable 

NIST to contribute to the discussion of future model 

choices and cooperate in the broader international 

effort to unify thermodynamic data. 

For More Information on this Topic 

U.R. Kattner, W.J. Boettinger, C.E. Campbell 

(NIST/MSEL) 

U.R. Kattner, CALPHAD and Alloy Thermodynamics, 

eds. P.E.A. Turchi, A. Gonis, and R.D. Shull, “Construction 

of a Thermodynamic Database for Ni-base Superalloys: 

A Case Study.” TMS, pp. 147–164, 2002. 

17 
Program Overview


Advanced Manufacturing Methods


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 

18 
Advanced Manufacturing Methods


Modeling Solidification and Microstructure Evolution


Many properties of structural and functional materials 

depend on the distribution of composition, phases, 

grain orientations, and microstructure on the scale of 

1–100 mm. Models of alloy eutectic solidification, 

dendrite coalescence and electrodeposition are being 

developed using several advanced computational 

methods. The goal of this research is to develop a 

suite of modeling tools for the evolution of complex 

microstructures for a wide variety of processes. These 

models are providing information to aid in designing 

materials processing systems that increase product 

yield and performance. 

James A. Warren and William J. Boettinger 

Modeling of the evolution of microstructure produced 

by solidification, electrodeposition and other 

processes involves mathematical solution of equations for 

heat flow, fluid flow, current flow and/or solute diffusion. 

Boundary conditions on external surfaces reflect the 

macroscopic processing conditions. Boundary conditions 

at internal interfaces correspond to the liquid-crystal (grain) 

or grain-grain interfaces. These internal interfaces are 

moving boundaries and require boundary conditions with 

thermodynamic and kinetic character. For solid-solid 

transformations, stress and strain replace fluid flow 

as a consideration. 

In order to deal with the complex interfacial shapes 

that develop during solidification, electroplating and 

grain growth, the phase field method has become 

the technique of choice for computational materials 

scientists. This approach often requires numerical 

techniques to solve the model equations but readily deals 

with complex interface shapes and topology changes. 

The research, conducted in the Metallurgy Division, is 

supported in part by the NIST Center for Theoretical 

and Computational Materials Science. 

Dendritic and eutectic growth is always present 

in castings and involves extremely complex interface 

shapes. Three major accomplishments of FY2002 deal 

with the application of diffuse interface modeling to 

these types of growth. 

Classical treatments of eutectic characterization and 

morphology selection require a priori knowledge of the 

eutectic microstructure. The phase-field method does 

not suffer from this limitation and serves as a useful 

tool for predicting microstructures of multi-component 

eutectics where complicated phase arrangements occur. 

In FY2002, a phase field model for solidification of 

binary eutectics was developed, was validated by classical 

models for eutectic morphology selection, and is now 

being used in regimes well outside the validity of those 

classical models (Figure 1). 

Phase field models of grain growth, pioneered at NIST, 

have been adopted by several other research groups, now 

investigating nucleation, polymer solidification, spherulitic 

growth and fractal structures. (See, for example, 

L. Gránásy, T. Börzsönyi, and T. Pusztai, Phys. Rev. Lett. 

88, 206105 (2002)). A comprehensive overview of the 

physics of these models has been submitted for publication. 

Solidification of metallic alloys has been extensively 

studied (dendrite tip kinetics, microsegregation, coarsening 

of dendrite arms, etc.), but surprisingly little is known 

about the last stage of solidification when the primary phase 

regions impinge. Yet, the details of the final stages of 

solidification of multigrain and/or dendritic materials have 

significant impact on casting defects such as hot tearing. 

Hot-tearing is caused by a lack of tensile strength of 

castings due to the thin continuous liquid film that remains 

between dendrite arms up to very high volume fraction of 

solid. It is therefore important to know when dendrite arms 

bridge (or coalesce) to form a coherent solid that can sustain 

tensile stresses. The details of the process determine the 

temperature at which a coherent solid forms; i.e., a solid 

that can sustain tensile stresses without rupture. Using 

one dimensional (1D) interface tracking calculations, 

diffusion in the solid phase perpendicular to the interface 

(back-diffusion) is shown to be a critical factor in 

determining the temperature where liquid finally disappears 

during solidification. To study the interaction of interface 

curvature and diffusion in the liquid film parallel to the 

interface, a multi-phase field approach has been used. After 

validating the method with the 1D interface tracking results 

for pure substances and alloys, the phase field approach 

shows that the coalescence process originates in small 

necks and involve rapidly changing liquid–solid interface 

curvatures. (M. Rappaz, A. Jacot and W.J. Boettinger, 

Metall. and Matls. Transactions, in press.) 

Figure 1: A snapshot of the concentration field in the liquid, 

at the liquid–solid interface, of a three-dimensional phase field 

simulation of a directionally solidified binary eutectic alloy. 

Contributors and Collaborators 

W. Boettinger, S. Coriell, J. Guyer, D. Lewis, 

R. Sekerka, G. McFadden (ITL); R. Kobayashi 

(Hokkaido University); W.C. Carter (MIT) 

19 
Advanced Manufacturing Methods


High Speed Machining 

The U.S. spends $200 billion annually on machining 

of metal parts. Industry studies have shown that 

considerable improvements in the efficiency of these 

operations are possible. Also, the rapid development 

of tooling and high-speed machines makes traditional 

knowledge-based approaches to improved efficiency 

ineffective. Predictive modeling has been promoted 

by industry as a method to realize the improved 

efficiency. Through this project, NIST will provide 

measurement capabilities, materials data, and phase 

transformation models needed to make accurate 

predictions. 

Richard J. Fields, William J. Boettinger, 

and Carelyn E. Campbell 

Machining of metal parts, e.g. turning, milling, 

drilling, broaching, etc., to required dimensional 

tolerances is an essential part of many manufacturing 

processes. Efficient processes can greatly reduce the 

price of a part and enhance the competitive position of 

the manufacturer. A recent industry survey found that 

industry chooses the correct tool for machining a part 

less than 50% of the time. Advances in spindles and 

tooling stimulated by the NIST Advanced Technology 

Program (ATP) now requires that the traditional, 

experience-based approaches to finding the optimal 

process parameters such as feed rate, cutting rate, tool 

material, tool shape, etc., be replaced by modeling and 

simulation. While initial results are impressive, data are 

still needed to validate the models and run the simulations. 

The current project is advancing the state-of-the-art 

in two complementary areas: 1) measurement of 

fundamental data on the behavior of materials at the 

extreme strain and heating rates needed for input into 

the models, and 2) modeling and characterization of the 

microstructural changes that occur during the severe 

deformation and heating in real machining operations. 

Measurements of residual stress, responsible for part 

distortion after machining, are also being conducted at 

the NIST Center for Neutron Research within MSEL. 

The first research effort is directed at obtaining 

materials data, which has required an extension of our 

current capabilities in high-rate heating to include high 

rate straining. Three significant activities have been 

completed. First, a “high-heating-rate model” of the 

modified Hopkinson bar compression test device has 

been created, allowing us to explore various approaches 

to obtaining uniform heating of samples during testing. 

Second, a Hopkinson bar compression tester has been 

constructed that provides strain rates on the order of 

105 s-1 (Figure 1) and heating rates of 103 Ks-1. 

Third, calibrations were completed that assure that the 

temperatures measured during the high rates of heating 

are accurate. The facility will be used to develop databases 

on a variety of materials of interest to the machining 

industry. These data will be used in simulations of 

prototypical machining operations and compared to the 

advanced machine metrological database. Evaluation of 

various models and simulations will provide direction to 

future research. 

Figure 1: Stress waves recorded on the input and output 

bars of the split Hopkinson bar. Reflected and transmitted 

waves provide data to calculate the dynamic stress–strain 

behavior. 

The second research effort focuses on characterizing 

and modeling microstructure changes in the 

deformation/hot zone of Al alloys during machining. 

Generally, significant softening occurs when precipitation 

hardened Al alloys are heated due to coarsening of the 

precipitate structure. Structure and dislocation density 

will be measured. A model that uses temperature vs time 

data from thermal images from the Physics Laboratory 

(Figure 2) will be used as input to a microstructure 

model. The model will employ thermodynamics and 

diffusion kinetics to predict microstructure changes. 

Figure 2: Thermal profile of a steel tube undergoing 

orthogonal cutting. 

Contributors and Collaborators 

D. Basak, L. Levine, R. deWit, H. Prask 

(NIST/MSEL); M. Davies, R. Rhorer, R. Polvani, 

K. Jurrens, B. Dutterer, M. Kennedy, R. Ivester, H. Soons 

(NIST/MEL); T. Burns (NIST/ITL); H. Yoon (NIST/PL) 

20 
Advanced Manufacturing Methods


Metal Powder Processing 

As engineering design requirements for Powder 

Metal (PM) parts become more demanding, powder 

size requirements have progressively dropped in 

average size and narrowed in size distribution range. 

The NIST Metallurgy Division atomization facility has 

been a test-bed for providing the PM industry with 

material property data and processing procedures for 

improving yield of desirable powder size distributions. 

This information will be provided in a comprehensive 

“Gas Atomization Recommended Practice Guide” 

to be published following a PM industry review in 

December 2002. 

Stephen D. Ridder 

Gas atomization is the primary source of material for 

many advanced Powder Metal (PM) processing 

procedures such as Powder Injection Molding (PIM), 

Hot Isostatic Press (HIP) consolidation, and Thermal 

Spray (TS) coatings. These processes are used to 

produce surgical tools and appliances, aircraft and 

power turbine engine parts, severe service parts for 

the petrochemical industry, and increasing numbers of 

critical automotive components. Powder size, because 

of its affects on microstructure, powder handling, 

and consolidation, controls the resulting PM material 

properties. The cost to produce these optimum powder 

size distributions can become prohibitively expensive 

when using traditional gas atomization techniques that 

require screening of the powder product for usable 

powder and recycling the waste. Research collaborators 

representing the major gas atomization companies and 

national laboratories have participated in various projects 

aimed at sensor development, alloy chemistry, particle 

size control, and powder characterization. Currently 

available information to be included in a NIST SP 

(Special Publication), “Gas Atomization Recommended 

Practice Guide,” includes: 1) sensors and control 

techniques to optimize the Gas to Metal mass flow-rate 

Ratio (GMR), 2) gas jet geometry designs that reduce 

adverse shock wave generation, and 3) advanced process 

control software that incorporates atomization plume 

video frames and “knowledge base” heuristics. This 

NIST SP will be available for discussion by PM industry 

participants at a workshop to be held at NIST in 

December 2002. 

Results from current aerodynamic studies of the 

supersonic gas flow produced by the atomizing nozzle 

will be published as a supplement to the NIST SP. 

Experimental evidence from a variety of sources has 

suggested that axial length scales have an important role 

in determining particle size distributions. Finer particle 

sizes tend to be produced when the length of supersonic 

gas velocity is extended in the axial direction. An 

extended supersonic zone improves secondary droplet 

atomization far from the nozzle tip (Figure 1), ultimately 

leading to finer powder. Because axial length scales have 

often been overlooked in the design of atomizing nozzles, 

opportunities exist for improving performance. For 

example, by designing nozzles to produce a specific 

axial supersonic velocity profile to achieve a desired 

size distribution, off-target particle size yields might be 

reduced, improving efficiency and reducing powder costs. 

Figure 1: Anatomy of a gas atomization plume. 

Before such benefits can be realized in practice, 

however, key questions must be addressed. Chief among 

these is determining the degree to which the supersonic 

length affects particle size. In practice, supersonic 

length is typically coupled with changes in gas velocity 

and dynamic pressure that also tend to refine particle 

size. Research efforts at NIST are therefore aimed at 

isolating the effect of supersonic length on particle size. 

Preliminary atomization experiments performed and 

presented to powder producers in FY2002 have shown 

that a 20% increase in supersonic length reduces 

median particle size by 10% [Ref. 1]. A soon-to-be 

installed vacuum system will expand the range of 

supersonic lengths that can be achieved and definitive 

experiments on supersonic gas flow will be completed 

in FY2003. Our goal is to have the results from this 

research incorporated into general design guidelines for 

gas atomizer nozzles. 

[1] S.P. Mates, F.S. Biancaniello and S.D. Ridder, 

“An Alternative View of Close-Coupled Gas Atomization 

of Liquid Metals,” PM2TEC Proceedings, MPIF, 2002. 

Contributors and Collaborators 

F.S. Biancaniello, R.D. Jiggetts, S.P. Mates 

21 
Advanced Manufacturing Methods


Electrochemical Processing of Nanoscale Materials


Precise temporal control of supersaturation provided 

by electrochemical methods holds promise for the 

synthesis and characterization of materials and 

structures of very small dimensions — nanomaterials. 

Variation of the electrochemical potential leads not 

only to changes in the metal deposition rate but also 

effects the adsorption of surfactants and segregation 

phenomena which exert a strong influence on the 

morphological evolution. Experiments are underway to 

explore the effect of manipulated growth schemes on 

roughness development during epitaxial film growth. 

Thomas P. Moffat 

Electrochemical synthesis has become an important 

tool in the fabrication of novel nanoscale devices and 

structures. Modulation of the electrode potential can be 

used to create films with a corresponding variation in 

composition and/or structure. This allows materials to 

be engineered with submonolayer precision. Looking to 

the future, exploitation of this technology will require a 

deeper understanding of potential dependent adsorption 

phenomena and its influence on morphological evolution 

during thin film growth. Several model systems are being 

examined at NIST which deal with issues important to 

both homo and heteroepitaxial film growth. A central 

aspect of this work is the combined use of atomic force 

and in situ scanning tunneling microscopy to probe 

the connection between atomistic processes and 

morphological evolution that occurs at larger length scales. 

Halide adsorption on copper represents a model 

system for such study. At potentials corresponding 

to the copper/cupric ion equilibrium, the surface is 

saturated with an ordered 2-D chloride adlayer which 

in the case of Cu(100) results in step faceting in the 

<100> direction. The adlayer floats on the surface 

during deposition and at low overpotentials pyramidal 

growth is observed with the in-plane orientation 

determined by the halide overlayer. At more negative 

potentials a transition from pyramidal to block-like 

growth is observed. The correlation between the 3-D 

growth transition and the known potential driven 2-D 

order–disorder phase transition in the halide adlayer is 

being examined. By varying the metal cation and halide 

electrolyte concentration, the relative contribution of the 

potential dependence of the metal deposition rate versus 

the dynamics of surface transport are being investigated. 

In the limit where metal deposition rate is under 

transport control, the effect of potential modulation on 

electrocrystallization events may be studied independent 

of its effect on the metal deposition kinetics. Related 

work is underway using underpotential deposition of 

simple metals, such as Pb, to be used in place of, or 

in combination with, anions. In this instance, the role of 

a coverage dependent alloying–dealloying transition is 

being examined with an eye towards understanding both 

surfactant and solute trapping effects. These processes 

are important in the production of alloy for applications 

ranging from microelectronics to fuel cell catalysts to 

biosensors. 

Figure 1: A time sequence (right to left) of in-situ (70 nmx 

70 nm) STM images of Pb deposition (bright contrast) at step 

edges on a chloride covered Cu(100) surface. 

In addition to our electroanalytical studies, pulse 

potential deposition is also being used to synthesize 

strained-layer superlattices of Co/Cu on semiconductors. 

In particular, ferromagnetic /semiconductor junctions 

are of interest for spin injection and detection in 

semiconductors. Interface structure is thought to 

play a critical role in the efficiency of spin transmission 

although limited experimental data exist. In the past year, 

we have examined the structure and magnetic properties 

of electrodeposited Co films on (001) n-GaAs. The 

films exhibit a strong hcp Co(1120)[001]||GaAs(001) 

[110] texture which is mediated by a thin interfacial 

bcc-Co phase. 

Figure 2: A thin metastable bcc Co film electrodeposited 

on GaAs with a cube-on-cube epitaxial orientation. 

The results of this project have led to a new project 

in FY2003 to be focused on using in-situ STM 

techniques for characterizing the surface reactivity of 

immersed interfaces relevant to biological and electronic 

device design. 

Contributors and Collaborators 

J.E. Bonevich, R.D. McMichael, M. Vaudin, A. Ford 

(NIST/SURF); J. Mallett, W. Schwarzacher (Fulbright 

Scholar from University of Bristol) 

22 
Advanced Manufacturing Methods


Instrumented Consolidation of Amorphous Powders


Recent developments in production of amorphous 

materials have resulted in a class of iron- and 

aluminum-based powders that exhibit plastic behavior 

in the absence of dislocations. Potential applications 

for these materials have motivated industrial interest in 

consolidating the powders into parts. The Metallurgy 

Division is using instrumented consolidation with 

warm gas and liquid phase pressurizing media to 

understand the kinetics of densification of noncrystalline 

materials, avoiding the deleterious effects of hot 

pressing or sintering that would cause crystallization. 

Stephen D. Ridder and Richard J. Fields 

Amorphous metallic alloys have been known for 

many years, but they have been mainly an academic 

curiosity. Attempts have been made to use them 

industrially, but most of these have met with failure. 

Recently, Boeing has identified a class of amorphous 

materials based on aluminum which may be used in 

airframes. This class of materials also includes an ironbased alloy. Some of these alloys can only be produced 

as powders. To use them, it is necessary to consolidate 

them without crystallization or with carefully controlled 

fine crystallization. An interesting feature of these 

amorphous alloys is that they can be deformed plastically 

despite the absence of dislocations. The phenomenon 

behind this behavior is unknown, although the hypothesis 

of Spaepen and Turnbull {Scripta Met. 8, 563 (1975)} 

seems applicable. In any case, the ability to deform 

plastically suggests that pressure would be effective 

in consolidation. We have shown that to be the case 

(Figure 1). To understand the densification behavior 

of these materials, a project was initiated to study the 

kinetics of consolidation by pressure and heat below 

the crystallization temperature. 

Figure 1: Micrograph of pressed amorphous aluminum 

alloy showing plastic yielding of powder particle contacts. 

This compact attained a relative density of about 80%. 

Several approaches are being pursued. The hot 

isostatic press (HIP) has been instrumented with 

the sensor developed at NIST to follow densification 

(Figure 2). The warm isostatic press that uses a liquid 

ester and can be pressurized to twice the pressure of 

the HIP is also being instrumented with another density 

sensor developed at NIST. These two units provide 

quantitative, real time monitoring of the progress of 

densification (Figure 3). Relative densities of more than 

86% have been obtained using these methods. 

Figure 2: Schematic diagram of NIST’s eddy-current 

based density sensor for in-situ monitoring of hot isostatic 

pressing. 

Figure 3: The instrumented HIP provides continuous 

information about the applied temperature, pressure, and 

resultant density of the sample as shown by this record. 

It is also intended to investigate the use of dynamic 

consolidation, and electric field and current assisted 

consolidation to break down the oxide that is usually 

present on these powders. This surface oxide is a great 

hindrance to effective consolidation. The Kolsky Bar 

Facility, discussed in the project report on High Speed 

Machining, will be used for this effort. 

Contributors and Collaborators 

F. Biancaniello, R. Jiggetts, T. Pierce, T. Zahrah 

(MatSys); R. Rowland (MatSys); M. Blackburn 

(University of Connecticut); D. Bowden (Boeing); 

L. Christodoulou (DARPA) 

23 
Program Overview


Combinatorial Methods


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 

24 
Combinatorial Methods


Combinatorial Materials Research: 

Interconnects to Optoelectronic Materials 

GaN and related nitrides have been identified as 

important materials for the realization of solid-state 

lighting, UV/blue lasers, LEDs and photodetectors. 

The engineering of improved electrical contacts to 

these devices is of particular industrial importance. 

This project develops a strategy for industry to reduce 

contact resistance, increase visible light transmittance, 

and improve thermal and mechanical stability of ohmic 

contacts to a variety of optoelectronic devices. Due to 

the large number of possible materials combinations 

and process variables involved, a combinatorial 

approach is valuable. 

Albert V. Davydov and Leonid A. Bendersky 

Typical electrical contacts to p-type GaN devices 

consist of thin film Au/Ni bi-layers, but contact 

resistance and reliability are far from ideal. The goal of 

this project is to establish techniques for industry to use 

to rapidly develop improved contacts for GaN and other 

compound semiconductor devices. A combinatorial 

approach (looking at Au/Ni ratio and metal film 

thickness) integrated with thermodynamic and diffusion 

modeling is being used to quantify the relationship 

between physical properties such as electrical resistance 

and optical transmittance of metal contacts and the 

fundamental microstructural and compositional 

properties of the metal-to-GaN interface. 

Thermodynamic information and diffusion data 

are being evaluated for the Au-Ni-Ga-N system to help 

interpret the metallurgical reactions in the Au/Ni/GaN 

structures. To date, we have measured the thermal 

stability of the GaN compound and modeled the 

P-T-composition phase diagram for the Ga-N system. 

In addition, the Ni-Ga-N phase diagram has been 

evaluated experimentally and thermodynamically and 

presented at the CALPHAD-2002 Meeting. 

A combinatorial array of Ni/Au bi-layer contacts of 

varying compositions has been fabricated by physical vapor 

deposition (e-beam evaporation) on commercial GaN 

wafers. The thickness of each metal layer varied discretely 

from 5 to 85 nm using a motion-controlled shutter system, 

producing an array of 88 elements (Figure 1(a)). The 

composition and microstructure of the contacts were 

examined with XRD (with Prof. I. Takeuch, UMD), optical 

microscopy, SEM and AFM. The transparency of metal 

layers to visible light was determined by reflectometry and 

transmission measurements. From transmission and XRD 

measurements (Figure 1b, c), we have identified library 

elements with optimum as-deposited Au/Ni compositions 

that are highly transparent and of good crystalline quality 

with epitaxial metal layers. 

In FY2003, we will fabricate combinatorial 

libraries with an extended compositional range to 

develop thermodynamic stability data for GaN with 

other metal contact materials as well as continue to 

establish the analysis techniques for quantifying phase 

transformations and interdiffusion in these GaN/metal 

contact systems and developing the relationships 

between phase transformations, microstructures, 

and electrical performance. 

Figure 1: (a) Array of as-deposited Au/Ni bi-layered 

metallization (88 elements) on 2-inch GaN/sapphire wafer; 

(b) Optical transmission imaging of the above sample at 

l = 450 – 713 nm; (c) XRD mapping of Au 111 reflection 

from all 88 Au /Ni elements. 

Contributors and Collaborators 

W.J. Boettinger, D. Josell, A.J. Shapiro (Metallurgy 

Division, MSEL); P.K. Schenck, J.E. Blendell (Ceramic 

Division, MSEL); I. Takeuchi (University of Maryland); 

V.A. Dmitriev (Technologies and Devices International, Inc.) 

25 
Combinatorial Methods


Combinatorial Methods for Thin Films


In the search for materials for use in high-performance 

communication technologies, complex oxide phases 

with various chemistry and structural states are 

under consideration. With the relatively new ability 

to measure dielectric and magnetic properties locally, 

combinatorial methods can be used to create miniature 

thin film assays designed to either search for 

compositions with an optimal set of physical properties 

or study fundamentals of the relationship between 

crystallo-chemistry and physical properties, e.g., electric 

polarization or magnetic ordering in complex oxides. 

Leonid A. Bendersky 

The effectiveness of the combinatorial approach 

to thin film electronic materials has recently been 

demonstrated. In this approach, in order to rapidly 

survey a large compositional landscape, combinatorial 

assays with continuously changing compositions are 

synthesized, processed, and measured in a single 

experiment. Dielectric, magnetic and other physical 

properties of the compositional spreads can be 

measured by using recently developed instruments with 

high spatial resolution, such as microwave microscopes 

and microSQUIDs. 

This project involves a close collaboration with the 

laboratory of Dr. I. Takeuchi (University of Maryland) 

where the combinatorial assays of oxide thin films are 

prepared by shutter-controlled pulsed laser ablation. 

NIST efforts are focused on detailed structural 

characterization of critical samples using transmission 

electron microscopy (TEM). Such characterization 

provides knowledge essential for understanding the 

deposition process and the correlations between physical 

properties and local microstructures. 

We have investigated BaTiO3-SrTiO3 spreads in 

order to find correlations between microstructural 

defects and measured local dielectric properties. 

These materials have important properties suitable for 

tunable microwave devices. In our work, we identified the 

presence of a high density of planar defects in thin film 

layers adjacent to the substrates. Careful high-resolution 

TEM and electron energy loss spectroscopy (EELS) 

mapping and simulation of contrast established that 

the defects belong to 1/2<110> non-conservative 

stacking faults with a double layer of TiO6 octahedra. 

Such defects result from the specifics of island growth, 

substrate/film mismatch and deviations from the 

Ba/Ti=1 stoichiometry. 

The ZnO-MgO system also exhibits a compositional 

spread in thin film form where a tunable bandgap is 

obtained by doping the semiconductor ZnO (bandgap 

3.3 eV) with MgO (bandgap 7.8 eV). Potential 

applications are in optical devices, including UV lasers, 

as well as transparent conducting layers for solar cells 

and phosphors. Epitaxial spreads were comprehensively 

studied for UV transmission and for microstructure by 

scanning microdiffractometer and TEM. The results 

show a continuously changing bandgap thereby allowing 

the material to be considered for an array of photodetectors 

with a range of detection frequencies separately active at 

different locations on the patterned film. 

In another facet of this project, a new method of 

rapid determination of ferromagnetic phase boundaries 

has been developed and used to examine composition 

gradients in thin films of LaMnO3-CaMnO3, a material 

which has attracted a great deal of attention for a strong 

colossal magneto-resistance effect. A high-resolution 

magneto-optical imaging technique was used to image 

stray magnetic fields at the edge of ferro/ferrimagnetic 

phases, thus directly visualizing phase boundaries in a 

temperature-composition space (Figure 1). The first 

application of the method has demonstrated its efficiency 

and accuracy as a combinatorial screening tool. 

Figure 1: (a, b) Schematic drawing showing the formation 

of a black /white pair of lines outlining boundaries of a 

ferromagnetic phase; (c) an experimental T-C diagram of a 

ferromagnetic phase in a thin film form; (d) diagram of the 

(La,Ca)MnO3 system obtained for bulk ceramics. 

Contributors and Collaborators 

L.A. Bendersky, C.J. Lu, R. Parke, M. Turchinskaya 

(MSEL); J.H. Scott (CSTL); I. Takeuchi, K.S. Chang 

(University of Maryland) 

26 
Program Overview


Data Evaluation and Delivery


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 

27 
Data Evaluation and Delivery


Reaction Path Analysis in Multicomponent Systems


Many commercial processes rely on multicomponent 

diffusion to control the formation and dissolution of 

precipitate phases within the matrix phase or at 

an interface. Development of a diffusion mobility 

database provides an efficient method to store a

wealth of diffusion data and enables the means to 

extrapolate the available data to higher-order systems. 

The developed Ni-based diffusion mobility database 

enables the modeling of a variety of processes, 

including non-isothermal precipitation of γ ́, heattreatment optimization, solidification, transient liquid

phase bonding, and coating applications. 

Carelyn E. Campbell and William J. Boettinger 

Multicomponent diffusion is important in many 

industrial processes, especially in the processing 

and application of Ni-based superalloys. An a priori 

understanding of diffusion-controlled microstructures 

would allow the optimization of heat treatments that 

avoid incipient melting and the prediction of freezing 

temperatures and solidification paths for Ni-based 

superalloys. All of these processes require the use of a 

diffusion mobility database to describe the compositiondependent diffusion coefficients. 

Diffusion Mobility Database 

Concentration-dependent diffusion coefficients in a 

multicomponent system are defined as the product of a 

thermodynamic factor and a mobility term. The NIST 

composition-dependent mobility database is constructed 

using an approach, which assumes that quaternary and 

higher order interactions are negligible. Thus, binary and 

ternary effects can be combined to extrapolate to higher 

order systems. For the Ni-Al-Cr-Co-Fe-Hf-Mo-Nb-ReTa-Ti-W system, a diffusion mobility database has 

been constructed for the γ (disordered FCC) phase. 

The current database includes only binary interactions. 

The development of this diffusion mobility database was 

published in Acta Materialia in 2002 where it is readily 

available to industry. General Electric Corporate Research 

and Development (GE-CRD) and Howmet Corporation 

provided results from multicomponent diffusion couples, 

which were compared with diffusion simulations. The 

experimental and calculated diffusion composition profiles 

for the Rene-N4/Rene-N5 diffusion couple agree quite 

well (Figure 1). The predicted location of maximum 

porosity also compared favorably to the observed pore 

formation. Figure 2 shows a back-scatter image of the 

100 h sample and the location of the predicted porosity. 

Results from this couple and other multicomponent 

diffusion couples are evaluated and used to refine the 

current diffusion mobility database. 

Applications 

As a part of a General-Electric-led DARPA/AIM 

project, the γ ́ precipitation process is being numerically 

modeled by, team member, Questek Innovations. This 

model requires inputs of equilibrium chemical potentials 

of γ and γ ́, the composition dependent diffusivity in the γ

matrix, γ and γ ́ lattice parameters, and interfacial energy. 

NIST has provided Questek with an electronic version of 

the diffusion database to calculate the necessary diffusion 

coefficients. NIST has also initiated an effort to develop 

heat treatment optimization techniques to address 

industry’s need for more efficient heat-treating practices 

of cast Ni-based superalloys. The ideal heat treatment of 

a cast Ni-base superalloy consists of a heating schedule 

that avoids incipient melting while minimizing either the 

power expenditure or the heating time to achieve a 

homogeneous single phase structure. 

Figure 1: Calculated (solid lines) and experimental 

(symbols) composition profiles for the Rene-N4/Rene-N5 

diffusion couple at 1293oC for 100 h. 

Figure 2: Back scatter image of Rene-N4/Rene-N5 after 

100 h at 1293oC. Thin white line indicates the position of 

microprobe scan. The dashed white line corresponds to the 

Matano interface. The dashed black line is the location of 

the predicted maximum porosity. 

Contributors and Collaborators 

U.R. Kattner, B. Mueller, T. Hansen (Howmet Corp.); 

J.C. Zhao (GE-CRD); T. Helander (Thermo-Calc Software 

AB); C. Kuehmann, H. Jou (Questek Innovations); 

Z.K. Liu (Penn State); G. Ghosh, D. Seidman, 

P. Voorhees (Northwestern University) 

28 
Data Evaluation and Delivery


Thermodynamic Databases for Industrial Processes


Many industries that process and use metals, from 

microelectronics to aerospace, need data for complex 

alloys (three or more components). The number 

of images that would be needed for graphical 

representation of these data is prohibitively large. 

Thus the development of thermodynamic databases 

that permit extrapolation of binary and ternary 

systems to higher order systems is needed. Access 

to these databases through an internet site with 

interactive software tools will allow the user to 

retrieve the needed phase diagram information. 

Ursula R. Kattner 

I

n order to deliver materials data efficiently to the end 

user, it is important to present technical data in a 

concise but useful form, and utilize the interactive 

medium that the worldwide web offers for their retrieval. 

Downloaded databases and software for thermodynamic 

calculations are efficient for regular, expert users but 

are cumbersome for the occasional, less expert user. 

Retrieval of data through direct interaction with software 

on the server may be convenient for the occasional 

user, but may slow server responses significantly. 

The challenge is to develop interactive software for the 

potentially large set of non-expert users with sufficient 

versatility to allow complicated technical questions to 

be answered, sufficient speed to make the calculations 

efficient, and sufficient interpretation to allow the user 

to properly use the information. 

A workshop on “Databases for Computational 

Thermodynamics and Kinetic Modeling” was organized. 

The approach of the workshop was to identify the 

database and information delivery tool needs of industry 

and education. The anticipated benefits from extended 

modeling and simulation capabilities are cost savings, 

improvements in environmental quality and energy 

conservation. Roadmaps were developed for how these 

needs can be met through expanded collaborative efforts 

in education, basic research and database development 

within the next decade. 

The thermodynamic databases developed in this project 

were used to generate phase equilibria data on the web 

pages in the form of phase diagrams. In addition, the 

thermodynamic databases are available in the form of 

downloadable files which can be processed into customized 

output by user software or by specialized software 

developed by us and downloadable from our website. 

The phase diagram website provides links to the 

NIST mechanical properties internet site allowing the 

user to examine the mechanical properties data that are 

available for the material. 

The following information has been added on the site 

www.metallurgy.nist.gov/phase/: 

■ A link to the file with the thermodynamic 10 

component database (Ni-Al-Co-Cr-Hf-Mo-Re-Ta-TiW) for superalloys with descriptions of liquid, γ (fcc) 

and γ ́ (L12) phases. 

■ A series of pages with binary phase diagrams for 

solder alloys. The binary systems are: Ag-Bi, Ag-Cu, 

Ag-Pb, Ag-Sb, Ag-Sn, Bi-Cu, Bi-Pb, Bi-Sb, Bi-Sn, 

Cu-Pb, Cu-Sb, Cu-Sn, Pb-Sb, Pb-Sn and Sb-Sn. 

■ A series of pages with ternary phase diagrams 

solder alloys with Sb. Each page contains a 

calculated liquidus projection for Sn-rich systems, 

enlargement of the Sn-rich corner, and a table of the 

invariant reactions in this system. The ternary systems 

are: Ag-Bi-Sb, Ag-Cu-Sb, Ag-Pb-Sb, Ag-Sb-Sn, 

Bi-Cu-Sb, Bi-Pb-Sb, Bi-Sb-Sn, Cu-Pb-Sb, Cu-Sb-Sn 

and Pb-Sb-Sn. 

■ Tutorial pages that illustrate the usage of phase 

diagram information. Examples are given for different 

cases with solidification following the lever rule 

equilibrium and Scheil path. 

■ Links to scripts for the simulation of DTA curves. 

Future work will include the development of 

easy-to-use interfaces for the task-specific software 

that will be posted either for interactive use or 

downloads on the web site. 

Figure 1: Calculated Sb-Sn phase diagram. 

Contributors and Collaborators 

W.J. Boettinger, R.J. Fields, J.E. Bonevich, 

K.-W. Moon 

29 
Data Evaluation and Delivery


Mechanical Properties of Metals and Alloys on the Internet


With the increased use of the Internet, being able 

to electronically access critically evaluated data 

pertaining to the mechanical properties of materials 

has become more important to the U.S. industry. 

This information is required for the material selection 

or computer simulation using finite element methods 

during key stages of the design process. During this 

past year, we have concentrated in developing the 

necessary infrastructure to easily deliver the vast data 

generated or evaluated in the Metallurgy Division in 

a coherent searchable manner. 

Richard J. Fields and Carlos R. Beauchamp 

Mechanical properties are used to predict the 

performance of metallic components during 

fabrication and in service. There is a great abundance 

of mechanical properties data, but access to this data 

by traditional literature searching is a time consuming, 

inefficient, and costly process. More and more scientists 

and engineers representing the full range of U.S. 

industry, academia, and government agencies search for 

data electronically almost to the exclusion of print media. 

This project intends to provide a special site for NIST 

generated or evaluated data, a portal to other sources 

of data, and an easily adaptable interactive site that will 

address more precisely the needs of specific industrial 

communities. 

To this end, collaboration between NIST and Granta 

Design Limited, United Kingdom, has yielded a materials 

property database that is in the pilot stages for access 

through the Metallurgy Division web homepages. 

Included in the database are: 

■ Mechanical and physical properties of solder alloys, 

including the results from three national consortia on 

lead-free solders for microelectronics applications; 

■ Mechanical and physical properties of solder joint 

intermetallics formed between tin and copper or nickel. 

Hardness and toughness of these alloys as a function 

of temperature as well as other room temperature 

properties are included; 

■ Mechanical property data forming the basis of constitutive 

equations for deformation of metals and alloys; and 

■ Deformation maps showing transitions in mechanisms 

with temperature, grain size, and other properties 

(Figures 1 and 2). 

Collaboration is continuing with Professor H.J. Frost 

of Dartmouth to develop an online access to the high 

information density of deformation mechanism maps. 

These maps not only include most available data for a 

given material, but also provide constitutive equations 

that permit calculation of behavior in regions of stress 

and temperature of interest to the user but where no 

data exist. This combination of deformation maps 

and constitutive equations will be a powerful tool for 

scientists and engineers to model and quantify the 

effects of microstructure, fabrication processes and 

use conditions on mechanical performance. 

Figure 1: Stress versus temperature map for 304 

stainless steel with 50 μm grain size. 

Figure 2: Strain rate versus temperature map for 304 

stainless steel with 100 μm grain size. 

Contributors and Collaborators 

C.A. Handwerker, U.R. Kattner, J. Bonevich, 

R. Brown, H.B. Gates, S. Tobery (NIST/MSEL); 

H.J. Frost (Dartmouth College) 

30 
Data Evaluation and Delivery


Electrodeposited Coating Thickness Standards


For over 50 years, NIST has been providing the 

coating industry with electrodeposited coating 

thickness Standard Reference Materials (SRMs). 

These standards are used for the calibration of 

instruments that measure coating thickness using 

magnetic methods. This year, the Metallurgy Division 

has extended their customary services of providing 

the standards and their periodic verification to include 

the preparation of a recommended practice guide for 

their proper use. 

Carlos R. Beauchamp 

The Electrochemical Processing Group has played 

an important role in the development of magnetic 

methods for the measurement of coating thickness. 

In the mid 1940’s, research at this institution made 

possible the development of instruments for the 

measurement of magnetic coatings over non-magnetic 

substrates and non-magnetic coatings over magnetic 

substrates based on the magnetic attraction principle. 

The instrumentation measured the force of attraction 

between a magnet and the magnetic material. It quickly 

became a principal tool in the measurement of the 

coating thickness due to the ease of use, simplicity of 

the method, and the wide range of coating/substrates 

that could be measured by the method. The involvement 

was not limited to the development of the technique 

since the Institution has been providing standards for 

the calibration of such instrumentation ever since the 

wide acceptance of the method. 

Although the instrumentation has evolved since its 

first appearance and new magnetic techniques are now 

employed, the use of the standards has essentially 

stayed the same. The standards provided by NIST 

consist of pre-configured sets of electrodeposited 

copper over low carbon steel substrate coupons with 

the coating thickness ranging from 6 μm to 2000 μm. 

The coatings are overplated with chromium, and the total 

coating thickness is certified. The maximum expanded 

uncertainties for these standards are 2% of the mean 

coating thickness over the surface of the coupon. 

Modern electronic gages have made the 

measurement extremely simple. The operator places a 

handheld probe in contact with three or four different 

standards, provides the certified values for the known 

coating thickness, and then proceeds to repeat the 

contact process on the location to be measured. 

The simplicity of the process masks potential 

problems that will arise during the process of obtaining 

the measurement. Factors such as mismatch of the 

composition or thickness of the substrate between the 

known and the unknown, curvature of the part being 

measured, proximity to edges or other part nonuniformity, roughness of the deposits, or type of 

calibration curve applied over the span of thickness 

being measured are usually paid little attention, if any, 

during the process of measurement. Such problems 

will usually create confusion amongst our customers 

when they try to match the values certified in our 

standards. 

To help them understand the extent of the 

effect of such factors over their measurement 

process, a publication has been prepared. The NIST 

Recommended Practice Guide — Using Magnetic 

Methods for the Measurement of Coating Thickness 

covers such issues by explaining the source of the 

effects and presents example data demonstrating the 

extent of the effects. Suggestions on how to account 

for such effects are presented. 

Figure 1: Effect of the substrate on the measurement of 

the coating thickness: the thinner the coating, the higher 

the scatter of the collected data for the same foil thickness. 

Contributors and Collaborators 

H.B. Gates, D.R. Kelley (NIST/MSEL); 

S.D. Leigh (NIST/ITL) 

31 
Program Overview


Forming of Lightweight Material for Automotive Applications


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 

32 
Forming of Lightweight Material for Automotive Applications


Plasticity, Fabrication Processes, and Performance


Inaccurate predictions of large strain plasticity 

under complex load histories such as those applied 

during industrially relevant processes are due to our 

limited understanding of the essential role played by 

microstructure. Significant advances in theoretical 

and modeling capabilities that include microstructure, 

and guided by experimental measurements and 

validation, are needed to shed new light on this 

problem. For example, NIST’s OOF modeling 

program is severely limited by its inability to deal 

with plasticity. Remedying this is one of the principal 

challenges of this project. 

Richard J. Fields 

Diffraction provides a powerful means of very 

accurately measuring both microstructure and 

mechanical behavior in a way that provides insight 

simultaneously into both and offers particular 

opportunities for understanding plasticity. This project 

is implementing one or more plasticity models in OOF 

and devising critical experimental and computational 

benchmarks to validate OOF using the NCNR’s neutron 

diffractometer to measure residual stress, texture, and 

elastic properties. Conventional x-ray sources are also 

being used where stress states measured at or near 

surfaces are important for understanding the behavior of 

materials or to compare with predictions. Synchrotron 

x-rays are used to deal with sub-surface residual 

stresses in the thin, highly-textured samples that result 

from simulated forming operations. Specifically, the 

following tasks are underway: 

■ Efforts to include plasticity in OOF and extend 

OOF to three-dimensional microstructures are being 

undertaken by continuing and expanding our current 

theory group meetings on these topics. Academic 

experts in this area are brought in to make sure our 

internal group is attacking these problems with the 

most up-to-date methods. Modification of the OOF 

program to include plasticity will involve the CTCMS 

staff currently working on OOF. The Metallurgy 

Division will supply them with algorithms for the 

code based on different types of plasticity. 

■ The effects of residual stresses, produced by heat 

treatment or initial machining, on distortion during 

subsequent machining steps are being established for 

prototype aluminum samples by neutron and x-ray 

diffraction to validate on-going calculations. (This part 

of the project includes collaborative contributions from 

MEL, Alcoa, and Boeing Corp.) 

Once plasticity has been implemented in OOF, 

additional verification tests will be carried out against 

analytical models and ABAQUS. Validation tests will be 

carried out against benchmark experiments run at the 

NCNR and in the Metallurgy Division. An effort to 

include some simple 3-D character to OOF based on 

stereology may be included in this part of the research. 

Accomplishments 

■ Installed a state-of-the-art goniometer on an x-ray 

source at NIST. 

■ Established a NIST access to residual stress 

measurement at the Advanced Photon Source and 

characterized the residual stress state in a standard 

Demeri cups supplied by Ford. 

■ Developed a research plan with Boeing and Alcoa to 

minimize machining distortion. 

■ Derived an analytical expression for the elastic behavior 

of polycrystalline materials to verify the performance of 

OOF. 

■ Collaborated with CTCMS staff to develop algorithms 

for a simple plasticity model for OOF. 

Figure 1: Residual stress measurement in Demeri cup at 

Advanced Photon Source. 

Impact 

This project has targeted a need expressed by 

numerous companies to extend OOF calculations into 

the plastic range. It is also responsive to the metal forming 

research needs of the auto industry, as well as Boeing, 

Alcoa and steel manufacturers with whom NIST currently 

collaborates. Improvements in predicting large plastic 

strain behavior under complex loading conditions will 

have significant benefits on product differentiation, timeto-market, and the cost of forming dies for U.S. products. 

Contributors and Collaborators 

Lyle Levine, Roland deWit (Metallurgy); Henry Prask, 

Thomas Herold, Vladimir Luzin (NCNR); Robert Polvani 

(MEL); David Bowden (Boeing); Edmund Chu (Alcoa); 

Robert Reno (University of Maryland); Lily Ma (Drexel) 

33 
Forming of Lightweight Material for Automotive Applications


Standard Test Method Development for Sheet Metal Formability


In order to meet the PNGV goals for fuel efficiency, 

the U.S. automotive industry is moving to lighter, 

high-strength materials for auto bodies. However, lack 

of experience in forming these materials translates 

into difficulty in making accurate dies for producing 

body parts. NIST’s survey of the industry has found 

that accurate material properties, and a way to 

incorporate them into finite element models of sheet 

metal forming dies, is a critical need for the U.S. auto 

industry. This project seeks to develop new standard 

tests and metrology to accurately determine sheet 

metal mechanical response under forming conditions. 

Timothy J. Foecke 

I

n order for the U.S. automotive industry to be able 

to transition to new materials for formed sheet metal 

parts, the starting materials must be mechanically 

characterized under various forming conditions. These 

data can then be used as input for die design models. 

The Metallurgy Division has initiated a project to develop 

a sheet metal formability test, along with associated 

metrology, that can be standardized and easily used 

by industry to accomplish this task. 

Springback is the elastic shape change to a part 

associated with the residual stresses that develop 

during the stamping process. This deviation in form 

complicates assembly and accurate fit-up resulting in a 

strong desire by the automotive industry to either avoid 

it or at least be able to predict its magnitude to account 

for it in die design. 

In conjunction with members of the U.S. Council 

for Automotive Research (USCAR), efforts this year 

have concentrated on the Demeri cup springback test. 

The driving force for standardization of this test is its 

simplicity in terms of tooling, measurement techniques, 

and basic understanding of the data. In this test, a 

circular blank is drawn into a flat bottom cup. The 

sidewalls of the cup undergo a stretch-bend deformation 

path that introduces large residual hoop stresses. 

A ring is cut from the sidewall and split to produce 

a large and measurable elastic opening as shown in 

Figure 1. Insights gained in writing finite element codes 

to calculate springback in this simple body can then be 

applied to codes used to design more complex dies. 

As part of a collaboration with Ford Motor Company, 

Fe- and Al-base samples are sent to NIST for inspection 

and measurement. While this test has several desirable 

attributes from a modeling perspective, such as 

axisymmetry, a number of experimental issues with this 

geometry have been found that complicate the analysis. 

As seen in Figure 2, the wall thickness varies around 

the perimeter of the cup. This was expected as the 

Figure 1: Split ring from Demeri cup springback test. 

mechanical behavior of the sheet varies with respect to 

the rolling direction, affecting how the material flows 

into the tooling. In addition, it was also seen that the 

thickness varies along the height of the sidewall, 

consistent with the fact that more material is being 

drawn at the end of the process than the beginning. 

Figure 2: Plot of wall thickness around perimeter of cup. 

Preliminary measurements of the stress in the ring 

prior to cutting have been made at the Advanced Photon 

Source and are consistent with initial predictions that the 

stresses are not linear through the thickness, as 

assumed by the models, but inflected in a complicated 

manner. This work is being expanded since it is of great 

interest to the forming industry. 

Contributors and Collaborators 

S.W. Banovic; T. Gnaeupel–Herold, H. Prask (856); 

M. Demeri (Ford); C. Xia (U.S. Steel); E. Chu (ALCOA) 

34 
Forming of Lightweight Material for Automotive Applications


Microstructural Origins of Surface Roughening


and Strain Localizations 

Existing data, measurements methods, and the basic 

understanding of metallurgical factors that influence 

friction, tearing, and surface finish during sheet metal 

fabrication are insufficient to meet the finite element 

modeling requirements of the automotive industry. 

This project approaches the resultant need by 

exploring the microstructural origins of the distribution 

of slip, surface roughening, and strain localization 

during plastic straining. Influence of initial material 

characteristics on the formability of Al and Fe base 

sheet metals as a function of biaxial deformation is 

the primary focus of the investigations. 

Stephen W. Banovic 

Replacement of conventional steel sheets by aluminum 

alloys and high-strength, low-alloy steels for various 

automobile closures is an effective means of reducing vehicle 

weight. However, wide-spread application of these metals 

by the automotive industry is limited due to formability 

issues related to a lack of experience with these new alloys. 

In addition, finite element modeling of new die designs has 

been hampered due to deficiencies in their inputs (existing 

materials databases) and the basic understanding of how 

metallurgical factors influence the resulting behavior of the 

material. Therefore, this project examines the underlying 

structure–property relationships associated with formability 

in an attempt to further numerical simulations that predict 

deformation behavior of materials. 

The main concentration of this past year was to 

develop and/or improve upon the understanding of the 

measurement techniques being utilized. Past measurements 

of the strain-induced surface roughness were conducted 

using a contact stylus profilometer. This technique 

was found to be labor intensive and yielded limited data. 

A new laser confocal microscope has been obtained that 

will allow for the automated, rapid sampling of large 

areas, as well as produce line traces across an area of 

interest. It is expected that pre-programmed routines 

will soon be measuring samples at a high throughput to 

increase accuracy of the measurements and improve the 

statistics of the data. 

Changes observed in the surface roughness due 

to plastic deformation have been correlated with the 

modification in crystallographic texture of the sheet. 

Three techniques are presently being used to measure 

this evolution, with each technique analyzing different 

sample volumes. The bulk measurement technique is 

Neutron diffraction (ND) which analyzes numerous 

pieces of sheet stacked on top of one another to 

produce a sample volume of approximately 125 mm3. 

The method of X-ray diffraction (XRD) probes the 

top 2–3 grain layers over a 1 cm2 area yielding data 

from roughly 5 mm3. The final technique is electron 

backscatter diffraction (EBSD), which is used to analyze 

approximately 10 nm of the surface layer. Assessment 

of these different systems is currently underway as each 

technique has advantages and drawbacks. An example 

of these comparisons is show in Figure 1 for a 5xxx 

series aluminum alloy. These results indicate that the 

crystallographic textural development is similar at the 

surface of the sheet as it is throughout the bulk, even 

though constraint of the exterior grains is relaxed at the 

free surface. Further analysis is being conducted to 

quantify these comparisons. 

Figure 1: Pole figures for AA5052-H32 deformed in a 

balanced biaxial mode to a strain level of 0.104. 

Future work will focus on surface roughness 

development and crystallographic texture evolution of 

samples deformed via multi-pass strain paths in attempts 

to simulate actual stamping operations. Transmission of 

this information to the technical community will be performed 

through the electronic databases of mechanical properties 

and material characteristics as a function of strain level 

made available on the NIST website. In addition, a 

workshop will be used to help introduce the work and 

identify the critical microstructural variables that are 

important to improving formability. 

Contributors and Collaborators 

T. Foecke, M.R. Stoudt, R.E. Ricker, D. Dayan; 

M.D. Vaudin, T. Gnaeupel-Herold, V. Luzin (NIST/ 

MSEL); W. Tong (Yale University); Y. Shim (University 

of Georgia) 

35 
Forming of Lightweight Material for Automotive Applications


Underlying Processes of Plastic Deformation


A substantial increase in the use of aluminum 

alloys and high-strength steels in automobiles would 

greatly increase fuel efficiency. The primary reason 

why this has not yet been done is a lack of accurate 

deformation models for use in designing the stamping 

dies. This project is developing a physically based 

model of plastic deformation using a combination 

of statistical physics approaches and advanced 

measurement techniques. 

Lyle E. Levine 

Plastic deformation of metals (as in cold rolling, 

stamping, drawing, extruding, and metal fatigue) 

is a topic of great importance to industries worldwide, 

and improvements in the basic technology would have 

a significant effect on our economy. As one example, 

stamped metal parts comprise about 1/3 of the weight 

of an automobile. If the currently used mild steel could 

be replaced by aluminum alloys or high-strength steels, 

weight could be reduced considerably, thus greatly 

increasing fuel economy. 

The design of new metal products is often 

accomplished by computer simulation of the production 

process using empirically derived constitutive equations. 

Unfortunately, existing constitutive equations cannot 

accurately predict the material behavior, and many 

tryout and redesign steps are required. Another related 

difficulty is in the design of new alloys with improved 

formability characteristics. Currently, alloy design is 

done empirically with little understanding of how the 

various constituents affect the mechanical properties. 

To address both of these issues, this project is 

focused on developing constitutive laws based upon the 

underlying physical processes that produce the observed 

mechanical behaviors in metal alloys. Such constitutive 

laws are inherently multi-scale since they must not 

only incorporate the atomic scale interactions in metal 

alloys but also contain transitions all the way from the 

atomistic to the macroscopic stress–strain behavior of 

bulk material. 

Almost all of the changes in mechanical behavior that 

occur during deformation result from the transport of 

dislocations. The most difficult aspect of this problem 

is in the mesoscale, where large numbers of dislocations 

interact to form complex three-dimensional structures 

that both impede the motion of mobile dislocations and 

act as sources for new dislocations. Several years 

ago, we introduced a statistical physics model for this 

process called strain percolation theory. The model 

successfully described how dislocations propagate 

through dislocation structures but the connection to 

the smaller-length-scale physics remained tenuous. 

In a major development over the past year, advances 

in our understanding of how strain is produced and 

transmitted during deformation has allowed us to make 

a firm connection to the smaller-length scales and to tie 

many apparently disparate phenomena together into a 

single theoretical framework that we call the segment 

length distribution model. The basic mechanism 

involves the interaction of the local and applied stress 

fields with the distribution of dislocation segments 

within dislocation walls. The evolution of this 

distribution directly determines the changes in the 

mechanical properties and it is strongly affected by 

the applied strain, stress, strain rate, temperature 

and alloy chemistry. Physical features such as 

vacancy concentration, diffusion rates, strain rates, 

and dislocation densities on the various slip systems 

can all be included directly. Although it is now clear 

how all of these features can be added to the model, 

much work remains to complete this. 

The explicit incorporation of these (largely) 

atomistic-level details means that chemistry effects 

can be addressed directly. Such work should allow 

quantitative predictions to be made of the effects that 

different alloying elements would have on the mechanical 

behavior. The role of chemistry comes in naturally, and 

this is expected to be a significant new research topic in 

the next fiscal year. 

A key observation that underlies most of our 

theoretical work is that slip is heterogeneous in both 

space and time. The strain percolation theory and 

segment length distribution model provide handles for 

addressing the time aspect and the spatial heterogeneity 

at short-length scales. An unresolved question is how 

the strain becomes localized (into slip bands) over larger 

length scales. This process is crucial to completing a 

physically-based constitutive law for single crystals. 

During the past year, we completed an experimental 

effort aimed at providing crucial input into our theory 

work on this topic. Numerous single-crystal Al samples 

were grown with different crystallographic orientations. 

After straining, the underlying dislocation structures 

were examined using transmission electron microscopy. 

Other identical specimens were strained incrementally in 

an atomic force microscope, and the resulting formation 

and evolution of slip lines and bands was measured as 

a function of strain and crystallographic orientation. 

Interpretation of these data is ongoing. Once the 

localization process is understood, we will have 

developed fully coupled models ranging from the 

atomistic scale up through the single crystal level. 

Contributors and Collaborators 

D. Kramer, D. Pitchure, M.F. Savage, R. Thomson; 

G.G. Long (852); Y. Shim (University of Georgia) 

36 
Forming of Lightweight Material for Automotive Applications


Anelasticity and Springback Predictability


Increased computing power coupled with finite 

element modeling methods has brought the prediction 

of springback and springback compensated die design 

within the reach of industry. In developing this technology, 

industry has identified areas where better measurement 

methods and data are required and, in some cases, 

where our scientific understanding of materials behavior 

is incomplete. One such case is the influence of plastic 

deformation on the mechanisms of anelastic recovery 

and springback. The objective of this project is to develop 

the fundamental understanding, test methods, and data 

required to predict this phenomenon. 

Richard E. Ricker 

AU.S. Council for Automotive Research (USCAR) 

Consortium on Springback Prediction has recently 

reduced the errors in finite element prediction of springback 

to the point where they consistently underpredict 

springback by about 20%. At a meeting of the consortia, 

NIST scientists pointed out that this consistent error 

could be eliminated by assuming that plastic deformation 

reduces the modulus of elasticity. This hypothesis created 

controversy among the consortium members. Since 

this debate concerned fundamental issues related to 

measurement methods, NIST has examined this issue 

and hypothesized that the modulus appears changed 

because plastic deformation stimulates anelastic relaxations 

that occur after unloading. 

To determine if this hypothesis warranted further 

investigation, springback was measured using existing 

laboratory equipment at NIST. First, springback was 

measured with the NIST Rockwell hardness calibration 

machine and it was found that anelastic recovery increased 

springback by about 20% (Figure 1). Second, springback 

was measured during 3-point bend tests using a 

servo-hydraulic testing machine with similar results. It was, 

therefore, concluded that developing a better measurement 

of anelastic relaxations and data on the influence of 

Figure 1: The total springback and anelastic (non-linear) 

contribution in Rockwell hardness tests. 

large-scale plastic strain on anelastic recovery would 

enable industry to make better springback predictions. 

To accomplish this objective, a dynamic thermalmechanical testing machine was acquired in FY02. 

This equipment is capable of conducting mechanical tests 

at temperatures from –150 to 600°C and frequencies 

from 0.01 to 200 Hz with a 1 nm resolution of sample 

displacement. During FY02, our focus has been on 

developing experimental techniques for using this apparatus 

to study the influence of alloy composition and thermal 

mechanical treatment on: 1) complex modulus and 2) 

anelastic recovery. The first of these will be used to develop 

the fundamental understanding that will frame this effort 

while the second will be used to relate the fundamental 

understanding to industry relevant data. Once the scientific 

boundaries and measurement issues are understood, a 

standard test method for generating industry relevant data 

using a servo-hydraulic machine will be developed and the 

method and data distributed to the sheet metal forming 

industry. 

An example of the influence of plastic deformation on 

anelastic behavior can be seen in Figure 2. In this figure, 

two samples of the same aluminum alloy that have received 

different thermal-mechanical treatments are compared and 

it can be seen that plastic deformation significantly increased 

anelastic behavior. Transmission electron microscopy of 

these samples confirmed the presence of a higher density 

of dislocations at grain boundary particles in the cold rolled 

sample. 

Figure 2: Comparison of the imaginary or anelastic 

component of the complex modulus for deformed and 

undeformed aluminum samples. 

Contributors and Collaborators 

D.J. Pitchure, D. Dayan, and the Springback 

Predictability Consortium (USCAR, Alcoa, Ford Motor 

Company, General Motors Corporation, DaimlerChrysler 

Corporation, Livermore Software Technology 

Corporation, U.S. Steel Corporation) 

37 
Program Overview


Materials for Micro- and Optoelectronics


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 

38 
Materials for Micro- and Optoelectronics


Mechanism of Sn Whisker Growth from Electrodeposits


The electrodeposition of metallic alloys has been 

central to the growth of the electronics industry. 

This is largely due to the exceptional properties 

exhibited by electrodeposited material as well as 

the favorable economy of scale associated with 

electrodeposition processes. A technology important 

to electronics manufacturing is the electrodeposition of 

Sn-based coatings and surface finishes to guarantee 

solderability. With the rapid move to Pb-free solder 

surface finishes, new test methods are needed for 

predicting the tendency of such coatings to form 

Sn whiskers that can lead to catastrophic failures. 

Christian E. Johnson, Maureen E. Williams, 

and Kil-Won Moon 

I

n FY2001, the National Electronics Manufacturing 

Initiative (NEMI) Pb-Free Task Force, of which NIST 

is a member, identified a serious concern of OEMs, 

contract manufacturers, and component manufacturers 

with the conversion from Sn-Pb to Pb-free surface 

finishes for circuit boards and component leads. It is 

well known that the use of pure Sn protective surface 

finishes can cause serious problems: tin whiskers 

(1 mm diameter and several mm long) can grow from 

the plated tin surface and cause electrical shorts and 

catastrophic failure. Historically Pb was added to 

Sn plate to prevent whisker growth, and, thus, the 

“whisker problem” disappeared. With the rapid move 

to environmentally-friendly Pb-free assemblies, the 

microelectronics industry must remove Pb from the 

surface finishes. For many applications, an electroplated 

Sn-based surface finish remains a preferred surface for 

ease of processing. However, the growth of whiskers is 

currently a perilous drawback. 

Based on these needs, this NIST project is focusing 

on: 1) understanding the effect of alloying elements 

other than Pb on the tendency for whisker formation, 

2) developing techniques to separate possible physical 

and microstructural factors affecting whisker formation, 

and 3) assisting the NEMI Standardization Technology 

Integration Group (TIG) with both test development 

and understanding the root causes of whisker 

formation. The Sn-Cu system was chosen as the most 

versatile for electroplating, since it is compatible with 

Sn-3.9Ag-0.6Cu and Sn-0.7Cu, the Pb-free solders 

selected as the new national standard alloys by NEMI 

for reflow soldering and for wave soldering, respectively. 

Whiskers are generally believed to grow to relieve 

residual stress in electroplated Sn. However, the origin 

of this stress has not been determined definitively. 

Therefore, as a starting point, we focused on the 

relationship of microstructural change and whisker 

formation as a function of Cu additions. Increased Cu 

content reduced the grain size of the Sn deposit from 

0.65 μm to 0.2 μm. Furthermore, Cu in deposits forms 

Cu6Sn5 intermetallic compounds (IMC) at the Sn 

grain boundaries. In the absence of Cu additions, 

no whiskers were observed after one year of room 

temperature aging. However, with Cu additions, whiskers 

were observed within two days increasing to a density 

of 50/mm2 after one year for the highest Cu levels. 

Our current hypotheses are that a smaller grain size 

produces a higher level of intrinsic stress and that the 

presence of IMC particles at the grain boundaries may 

prevent relaxation of the stress. As a consequence, the 

stress level in the Sn-Cu deposits is relieved through 

whisker growth. To investigate this idea, cantilever beam 

test coupons were made from phosphor bronze and a 

commercial bright electrolyte. Using Stoney’s Equation, 

an average planar stress of the deposited film was 

calculated from the deflection of the beam as a function 

of time. Preliminary results of pure Sn and Sn-Cu 

deposits indicated that the presence of the IMC particles 

in the Sn-Cu deposits inhibited stress relaxation. The 

compressive stress in the pure Sn deposit went from 

an initial level of 14 MPa to zero after four days. In 

contrast, the initial compressive stress in the Sn-Cu 

deposit was 32 MPa and after 100 days was still at 

21 MPa. Whiskers were present after four days on the 

Sn-Cu sample, but after 100 days, the pure Sn sample 

was still whisker-free. 

Figure 1: Calculated stress levels with and without Cu 

additions. 

NIST is providing leadership in two NEMI 

whisker projects: identifying the fundamental growth 

mechanism and developing an accelerated test method. 

Our goal at NIST is to provide an understanding of the 

fundamentals of the whisker formation, which will ensure 

that the test developed by the NEMI group will have 

widespread applicability. 

Contributors and Collaborators 

W.J. Boettinger, G. Stafford (NIST); R. Gedney, 

I. Boguslavsky, P. Swaminath (NEMI project members) 

39 
Materials for Micro- and Optoelectronics


Superconformal Film Growth: Measurements and Modeling


State of the art manufacturing of microelectronic 

devices relies on superconformal deposition of copper 

for on-chip interconnects. Superfilling of trenches and 

vias results from the interplay of rate inhibiting and 

accelerating adsorbates. NIST has recently identified 

the mechanism that explains “bottom-up” filling of 

submicrometer features. A quantitative capability for 

predicting the influence of adsorbates on superconformal 

film growth has been demonstrated. The mechanism 

has also been shown to apply to the electrodeposition 

of elements beyond copper, as well as CVD processing. 

Thomas P. Moffat and Daniel Josell 

The mechanism of superfilling or “bottom-up” filling 

of submicrometer features has been explained. The 

chief tenets are: a) the deposition rate is proportional 

to catalyst coverage and b) the catalysts “floats” or 

remains segregated at the interface during film growth. 

Superfilling follows as a natural consequence of these 

stipulations. Namely, the catalysts coverage increases 

(decreases) as the local surface area decreases during 

deposition, thereby giving rise to “bottom-up” filling 

and a bright surface finish. 

Figure 1: “Bottom-up” filling of vias with silver. 

Quantitative description of the curvature enhanced 

accelerator coverage (CEAC) mechanism enables the 

simulation of feature filling. Three different electrode 

shape-change algorithms have been developed: 1) a simple 

model based on the solution of a single first-order 

differential equation, 2) a parameterized interface tracking 

code, and 3) a level set model, which incorporates a 

rigorous description of all concentration fields. Good 

agreement was found between these formalisms and feature 

filling experiments. A summary of the “simple model” 

simulations for filling trenches of variable aspect ratio as 

a function of applied potential and catalyst concentration 

is shown in Figure 2. 

The generality of the CEAC mechanism has been 

verified by demonstrating superfilling of metals other 

than copper, i.e. silver electrodeposition from an alkalin 

Figure 2: Feature fill/fail bondaries as a function of 

processing parameters: catalyst concentration, etc. 

electrolyte, as well as the first quantitative predictions of 

superfilling by iodine catalyzed chemical vapor deposition 

(CVD). 

All kinetic parameters were determined from 

voltammetric (i-V) and chronoamperometric (i-t) 

experiments performed on planar substrate. Correlation 

between the reactivity and catalyst coverage was determined 

by surface analysis following metal deposition or, 

alternatively, by dosing the surface with a prescribed 

quantity of catalyst prior to the metal deposition 

experiment. The second scheme not only substantiates 

the CEAC mechanism but may also be implemented in 

manufacturing in order to circumvent the challenging 

control issues associated with catalyst consumption 

during electrolyte aging. 

Figure 3: A one-to-one correlation between catalyst 

coverage (red) and the deposition rate (blue). 

Contributors and Collaborators 

D. Wheeler, J. Bonevich, W. Egelhoff, G. McFadden 

(ITL); S. Coriell, B. Baker, C. Yang, L. Richter, 

S. Robertson (CSTL); J. Mallett, C. Witt (International 

SeMaTech); B. Melnick, M. Freeman (Motorola); 

S.G. Pyo (Hynix Semiconductor) 

40 
Materials for Micro- and Optoelectronics


Solder and Solderability Measurements for Microelectronics


Solders and solderability are increasingly tenuous 

links in the assembly of microelectronics as a 

consequence of ever-shrinking chip and package 

dimensions and the international movement toward 

environmentally-friendly, lead-free solders. Through 

collaboration with the NEMI Pb-Free Assembly 

Project, we are providing the microelectronics industry 

with measurement tools, data, and analyses that 

address national needs in the implementation of leadfree solders. We also work with industrial standards 

organizations to provide measurement methods and 

guidance for integration of lead-free solders and new 

component types into assembly processes. 

Maureen E. Williams, William J. Boettinger, 

Carol A. Handwerker, Ursula R. Kattner, 

and Frank W. Gayle 

The U.S. microelectronics industry has clearly 

articulated the measurement needs for Pb-free solders 

and for solderability and assembly. For example, the 

urgency for materials data for Pb-free solders has been 

specified in the 1997 IPC, 1999 ITRS, 2000 NEMI, and 

2000 IPC Lead-Free Solder Roadmaps. The pressure from 

the Japanese consumer product market and from the EU 

to produce lead-free microelectronics continues to increase. 

In addition, the lack of understanding and control of current 

standard solderability measurements has inhibited the 

development of improved measurements necessary for new 

solders and for new packaging schemes. These industrial 

needs are addressed through this NIST project. 

Since 1999, NIST has served a major role in the 

NEMI Pb-Free Assembly Project to identify and move 

Pb-free solders into practice. Last year, NIST held a 

workshop cosponsored by NEMI, NSF, and TMS, on 

Modeling and Data Needs for Lead-Free Solders. The 

report from this workshop is serving as a roadmap for 

research on the reliability of lead-free solders. In FY2002, 

the NEMI Lead-free Task Force and the National 

Institute of Standards and Technology (NIST) have 

worked together to respond to the identified needs by: 

■

Identifying the most important lead-free solder data 

for the microelectronics community; 

■

Developing “a guide to recommended practices” for 

measuring the mechanical, thermal, electrical and 

wetting properties of lead-free solders. This document 

is being distributed to all interested parties through the 

NEMI and NIST websites and through NIST in hard 

copy form; 

■

Gathering into a single database existing physical and 

mechanical property data that have been developed by 

researchers around the world; 

■

Critically reviewing existing materials property data for 

the most important alloys for use in finite element 

analyses; and 

■

Providing a list of literature references on alloys, 

processing, reliability, environmental issues, and 

components for assisting in the implementation of 

lead-free solders. 

In a second major activity with the NEMI Lead-Free 

Assembly Project, NIST completed the microstructurebased failure analysis of thermally-cycled assemblies as 

part of the project’s full-scale reliability trials with the 

new national standard Pb-free solder. The NEMI Final 

Report will be issued in early FY2003. 

NIST is also working in collaboration with the IPC 

Standards Committees (most closely with members from 

Celestica, Lucent, Raytheon, Rockwell, and Shipley-Ronel) 

to establish reproducible solderability test standards for 

board assembly. Activities include: 1) providing benchmark 

experiments for the wetting balance tests to predict 

on-line solderability for a wide range of surface finishes, 

lead materials, and solder alloys; 2) developing a “best 

practice” for globule solderability test for small components 

and pads; and 3) evaluation of the effect of component 

lead geometery on industrial solderability tests. 

Figure 1: Metallographic cross-section of a lead-free SnAgCu 

solder joint showing fracture in the solder adjacent to the 

interface with the component following accelerated thermal 

cycling. Failure location is the same as for Sn-Pb eutectic 

solder, which this alloy is replacing as a standard alloy. 

Highlights 

■

Sources of uncertainty have been established for 

wetting balance solderability tests leading to increased 

repeatability and reproducibility of tests. 

■

Recent flux studies performed at NIST led to a change 

in test procedures for the IPC/EIA/JEDEC J-STD 

002 solderability standards. 

■

Research at NIST helped to separate the role of solder 

melting temperatures from solder paste wetting 

dynamics and the effect of air reflow. 

Contributors and Collaborators 

L.C. Smith (NIST); K.-W. Moon (University of 

Maryland); D. Napp (National Center for Manufacturing 

Sciences and associated consortium members); 

R. Gedney (NEMI Lead-Free Task Force and 

associated consortium members) 

41 
Materials for Micro- and Optoelectronics


Magnetic Properties and Standard Reference Materials


Users of magnetic materials, including the recording 

industry, the permanent magnet industry, and the 

manufacturers of electric motors and transformers of 

all types, need standard reference materials (SRM’s) 

to calibrate instruments used to measure the critical 

magnetic properties of their starting materials. 

The magnetic materials group is in the process of 

developing such standards. Methods for improving 

the efficiency and accuracy of measuring and 

characterizing magnetic materials of industrial 

importance, including measurement of magnetic 

susceptibility over wide frequency ranges, are also 

under investigation. 

Robert D. Shull and Robert D. McMichael 

I

n collaboration with scientists from universities, 

industry, and other Divisions at NIST, magnetic 

materials important to the scientific and industrial 

communities are prepared and methods for the improved 

measurement of their properties are developed. Standard 

Reference Materials for the calibration of existing and 

planned instruments used in the measurement of magnetic 

properties are developed and produced. An equally 

important parameter to know how to measure is time 

dependence of magnetization. Consequently, methods 

for the characterization of accommodation and aftereffect 

in magnetic recording and permanent magnetic materials 

are developed. Models are also developed for determining 

the most efficient methods to fully characterize the 

hysteresis and magnetostriction in magnetic materials. 

Commercial instruments for the measurement of 

magnetic properties are relative instruments that rely 

on known samples for their calibration. To produce 

standard samples for such instruments, an absolute 

magnetometer was developed and assembled at NIST. 

A picture of this instrument is shown below. 

Figure 1: Absolute magnetometer. 

Figure 2: Thorpe-Sentfle Method for Absolute 

Susceptibility Measurement. 

Prior to FY02, two SRM’s were issued: a nickel 

sphere (SRM 772a) and a nickel disc (SRM 762). 

The measurements for the complete series of magnetic 

SRMs are made using the Thorpe–Sentfle method 

shown above. This technique has the advantage of not 

requiring knowledge of the field gradient anywhere in 

the apparatus. As that is the largest source of error, 

higher accuracy is possible. 

We measure the susceptibility by physically moving 

the sample to various positions from the field center to 

some distance outside of the magnet measuring the 

magnetic force and then integrate that force vs. distance 

relationship. 

Two new SRMs were developed this year. The first 

was a 1 mm diameter yttrium iron garnet (YIG) sphere 

for use in calibrating the more sensitive ranges of 

magnetometers (SRM 2853). In addition, it will be 

useful in calibrating very sensitive instruments such 

as alternating gradient magnetometers and SQUID 

magnetometers. Because of its high resistivity, the 

yttrium iron garnet sphere should also be useful for 

calibrating magnitude and phase in alternating current 

magnetometers. The second SRM is a platinum cylinder 

paramagnetic susceptibility standard (SRM 764a). 

This will be useful in calibrating the zero field point 

and linearity of magnetometers due to its paramagnetic 

nature, and it will also be useful for calibrating the field 

scale after the moment scale has been calibrated. 

Contributors and Collaborators 

A.J. Shapiro, R.V. Drew; S.D. Leigh (ITL); 

Industrial and academic collaborators: L.J. Swartzendruber, 

D.E. Matthews, G.E. Hicho, L.C. Smith, L.H. Bennett, 

E. Della Torre (George Washington University) 

42 
Materials for Micro- and Optoelectronics


Magnetic Properties of Nanostructured Materials


In the past decade, there has been a remarkable 

improvement in the technology for materials 

preparation resulting in present day’s capability 

of controlling morphology and features at the 

nanometer level. In magnetism, such control allows 

the fabrication of nm-thick composite materials of 

dissimilar magnetic behavior, leading to materials with 

novel bulk magnetic character and unusual properties. 

We are providing materials metrology necessary for 

U.S. industry to understand the behavior of these new 

materials and take advantage of the novel properties. 

Alexander J. Shapiro and Robert D. Shull 

Greater information storage on recording discs 

is being accomplished by reducing the size of 

the regions in which information is stored down to 

nanometer sizes. Unfortunately, when those regions 

become too small, the material ceases to be ferromagnetic 

(FM) and, instead, becomes superparamagnetic and no 

longer retains magnetic information. In order to exceed 

the so-called “superparamagnetic limit,” the recording 

industry has recently introduced magnetic media containing 

two layers of a ferromagnet separated by a sub-nanometer 

thick layer of Ru. In this structure, the thickness of the 

nm-diameter regions has been effectively increased by 

providing magnetic coupling between the two ferromagnetic 

layers via the in-between Ru. Consequently, the volume 

of the element has been maintained large, even though 

the lateral dimensions of the recording “bit” have been 

decreased, thereby enabling retention of the ferromagnetic 

state. However, for this new type of media, it is unknown 

how long information will be retained in those “bits” 

and what sort of fields are necessary for reversing their 

magnetization. We have addressed this problem by imaging 

the magnetic domains in this new type of media using the 

magneto-optic indicator film (MOIF) technique developed 

in our laboratory (Figure 1). 

Figure 1: MOIF image of the remagnetization process of 

a Co/Ru/Co homogeneous structure containing pinholes 

in the Ru in a field oriented along the total magnetization 

vector. (a) :oH = 0 mT after magnetization in a field of 

+60 mT; (b) :oH = –9.4 mT; (c) :oH = –9.4 mT after a 

5 sec. wait; (d) :oH = -13.0 mT. The inserts in (a) and 

(d) show the intensity change of the MO signal. 

The first conclusion from the MOIF observations 

was that, surprisingly, the magnetization vectors in the 

two FM layers in this 3-layer structure were not colinear 

as originally assumed. In Figure 1, the lack of colinearity 

is seen by the 100 degree angle between the magnetization 

vectors (one white and the other black) of the two FM 

layers. As a consequence of this non-colinearity, the 

magnetization reversal mechanism now involves the 

cooperative behavior of both Co layers simultaneously, 

leading to different coercive fields and switching speeds. 

Figure 2 (e-h) shows that this non-colinearity is due to 

the presence of pinholes in the 0.5 nm thick Ru. 

Figure 2: MOIF image of the remagnetization process of 

a Co/Ru (a-d) and a Co/Ru/Co (e-h) thin film containing no 

pinholes in a field oriented along the total magnetization vector. 

H is directed vertically in the figure at increasing magnitude 

from 4 mT to 4.8 mT (a-d) and from 2 mT to 54 mT (e-h). 

For the Co/Ru /Co multilayer with no pinholes, the 

two FM layers have magnetization vectors which are colinear. 

With pinholes present, the greater their number, the greater 

their effect on the magnetic spin misalignment shown in 

Figure 1. Since most sub-nanometer thin films contain 

pinholes, these results clearly demonstrate the importance 

of knowing the effect of these defects. One of the 

ramifications of the non-colinearlity is the presence of time 

dependence in the coercivities of the stored information, a 

particularly deleterious situation. Information safely stored 

now may not be safely stored tomorrow. Two papers have 

been published presenting these results and a third is in 

progress to clarify the situation. 

Contributors and Collaborators 

Alexander J. Shapiro, Robert D. Shull, Robert D. 

McMichael, William F. Egelhoff (NIST); Valerian I. 

Nikitenko (Johns Hopkins University); Vladimir S. 

Gornakov (ISSP, Russian Academy of Sciences, NIST) 

43 
Materials for Micro- and Optoelectronics


Nanomagnetodynamics 

For GHz data rate hard drives, magnetic memory 

chips and other high-frequency magnetic devices, 

magnetization damping will be an important factor 

affecting performance. Another consequence of 

damping is thermal fluctuations that cause sensor 

noise and data loss in media. We provide industry 

with: 1) an improved understanding of magnetic 

damping mechanisms, 2) improved magnetic 

damping measurements and standards, and 

3) data and methods for controlling magnetic 

damping in technically relevant materials. 

Robert D. McMichael 

This project is concerned with the metrology and 

mechanisms of magnetization damping, a process 

where magnetic energy is dissipated as the magnetization 

comes to equilibrium. The same mechanisms that allow 

damping also allow thermal energy to cause magnetization 

fluctuations that cause noise in sensors such as disk 

drive read heads and data loss in recorded media. 

Damping mechanisms are recognized as being important 

both for GHz data rate writing and reading processes 

and for long-term stability of stored data. A convenient 

measurement of damping is the ferromagnetic resonance 

(FMR) linewidth, a measurement that is complicated by 

the presence of inhomogeneities. 

In FY2002, our accomplishments include: 

1) a very successful model of ferromagnetic resonance in 

inhomogeneous films (see highlight), 2) demonstrations 

of the effects of intentional defects, 3) measurements of 

damping in thin magnetic metal films by spin transport 

Figure 1: Increased FMR linewidth resulting from 

intentionally-created defects created to clarify the effects 

of nanoscale defects on FMR damping measurements. 

Our modeling describes the effects of the random coupling 

to the polycrystalline, antiferromagnetic NiO. 

into normal metals, and 4) measurements of the very low 

damping in high moment, soft materials under development 

for read heads. 

We have measured the intrinsic linewidth of 

Permalloy films, and we have found that it follows one 

of several proposed phenomenological forms. This data 

has been very valuable to theorists working on physical 

damping mechanisms. 

One novel physical damping mechanism is damping 

via spin-polarized electron transport. It had been shown 

elsewhere that additional damping can be created by 

polarized electrons propagating into Pt or Pd surface 

layers. We have shown that the enhanced damping can 

be achieved with as little as 0.5 nm of Pt, and we have 

shown that the effect is substantially reduced by a Cu 

spacer between the Permalloy and Pt that is as thin as 

0.5 nm. The abrupt decrease with a thin Cu spacer 

suggests that the damping enhancement has a contact 

component in addition to the spin transport component. 

In FY2002, four papers related to this project were 

published, five contributed talks presented and three 

invited talks given at Seagate Research, U.C. San Diego, 

and a National Storage Industry Consortium meeting, 

and two more invitations have been received to speak at 

the 47th annual MMM conference in November 2002. 

Figure 2: Effect of Pt overlayers on damping in Permalloy 

films. The effect shows how spin polarized electron 

transport across the interface contributes to damping. 

Contributors and Collaborators 

R.D. McMichael, A.B. Kunz, D.J. Twisselmann, 

A.P. Chen, W.F. Egelhoff (Metallurgy Division, MSEL); 

S.E. Russek (EEELM); E. McHenry, H. Okumura 

(Carnegie Mellon University) 

44 
Materials for Micro- and Optoelectronics


New Materials for Ultra-High Density Data Storage


The objective of this program is to provide assistance 

to U.S. companies in the ultrahigh density data 

storage industry, which includes such products as 

hard disk drives and magnetoresistive random access 

memory chips. Our work provides U.S. companies 

with significant competitive help by investigating the 

scientific issues underlying the manufacturing process. 

Often, this scientific understanding will point the way 

to improved manufacturing processes. One such 

example is illustrated in the figures below. 

William F. Egelhoff, Jr. 

Hard disk drives play a crucial role in the 

information revolution. The World Wide Web is 

stored on millions of hard disk drives around the world. 

The exponential growth of the Web has depended on 

the exponential growth in hard disk storage capacity. 

Maintaining these exponential growth rates is one of 

the great challenges of the information age. 

Today, giant magnetoresistance (GMR) is the current 

technology used for read heads in hard disk drives. It is 

unrivaled in its ability to read sub-micron-sized bits at 

gigahertz frequencies. However, the time is not far off 

when technologies better than GMR will be needed to 

maintain the historical exponential growth rates in 

storage density. 

Our aim is to assist the U.S. companies that are 

developing these new technologies. One promising new 

technology is magnetic tunnel junctions (MTJs). MTJs 

are magnetic thin films with a typical layer structure of 

Co /Al2O3 /Co. Electrons tunnel from one Co layer to 

the other through the Al2O3. One problem with MTJs 

is that they are not highly reproducible. 

To understand the origin of this problem, NIST 

began a series of measurements at the Magnetic 

Engineering Research Facility (MERF) to determine 

the fundamental growth mechanisms in MTJ fabrication. 

MERF is a unique facility specifically designed to 

study surface and interface effects occurring during the 

growth of magnetic thin films for ultrahigh density data 

storage applications. The results at MERF identified 

interdiffusion at the Al/Co interface as a problem in the 

growth of MTJs, as illustrated in Figure 1. 

When the Al is oxidized to make Al2O3 some of the 

Al remains in metallic form in the Co. The extent of the 

interdiffusion is highly susceptible to small changes in 

experimental conditions. As a result, nominally identical 

MTJs exhibit a lot of scatter in their performance data, 

as illustrated in Figure 2. 

NIST demonstrated at MERF that oxidizing 

two atomic layers of the Co surface prior to the Al 

deposition provided an excellent diffusion barrier and 

that the Al reduced the Co oxide back to Co metal. 

NIST transferred this technology to Read-Rite, which 

found greatly improved manufacturing uniformity for 

MTJs and an improved magnetoresistance when this 

approach was used. 

Magnetic Tunnel Junction Fabrication 

Figure 1: An illustration of the intermixing that occurs 

in the standard method of MJT fabrication when Al is 

deposited on Co and the NIST modification using a thin 

Co oxide diffusion barrier to prevent the intermixing. 

Figure 2: Read-Rite Corp. data on magnetic tunnel junctions. 

“The results were amazing. The scattered data 

collapsed into a single point.” 

Dr. H.C. Tong 

Director of Advanced Read-Head 

Research, Read-Rite Corp. 

Contributors and Collaborators 

W.F. Egelhoff, Jr., R.D. McMichael (NIST/MSEL); 

M.D. Stiles (NIST/Physics); 6 U.S. Corporations, the 

Naval Research Laboratory, 7 U.S. Universities, and 

13 International Universities 

45 
Program Overview


Materials Property Measurements


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 

46 
Materials Property Measurements


Hardness Standardization: Rockwell, Vickers, Knoop


U.S. industry needs to be able to make measurements 

that are traceable to national standards and compatible 

with the measurements made in other countries. This 

need is being emphasized by the requirements of quality 

standards such as ISO 17025. For the measurement 

of hardness, NIST is meeting this need by standardizing 

U.S. national hardness scales, producing hardness 

reference standards, and providing assistance and 

guidance to U.S. industry through national and 

international standards activities. 

Samuel R. Low, Christian E. Johnson, 

James L. Fink, and David R. Kelley 

Hardness is the primary test measurement used to 

determine and specify the mechanical properties 

of metal products. The Metallurgy Division is engaged 

in all levels of hardness standards activities to assist 

U.S. industry in making measurements compatible 

with other countries around the world. These activities 

include the standardization of the national hardness 

scales, development of primary reference transfer 

standards, leadership in national and international 

standards writing organizations, and interactions and 

comparisons with U.S. laboratories and the National 

Metrology Institutes of other countries. 

International Activities 

At the international level, we are participating in 

the Working Group on Hardness (WGH) under the 

International Committee for Weights and Measures 

(CIPM) (Figure 1). The primary goal is to standardize 

hardness worldwide. With NIST serving as secretary 

of the WGH, this year’s WGH work has included an 

initial effort to better define the Rockwell hardness 

test procedure used by National Metrology Institutes 

(NMIs). Other international activities include: heading 

the U.S. delegation to the International Organization 

for Standardization (ISO) TC 164/SC 3 committee 

on hardness testing of metals, which oversees the 

ISO hardness test method standards; acting as the 

U.S. representative to the International Measurement 

Confederation (IMEKO) TC5 committee on hardness; 

Figure 1: Attendees of the 5th WGH meeting at INMETRO 

(Brazil) in May 2002, representing international standards 

organizations and the hardness laboratories of nine NMIs. 

and because NIST is the Secretariat for the International 

Organization of Legal Metrology (OIML) TC10/SC5 

committee on hardness, we are revising the international 

requirements for regulating hardness. 

National Activities 

Our primary task at the national level is to standardize 

the U.S. national hardness scales and to provide a means 

of transferring these scale values to industry. Currently, 

we are producing test block Standard Reference 

Materials® (SRMs) for the Rockwell, Vickers and Knoop 

hardness scales (Figure 2), as well as developing new 

reference standards. Ten different microhardness SRMs 

for Vickers and Knoop hardness are now available. Using 

electro-deposition technology, the standards are produced 

with uniform properties and microstructure. Work is 

progressing in developing a prototype high hardness 

Vickers microhardness SRM having a hardness range 

of 750 to 800. 

Figure 2: SRM test blocks for Rockwell, Vickers and 

Knoop hardness (metals). 

We also completed the calibration of three new SRMs 

for the Rockwell B scale (HRB) to compliment the three 

SRM Rockwell C scale blocks currently available. The HRB 

scale is used for testing softer metals, such as aluminum, 

copper and brass. Initial work is also being planned to 

produce a new Rockwell indenter SRM, which has become 

feasible due to the successful completion of a Small 

Business Innovative Research (SBIR) Phase-2 project 

with Gilmore Diamond Tools to develop an improved 

method for manufacturing geometrically correct Rockwell 

diamond indenters. 

It is important that knowledge gained from the NIST 

calibration work be shared with industry. Since the new 

NIST Recommend Practice Guide: Rockwell Hardness 

Measurement of Metallic Materials was published in 

May 2001, almost 5000 copies have been requested 

by and distributed to industrial facilities. 

Contributors and Collaborators 

J. Song, C. Evans, R. Clary (NIST/MEL); 

W. Liggett, Jr., N. Zhang (NIST/ITL); C. Beauchamp, 

D. Faison, W. Stiefel (NIST/TS); M. Mihalec (Gilmore 

Diamond Tools, East Providence, RI) 

47 
Materials Property Measurements


Deformation Mechanisms and Constitutive Laws 

in Thin Film Superlattices 

Thin film superlattices exhibit favorable deformation To solve this problem, research was underway in 

and wear properties compared to existing protective FY2002 to characterize the physical processes and 

coatings. However, little understanding of the deformation structures that arise during nanoindentation 

deformation mechanisms or constitutive laws and, using multi-scale modeling and simulation, develop 

governing deformation in these materials exists, a framework for prescribing stress/strain relationships. 

making it difficult to assess lifetime estimates, cost A technique to observe the deformation structures with 

feasibility or perform predictive modeling. This project transmission electron microscopy (TEM) under nanoscale contacts was developed last year at NIST. This aims to combine experimental and computational approach uses a wedge indenter to impose a line of methods to study deformation mechanisms and deformation on the surface rather than a single point. stress/strain relations in thin film superlattices. An example of the surface deformation can be seen in the 

atomic force microscopy image on the left. This has two Donald E. Kramer and Timothy J. Foecke	 advantages: the deformation zones under these indents 

can be readily located in the TEM and the plane strain 

conditions under the wedge reduce the computational 

he mechanical properties of thin films can play intensity for methods such as finite element simulations. Tan important role in the design and reliability of An example of the deformation structure in a W/NbN devices. Regardless of the material property of interest, superlattice is shown in the middle figure as seen by mechanical integrity must be maintained to assure TEM. The superlattice is embedded below a 250 nm 

proper device performance. However, measurement layer of tungsten. The direction of indentation is from and modeling of thin film mechanical properties the top normal to the layer interfaces with the long axis present significant challenges without knowledge of of the wedge normal to the image plane. Planar defects an appropriate constitutive law for deformation. This is are seen in the lighter NbN layers, while the dark particularly true for thin film superlattices. These thin W layers are comparatively defect free. film materials are composed of hundreds to thousands The finite element simulation in the right figure of alternating layers of two different materials. Each 

was compared to the observed deformation field to layer may be from single to tens of nanometers in 

thickness. The result of this layered structure is a understand where plastic strain initiated and the volume 

material that exhibits high resistance to deformation into which it expanded. The mesh consists of a 1 μm 

and wear. The superlattice derives its strength from the superlattice layer sandwiched between a 250 nm 

high density of bi-material interfaces. However, neither tungsten capping layer and a tungsten substrate. 

As the indenter compresses the capping layer, plastic the mechanism by which these interfaces provide that deformation in the embedded superlattice initiates at the strength nor the quantitative effect on the stress/strain lower film/substrate interface and expands toward the relationship is well understood. capping layer interface. These experiments help in the 

development of deformation mechanisms and, hence, Nanoindentation is an experimental tool that can constitutive equations that operate for nanolayers. probe the mechanical properties of surfaces with 

nanometer depth sensitivity. This makes it a potentially 

useful tool for studying the mechanical properties of thin Contributors and Collaborators films. However, at the nanometer length scale, extraction


of mechanical properties is not straightforward due M.F. Savage, L. Ma, D.T. Smith (NIST);


to the discreet nature of the lattice, the influence of P.M. Anderson (Ohio State University); S.A. Barnett


substrate mechanical properties, and the large strain (Northwestern University); H. Kung (Los Alamos


gradients under the indenter. National Laboratory)


48 
Materials Property Measurements


Analysis of Structural Steel in the World Trade Center Investigation


In 2002, NIST became the lead agency in a planned 

investigation of the World Trade Center collapse. 

The investigation addresses many aspects of the 

catastrophe, from occupant egress to factors affecting 

how long the Twin Towers stood after being hit by the 

airplanes, with the goal of gaining valuable information 

for the future. A critical aspect of the investigation is 

the metallurgical and mechanical analysis of structural 

steel from the Twin Towers and WTC 7. The analysis 

includes characterization of properties, failure modes, 

and temperature excursions seen by the steel. 

Frank W. Gayle, Richard J. Fields, 

and Stephen W. Banovic 

The collapse of the twin World Trade Center towers 

on September 11, 2001 was the worst building 

disaster in human history. Engineers, emergency 

responders, and the nation did not anticipate, and were 

largely unprepared for, such a catastrophe. Among 

other national needs, these events highlight the 

following technical priorities: 

■ To establish the probable technical causes of the 

collapses and derive the lessons to be learned; 

■ To develop and disseminate immediate guidance and 

tools to assess and reduce future vulnerabilities; and 

■ To produce the technical basis upon which costeffective changes to national practices and standards 

can be developed. 

NIST has prepared a technical investigation plan to 

address these issues (see <http://wtc.nist.gov/>). 

A primary objective of the investigation is to determine 

why and how the World Trade Center Buildings collapsed 

after the initial impact of the aircraft. To aid in this 

investigation, more than 100 WTC steel structural 

elements were brought to NIST to be studied. The 

NIST Metallurgy and Materials Reliability Divisions’ 

project to study the steel is outlined here. 

Task 1 — Identification of steel. Steels in the 

exterior and core columns, welds, spandrels, trusses, 

truss seats, and fasteners of the WTC Towers 1 and 2, 

and WTC 7 will be identified based on composition, 

microstructure, and mechanical properties, and 

compared to specifications from the period. 

Task 2 — Failure mechanisms based on visual 

evidence. Steel pieces at NIST, and evidence available 

from other sources, will be examined and documented 

as to failure mechanisms. 

Task 3 — Property data to support structure 

performance and airplane impact modeling studies. 

In addition to the mechanical properties provided in 

Task 1, the steels in the exterior and core columns, 

welds, spandrels, and fasteners of WTC 1 and 2 will be 

tested for high strain rate properties, including tensile 

and yield strength, ductility, and impact properties. 

Task 4 — Steel property data to support models 

of steel frame performance in fire. Creep and high 

temperature tensile properties will be measured for 

columns, bolts on columns, trusses, hangers, and bolts 

or welds associated with truss seats. 

Task 5 — Steel property data to support models 

of steel performance during collapse. High-strain-rate, 

room-temperature tensile properties will be measured 

for truss seats and associated bolts and welds. 

Task 6 — Models of elevated temperature deformation 

behavior. Models of elevated temperature deformation as 

a function of load and time at temperature will be provided 

for relevant steels, giving deformation information for steels 

with any given history of loading and temperature. 

Task 7 — Determination of maximum temperatures 

exposure. The steel will also be analyzed to estimate 

maximum temperatures reached, although it is recognized 

that high temperature exposure before the collapse may 

be difficult or impossible to distinguish from exposure 

during post-collapse fires. Studies of paint condition 

on the steel, microstructural changes in the steel, and 

stress relief in high strength bolts, washers, and weld 

zones will be done. 

Figure 1: Exterior columns and floor trusses during WTC 

tower construction. These critical elements of the steel 

structure will be characterized in the NIST investigation. 

Contributors and Collaborators 

J.D. McColskey, T. Siewert, C. McCowan, R. Santoyo 

(Materials Reliability Division, MSEL); T. Foecke, 

M. Williams, D. Kelley, S. Claggett, W. Luecke, J. Cahn 

(Metallurgy Division, NIST Materials Science and 

Engineering Laboratory); P. Brand (NIST Center for 

Neutron Research, MSEL); John Gross (NIST Building 

and Fire Research Laboratory) 

(Skilling Ward Magnusson Barkshire Inc.) 

49 
Program Overview


Materials Structure Characterization


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 

50 
Materials Structure Characterization


Nanoscale Characterization: Electron Microscopy


Electron microscopy is used to characterize the 

structure and chemistry of materials at the nanometer 

scale to better understand and improve their 

properties. New measurement techniques in electron 

microscopy are being developed and applied to 

materials science research. The MSEL Electron 

Microscopy Facility primarily serves the Metallurgy, 

Ceramics, and Polymers Divisions as well as other 

NIST staff and outside collaborative research efforts. 

John E. Bonevich 

Atomic-scale structure and compositional 

characterization of materials can lend crucial 

insights to the control of their properties. For instance, 

direct observation of local structures by transmission 

electron microscopy (TEM) provides an important 

information feedback to the optimization of crystal 

growth and processing techniques. Various 

characteristics may be observed such as crystal 

structure and orientation, grain size and morphology, 

defects, stacking faults, twins and grain boundaries, 

second phase particles — their structure, composition 

and internal defect structure, compositional variations 

and the atomic structure of surfaces and interfaces. 

The MSEL Electron Microscopy Facility consists of 

two transmission electron microscopes, three scanning 

electron microscopes, a specimen preparation laboratory, 

and an image analysis /computational laboratory. The 

JEOL3010 UHR-TEM has atomic scale resolution as 

well as detectors for analytical characterization of thin 

foil specimens. An X-ray detector (EDS) provides 

compositional analysis and an energy-selecting imaging 

filter (IF) allows compositional mapping at atomic 

resolution. The JSM6400 is equipped with electron 

backscattered diffraction/phase identification (EBSD) 

and EDS systems for characterization of texture and 

composition of materials. 

FY2002 Highlights 

■ ATP intramural research collaboration with the 

Semiconductor Electronics and Electricity Divisions 

(EEEL) to characterize quantum effects in confined 

Si devices. 

■ ATP intramural research collaboration with the 

Optoelectronics Division (EEEL) to characterize 

quantum dot III-V materials. 

■ Measurement of size distributions in CeO2 nanoparticles 

for use as an x-ray particle size standard reference 

material. 

■ Characterization of superconformal deposition of silver 

in sub-100 nm features for on-chip interconnections. 

The shape of self-assembled quantum dots 

(QDs) play a major role in their electronic properties. 

In conjunction with RHEED and AFM, TEM studies 

of QD shape and faceting have revealed novel structures 

in In0.44Ga0.56As (see Figure 1). Typical models for 

QD shape include hexagonal dots as well as diamond 

shaped pyramids. However, TEM results show unusual 

facets. Instead of appearing with trapezoidal or triangular 

cross-sections, the QDs have multiple facets at their 

peaks and bases. The varied shapes have implications 

for the control and reproducibility of the MBE growth 

process of QDs. 

Figure 1: Plan-view TEM of InGaAs QDs reveals “X” 

features indicating the shape due to surface facets. 

Some QDs have additional facets (arrowed). 

Figure 2: Cross-sectional HRTEM of InGaAs QDs 

indicating unusual faceting. 

Contributors and Collaborators 

R.D. McMichael, D. Josell, T.P. Moffat, J. Cline 

(MSEL); A. Roshko, S. Lehman (EEEL); E. Vogel, 

N. Zimmerman (EEEL); Prof. A. Stanishevsky 

(University of Maryland, Institute for Plasma Research) 

51 

Metallurgy Division FY02 Annual Report Publication List


Metallurgy Division FY02 Annual Report Publication List0

Modeling Solidification and 

Microstructural Evolution 

Boettinger, W.J., Warren, J.A., Beckermann, C., 

and Karma, A., “Phase-field simulation of solidification.” 

Annual Review of Materials Research, vol. 32, 

pp. 163–194, 2002. 

Ferreiro, V., Douglas, J.F., Warren, J.A., and 

Karim, A., “Nonequilibrium pattern formation in the 

crystallization of polymer blend films.” Physical 

Review E, vol. 65, no. 4, pp. 042802-1–042802-4, 

Apr. 2002. 

Ferreiro, V., Douglas, J.F., Warren, J.A., and 

Karim, A., “Growth Pulsations in symmetric dendritic 

crystallization in thin polymer-blend films.” Physical 

Review E, vol. 65, no. 5, pp. 051606-1–051606-16, 

May 2002. 

George, W. and Warren, J.A., “Parallel 3D dendritic 

growth simulator using the phase-field method.” Journal 

of Computational Physics, vol. 177, pp. 264–283, 

2002. 

Guyer, J.E., Boettinger, W.J., Warren, J.A., and 

McFadden, G.B., “Model of electrochemical double 

layer using the phase field method,” 2002. 

Proceedings of 201st Meeting of the Electrochemical 

Society: Design and Mathematical Modeling of 

Electrochemical Systems. van Zee, J.W., Orizama, M.E., 

Fuller, T., and Doyle, C.M., (in press). 

Josell, D., Basak, D., McClure, J.L., Kattner, U.R., 

Williams, M.E., Rappaz, M., and Boettinger, W.J., 

“Moving the pulsed heating technique beyond monolithic 

specimens: experiments with coated wires.” Journal of 

Materials Research, vol. 16, pp. 2421–2428, 2001. 

Lobkovsky, A.E. and Warren, J.A., “Phase field 

modeling of the premelting of grain boundaries.” 

Physica D, vol. 164, no. 3–4, pp. 202–212, Apr. 2002. 

Rappaz, M., Jacot, A., and Boettinger, W.J., “Last 

stage solidification of alloys: a theoretical study of 

dendrite arm and grain coalescence.” Metallurgical and 

Materials Transactions, 2002, (in press). 

High Speed Machining 

Basak, D., Yoon, H.W., Rhorer, R., and Burns, T., 

“Microsecond time-resolved pyrometry during rapid 

resistive heating of samples in a Kolsky bar apparatus,” 

2002, Chicago, IL. Proceedings of the 8th Symposium 

on Temperature: Its Measurement and Control in 

Science and Industry. 

Metal Powder Processing 

Biancaniello, F.S., Jiggetts, R.D., Stoudt, M.R., 

Ricker, R.E., and Ridder, S.D., “Suitability of powder 

processed high nitrogen stainless steel alloys for high 

performance applications,” 2002, Orlando, FL. 

Proceedings of PM 2TEC 2002, (in press). 

Gnäupel-Herold, T., Prask, H.J., and Biancaniello, 

F.S., “Residual stresses and elastic constants in thermal 

deposits,” in Gdoutos, E.E. (ed.). Recent Advances in 

Experimental Mechanics In Honor of Isaac M. Daniel, 

Dordrecht, Netherlands: Kluwer Academic Publishers, 

pp. 507–514, 2002. 

Magness, L., Kecskes, L., Biancianello, F.S., Ridder, 

S.D., Chung, M., and Kapoor, D., “The Performance of 

a Nanocrystalline Tungsten Composite in Ballistic 

Impacts,” 4608, pp. 216–224, SPIE, 2002. 

Mates, S.P., Biancaniello, F.S., and Ridder, S.D., 

“An alternative view of close-coupled gas atomization of 

liquid metals,” 2002, Orlando, FL. Proceedings of 

PM2TEC 2002, (in press). 

Mates, S.P. and Settles, G.S., “A study of liquid 

metal atomization using close-coupled nozzles, Part 1: 

gas dynamics.” Atomization and Sprays, 2002, 

(in press). 

Mates, S.P. and Settles, G.S., “A study of liquid 

metal atomization using close-coupled nozzles, Part 2: 

atomization behavior.” Atomization and Sprays, 2002, 

(in press). 

Ridder, S.D., “Measurement and control of metal 

flow-rate in a gas-metal atomizer,” 2002, Orlando, FL. 

Proceedings of PM2TEC 2002, (in press). 

Electrochemical Processing of 

Nanoscale Materials 

Ford, A., Bonevich, J.E., McMichael, R.D., 

Vaudin, M., and Moffat, T.P., “Structure and magnetic 

properties of electrodeposited Co and Co-Fe thin films 

on GaAs (001).” Journal of the Electrochemical 

Society, 2002, (submitted). 

Moffat, T.P., “Electrochemical STM,” in Bard, 

A.J. and Stratmann, M. (eds.). Encyclopedia of 

Electrochemistry, Vol. 3, 2002, (in press). 

Shima, M., Salamanca-Riba, L., McMichael, R.D., 

and Moffat, T.P., “Magnetic properties of ultrathin 

laminated Co/Cu films prepared by electrodeposition.” 

Journal of the Electrochemical Society, vol. 149, no. 9, 

pp. C439–C444, 2002. 

53 
Metallurgy Division FY02 Annual Report Publication List


Tsuda, T., Hussey, C., Stafford, G.R., and 

Bonevich, J.E., “Electrochemistry of titanium and the 

electrodeposition of Al-Ti alloys in the lewis acidic 

aluminum chloride-1-ethyl-3-methylimidazolium chloride 

melt.” Journal of the Electrochemical Society, 2002, (in 

press). 

Combinatorial Materials Research: 

Interconnects to Optoelectronic Materials 

Davydov, A.V., Boettinger, W.J., Kattner, U.R., and 

Anderson, T.J., “Thermodynamic assessment of the 

gallium-nitrogen system.” Physica Status Solidi A-Applied 

Research, vol. 188, no. 1, pp. 407–410, Nov. 2001. 

Mastro, M.A., Kryliouk, O.M., Reed, M.D., 

Anderson, T.J., Davydov, A.V., and Shapiro, A.J., 

“Thermal stability of MOCVD and HVPE GaN layers 

in H2, HCl, NH3 and N2,” Physica Status Solidi 

A-Applied Research, vol. 188, no. 1, pp. 467–471, 

Nov. 2001. 

Motayed, A., Davydov, A.V., Bendersky, L.A., 

Wood, M.C., Derenge, M.A., Wang, D.F., Jones, K.A., 

and Mohammad, S.N., “Novel high-transparency Ni/Au 

bilayer contacts to n-type GaN.” Journal of Applied 

Physics, 2002, (in press). 

Soukhoveev, V., Ivantsov, V., Melnik, Y., Davydov, A.V., 

Tsvetkov, D., Tsevetkova, K., Nikitina, I., Zubrilov, A., 

Lavrentiev, A., and Dmitriev, V., “Characterization of 

2.5-inch diameter bulk GaN grown from melt-solution.” 

Physica Status Solidi A-Applied Research, vol. 188, 

no. 1, pp. 411– 414, Nov. 2001. 

Tsvetkov, D., Melnik, Y., Davydov, A.V., Shapiro, A.J., 

Kovalenkov, O., Lam, J.B., Song, J.J., and Dmitriev, V., 

“Growth of submicron AlGaN/GaN/AlGaN 

heterostructures by hydride vapor phase epitaxy 

(HVPE).” Physica Status Solidi A-Applied Research, 

vol. 188, no. 1, pp. 429– 432, Nov. 2001. 

Combinatorial Methods for Thin Films 

Bendersky, L.A., Lu, C.J., Scott, J.H., Takeuchi, I., 

and Chang, K., “Microstructure and microstructural 

evolution in BaTiO3 films fabricated using the 

combinatorial precursor method.” Journal of Materials 

Research, 2002. 

Chang, K., Aronova, M., Famodu, O., HattrickSimpers, J., Lofland, S.E., Takeuchi, I., Lu, C.J., 

Bendersky, L.A., and Chang, H., “Fabrication and 

characterization of in-situ grown epitaxial Ba1-xSrxTiO3 

composition spreads.” Materials Research Society 

Proceedings, 2001, (in press). 

Hewes, J. and Bendersky, L.A., “High throughput 

method for materials R&D: A growing effort at NIST.” 

Applied Surface Science, vol. 7736, pp. 1, 2002. 

Reaction Path Analysis in 

Multicomponent Systems 

Campbell, C.E., Boettinger, W.J., and Kattner, U.R., 

“Development of a diffusion mobility database for 

Ni-base superalloys.” Acta Materialia, vol. 50, 

pp. 775–792, 2002. 

Thermodynamic Databases for 

Industrial Processes 

Ågren, J., Hayes, L., Höglund, L., Kattner, U.R., 

Legendre, B., and Schmid-Fetzer, R., “Applications of 

computational thermodynamics.” Zeitschrift Fur 

Metallkunde, vol. 93, pp. 128–142, 2002. 

Boettinger, W.J. and Kattner, U.R., “Simulation 

of DTA measurements from calculated enthalpytemperature data.” Metallurgical and Materials 

Transactions A, vol. 33, pp. 1779–1794, 2002. 

Davydov, A.V., Boettinger, W.J., Kattner, U.R., 

and Anderson, T.J., “Thermodynamic assessment of 

the gallium-nitrogen system.” Physica Status Solidi 

A-Applied Research, vol. 188, no. 1, pp. 407– 410, 

Nov. 2001. 

Davydov, A.V., Kattner, U.R., Josell, D., 

Blendell, J.E., Waterstrat, R.M., Shapiro, A.J., and 

Boettinger, W.J., “Determination of the CoTi congruent 

melting point and re-assessment of the Co-Ti system.” 

Metallurgical and Materials Transactions A, vol. 32, 

pp. 2175–2186, 2001. 

Kattner, U.R., “Construction of a thermodynamic 

database for Ni-base superalloys: a case study,” 

pp. 147–164, 2002, Warrendale, PA, TMS. 

Proceedings of CALPHAD and Alloy Thermodynamics. 

Turchi, P. E. A., Gonis, A., and Shull, R. D. 

Kattner, U.R., “Phase diagrams for solder alloys.” 

Journal of The Minerals, Metals & Materials Society, 

2002, (in press). 

Electrodeposited Coating Thickness Standards 

Beauchamp, C.R., Gates, H.B., Kelley, D.R., 

and Leigh, S.D., “Using magnetic methods for the 

measurement of coating thickness.” National Institute 

of Standards and Technology Recommended Practice 

Guide Series, 2002, (in press). 

54 
Metallurgy Division FY02 Annual Report Publication List


Microstructural Origins of Surface Roughening 

and Strain Localizations 

Banovic, SW. and Foecke, T., “Correlations of 

texture and roughening during in-plane balanced 

biaxial straining in 5XXX series aluminum alloys,” 

pp. 112–115, 2002, Fulton, MD, NEAT Press. 

Proceedings of Plasticity ’02: Plasticity, Damage and 

Fracture at Macro, Micro and Nano Scales. Khan, A.S. 

and Lopez–Pamies, O. 

Banovic, S.W. and Foecke, T., “Development of 

strain induced surface topography of 6XXX series 

aluminum sheet under balanced biaxial tension,” 

2002, Warrendale, PA, TMS. Aluminum 2002. 

Skillingberg, M.H. and Das, S.K. 

Banovic, S.W. and Foecke, T., “Evolution of 

strain-induced microstructure and texture in commercial 

aluminum sheet under balanced biaxial stretching.” 

Metallurgical and Materials Transactions A, 2002, 

(in press). 

Banovic, S.W. and Foecke, T., “The effect of 

microstructural variables on the surface roughening 

of 5XXX series aluminum sheet in biaxial tension,” 

02M-98, 2002, Warrendale, PA, SAE. Proceedings 

of SAE 2002 World Congress. 

Shim, Y., Stoudt, M.R., Levine, L.E., Banovic, S.W., 

and Fields, R.J., “Material model for strain-induced 

surface roughening of sheet metal,” 2002, Seoul, 

Korea. 5th International Conference & Workshop on 

Numerical Simulation of 3D Sheet Forming Processes. 

Stoudt, M.R., “The influence of surface roughness 

on the deforming friction behavior of Al-Mg alloys.” 

Demeri, M., “Innovations in Processing and 

Manufacturing of Sheet Materials,” pp. 237–244, 

2002, Warrendale, PA, TMS. Automotive Alloys, 

2002. Skillingberg, M.H. and Das, S.K., (in press). 

Stoudt, M.R. and Ricker, R.E., “The relationship 

between grain size and the surface roughening 

behavior of Al–Mg alloys.” Metallurgical and Materials 

Transactions A 33, 2002, (in press). 

Underlying Processes of Plastic Deformation 

Levine, L.E., Thomson, R., Savage, M.F., 

Kramer, D.E., and Shim, Y., “Single-crystal plasticity: 

statistical physics and experiments,” pp. 75–77, 2002, 

Fulton, MD, Neat Press. Proceedings of Plasticity ’02: 

Plasticity, Damage and Fracture at Macro, Micro and 

Nano Scales. Khan, A.S. and Lopez-Pamies, O. 

Roytburd, A. and Slutsker, J., “Coherent phase 

equilibria in a bending film.” Acta Materialia, vol. 50, 

pp. 1809-1824, 2002. 

Roytburd, A. and Slutsker, J., “Theory of multilayer 

SMA actuators.” Materials Transactions, vol. 43, 

pp. 1115–1125, 2002. 

Shim, Y., Levine, L.E., and Thomson, R., “Critical 

behavior of a strain percolation model for metals.” 

Physical Review E, vol. 65, p. 046146, 2002. 

Shim, Y., Levine, L.E., Thomson, R., and 

Kramer, D.E., “Asymptotic behavior of a strain 

percolation model for a deforming metal,” in 

Landau, D.P. (ed.). Computer Simulation Studies in 

Condensed-Matter Physics XV, Heidelberg, Germany: 

Springer Verlag, 2002, (in press). 

Shim, Y., Levine, L.E., Thomson, R., and 

Savage, M.F., “Critical behavior of a strain percolation 

model for metals with unstable locks.” Physica A, 2002, 

(submitted). 

Slutsker, J. and Roytburd, A., “Deformation of 

heterogeneous adaptive composite.” Materials 

Transactions, vol. 43, pp. 1001–1007, 2002. 

Slutsker, J. and Roytburd, A., “Control of intrinsic 

instability of superelastic deformation.” International 

Journal of Plasticity, 2002, (in press). 

Slutsker, J., Artemev, A., and Roytburd, A., 

“Morphological transitions of elastic domain structures 

in constrained layers.” Journal of Applied Physics, 

vol. 91, pp. 9049–9058, 2002. 

Thomson, R., Levine, L.E., and Shim, Y., 

“Deformation of metals,” 2002, Santa Fe, PA, 2002. 

Conference on Non-Linear Systems, (in press). 

Thomson, R., Levine, L.E., Shim, Y., Savage, M.F., 

and Kramer, D.E., “A multi-scale theoretical scheme for 

metal deformation.” Comp.Mod.in Eng.& Sci., vol. 3, 

pp. 245–253, 2002. 

Anelasticity and Springback Predictability 

Dayan, D., Pitchure, D., and Ricker, R.E., “Anelastic 

effects due to precipitation in the commercial Al-Mg-Si 

alloy (6061).” Washington Editorial Review Board, 

2002, (in press). 

Dayan, D., Pitchure, D., Savage, M.F., and 

Ricker, R.E., “Internal friction effects in pure Al and in 

Al-1 atomic percent Cu.” Washington Editorial Review 

Board, 2002, (in press). 

55 
Metallurgy Division FY02 Annual Report Publication List


Mechanism of Sn Whisker Growth 

from Electrodeposits 

Moon, K.-W., Williams, M.E., Johnson, C.E., 

Stafford, G.R., Handwerker, C.A., and Boettinger, W.J., 

“The formation of whiskers on electroplated Sn 

containing Cu.” Hanada, S., Zhong, Z., Nam, S.W., and 

Wright, R.N., pp. 1115–1118, 2001, Sendai, Japan, 

The Japanese Institute of Metals. Proceedings of 

the Fourth Pacific Rim International Conference on 

Advanced Materials and Processing. 

Williams, M.E., Johnson, C.E., Moon, K.-W., 

Stafford, G.R., Handwerker, C.A., and Boettinger, W.J., 

“Whisker formation on electroplated Sn-Cu,” pp. 31–39, 

2002, Orlando, FL, American Electroplaters and 

Surface Finishers Society, Inc. Proceedings of the 

American Electroplaters and Surface Finishers Society 

(AESF) SUR/FIN 2002 Annual International Technical 

Conference. 

Superconformal Film Growth: 

Measurements and Modeling 

Baker, B.C., Freeman, M., Melnick, B., 

Wheeler, D., Josell, D., and Moffat, T.P., 

“Superconformal electrodeposition of silver from a 

KAg(CN)2 - KCN - KSeCN electrolyte.” Journal of 

the Electrochemical Society, 2002, (submitted). 

Josell, D., Baker, B.C., Witt, C., Wheeler, D., 

and Moffat, T.P., “Via filling by electrodeposition: 

Superconformal silver and copper and conformal nickel.” 

Journal of the Electrochemical Society, 2002, (in press). 

Josell, D., Kim, S., Wheeler, D., Moffat, T.P., and 

Pyo, S.G., “Interconnect fabrication by superconformal 

iodine-catalyzed chemical vapor deposition of copper.” 

Journal of the Electrochemical Society, 2002, (submitted). 

Josell, D., Kim, S., Wheeler, D., Moffat, T.P., 

and Pyo, S.G., “Superconformal deposition by 

iodine-catalyzed chemical vapor deposition.” Journal 

of the Electrochemical Society, 2002, (submitted). 

Josell, D., Wheeler, D., Huber, W.H., Bonevich, J.E., 

and Moffat, T.P., “A simple equation for predicting 

superconformal electrodeposition in submicrometer 

trenches.” Journal of the Electrochemical Society, 

vol. 148, no. 12, pp. C767– C773, 2001. 

Josell, D., Wheeler, D., and Moffat, T.P., “Catalyst 

induced superconformal filling: electrodeposition and 

chemical vapor deposition.” McKerrow, A.J., ShachamDiamand, Y., Zaima, T., and Ohba, T. pp. 363–369. 

2002. Warrendale, PA, Materials Research Society. 

Advanced Metallization Conference 2001 (AMC 2001). 

Josell, D., Wheeler, D., and Moffat, T.P., 

“Superconformal deposition by surfactant-catalyzed 

chemical vapor deposition.” Electrochemical and 

Solid-State Letters, vol. 5, no. 3, pp. C44–C47, 2002. 

Josell, D., Wheeler, D., and Moffat, T.P., 

“Superconformal electrodeposition in submicron 

features,” pp. 385–390, 2001, Santa Clara, CA. 

2001 Proceedings Eighteenth International VLSI 

Multilevel Interconnect Conference (VMIC). 

Josell, D., Wheeler, D., and Moffat, T.P., 

“Superconformal electrodeposition in vias,” 

Electrochemical and Solid-State Letters, vol. 5, no. 4, 

pp. C49–C52, 2002. 

Moffat, T.P., Baker, B.C., Wheeler, D., 

Bonevich, J.E., Edelstein, M., Kelley, D.R., Gan, L., 

Stafford, G.R., Chen, P.J., Egelhoff, W.F., and Josell, D., 

“Superconformal electrodeposition of silver in submicron 

features.” Journal of the Electrochemical Society, 

vol. 149, no. 8, pp. C423–C428, 2002. 

Moffat, T.P., Wheeler, D., Witt, C., and Josell, D., 

“Superconformal electrodeposition using derivitized 

substrates.” Electrochemical and Solid-State Letters, 

2002, (submitted). 

Pyo, S.G., Kim, S., Wheeler, D., Moffat, T.P., and 

Josell, D., “Seam-free fabrication of sub-micrometer 

copper interconnects by iodine-catalyzed chemical vapor 

deposition.” Journal of Applied Physics, 2002,(submitted). 

Pyo, S.G., Kim, S., Wheeler, D., Moffat, T.P., and 

Josell, D., “Superconformal deposition by iodinecatalyzed chemical vapor deposition.” Journal of Applied 

Physics, 2002, (submitted). 

Wheeler, D., Josell, D., and Moffat, T.P., “Modeling 

superconformal electrodeposition in trenches,” 2002, 

San Diego, CA. Proceeding of I Therm 2002, (in press). 

Wheeler, D., Josell, D., and Moffat, T.P., “Modeling 

superconformal electrodeposition using the level set 

method.” Journal of the Electrochemical Society, 2002, 

(submitted). 

Solder and Solderability Measurements 

for Microelectronics 

Boettinger, W.J., Handwerker, C.A., Newbury, B., 

Pan, T.Y., and Nicholson, J.M., “Mechanism of fillet 

lifting in Sn-Bi alloys.” Journal of Electronic Materials, 

vol. 31, no. 5, pp. 545–550, 2002. 

Boettinger, W.J. and Kattner, U.R., “On Differential 

Thermal Analyzer curves for the melting and freezing 

of alloys.” Metallurgical and Materials Transactions A, 

vol. 33, no. 6, pp. 1779–1794, 2002. 

Bradley, E., Charbonneau, R., Bath, J., 

Handwerker, C.A., Parker, R., Sohn, J., and Gedney, R., 

“Lead-free soldering trends in the U.S. NEMI Pb-free 

task group,” pp. 134–139, 2001. Proceedings of 

JISSO/PROTEC Forum Japan 2001. 

56 
Metallurgy Division FY02 Annual Report Publication List


Handwerker, C.A., Noctor, D., and Whitten, G., 

“Reliability of lead-free solders,” in Hwang, J.S. (ed.). 

Environment-friendly electronics: lead-free technology, 

Electrochemical Publications LTD, pp. 566–589, 2001. 

Josell, D., Wallace, W.E., Warren, J.A., and 

Wheeler, D., “Misaligned flip-chip solder joints: prediction 

and experimental determination of force-displacement 

curves.” Journal of Electronic Packaging, 2002, (in press). 

Kattner, U.R., “Phase diagrams for solder alloys.” 

Journal of The Minerals, Metals & Materials Society, 

2002, (in press). 

Lewis, D.J., Allen, S.L., and Notis, M.R., 

“Ag-Cu-Sn eutectic structure determination.” Journal of 

Electronic Materials, vol. 31, no. 2, pp. 161–167, 2002. 

Magnetic Properties of 

Nanostructured Materials 

Chien, C.L., Gornakov, V.S., Nikitenko, V.I., 

Shapiro, A.J., and Shull, R.D., “Dynamic 

antiferromagnetic spin structure and domains in 

exchange-coupled multilayers,” 2002, Amsterdam, 

Netherlands. Proceedings of Intermag, (in press). 

Gornakov, V.S., Nikitenko, V.I., Egelhoff, W.F., 

McMichael, R.D., Shapiro, A.J., and Shull, R.D., 

“Anomalous switching behavior of antiparallel-coupled 

Co layers separated by a super thin Ru spacer.” Journal 

of Applied Physics, vol. 91, no. 10, pp. 8272– 8274, 

2002. 

Gornakov, V.S., Nikitenko, V.I., Shapiro, A.J., 

Shull, R.D., Jiang, J.S., and Bader, S.D., “Direct 

experimental study of the exchange spring formation 

process.” Journal of Magnetism and Magnetic Materials, 

vol. 246, no. 1–2, pp. 80– 85, Apr. 2002. 

Jiang, J.S., Bader, S.D., Kaper, H., Leaf, G.K., 

Shull, R.D., Shapiro, A.J., Gornakov, V.S., Nikitenko, V.I., 

Platt, C.L., Berkowitz, A.E., David, S., and Fullerton, E.E. 

“Rotational hysteresis of exchange-spring magnets.” 

Journal of Physics D-Applied Physics, 2002, (in press). 

King, T.T., Rowlett, B.A., Ramirez, R.A., Shirron, P.J., 

Canavan, E.R., DiPirro, M.J., Panek, J.S., Tuttle, J.G., 

Shull, R.D., and Fry, R.A., “Rare-earth garnets and 

perovskites for space-based ADR cooling at high T 

and low H,” 613[1], pp. 1191–1200, 5-10-2002. 

American Institute of Physics Conference Proceedings. 

Nikitenko, V.I., Gornakov, V.S., Kabanov, Y.P., 

Shapiro, A.J., Shull, R.D., Chien, C.L., Jiang, J.S., 

and Bader, S.D., “Magneto-optic indicator film study of 

the hybrid exchange spring formation and evolution 

processes.” Journal of Magnetism and Magnetic 

Materials, 2002, (in press). 

Shapiro, A.J., Gornakov, V.S., Nikitenko, V.I., 

McMichael, R.D., Egelhoff, W.F., Tahk, Y.W., Shull, R.D., 

and Gan, L., “Features of domain nucleation and growth 

in Co/Ru/Co synthetic antiferromagnets deposited 

on obliquely sputtered Ta underlayers.” Journal of 

Magnetism and Magnetic Materials, vol. 240, no. 1–3, 

pp. 70–72, Feb. 2002. 

Taketomi, S. and Shull, R.D., “Experimental study 

of magnetic interactions between colloidal particles in 

magnetic fluids.” Virtual Journal of Nanoscale Science 

and Technology, vol. 5, no. 22, 2002. 

Taketomi, S. and Shull, R.D., “Experimental study 

of magnetic interactions between colloidal particles in 

magnetic fluids.” Journal of Applied Physics, vol. 91, 

no. 10, pp. 8546– 8548, 2002. 

Taketomi, S. and Shull, R.D., “Magnetic behavior 

of yttrium-iron-garnet nanoparticles dispersed in glass 

composites.” Virtual Journal of Nanoscale Science and 

Technology, vol. 5, no. 22, 2002. 

Taketomi, S. and Shull, R.D., “Magnetic behavior 

of yttrium-iron-garnet nanoparticles dispersed in glass 

composites.” Journal of Applied Physics, vol. 91, 

no. 10, pp. 8468–8470, 2002. 

Yang, F.Y., Shang, C.H., Chien, C.L., Ambrose, T., 

Krebs, J.J., Prinz, G.A., Nikitenko, V.I., Gornakov, V.S., 

Shapiro, A.J., and Shull, R.D., “Multi-step magnetic 

switching in single-crystal (001) Co2MnGe films.” 

Physical Review B, vol. 65, no. 17, pp. 174410-1– 

174410-8, May 2002. 

Zheng, L.A., Barrera, E.V., and Shull, R.D., 

“Formation and stabilization of nanosize grains in 

ferromagnetic thin films by dispersed C60.” Journal of 

Applied Physics, vol. 92, no. 1, pp. 523–530, 2002. 

Nanomagnetodynamics 

Kunz, A.B. and McMichael, R.D., “Normal mode 

mixing and ferromagnetic resonance linewidth.” IEEE 

Transactions on Magnetics, 2002, (in press). 

McMichael, R.D. and Kunz, A.B., “Calculation of 

damping rates in thin magnetic films due to coupling to 

lattice vibrations.” Journal of Applied Physics, vol. 91, 

no. 10, pp. 8650–8652, 2002. 

Russek, S.E., Kabos, P., McMichael, R.D., Lee, C.G., 

Bailey, W.E., Ewasko, R., and Sanders, S.C., 

“Magnetostriction and angular dependence of 

ferromagnetic resonance linewidth in Tb-doped 

Ni_{0.8}Fe_{0.2} thin films.” Journal of Applied 

Physics, vol. 91, no. 10, pp. 8659–8661, 2002. 

57 
Metallurgy Division FY02 Annual Report Publication List


New Materials for Ultra-High Density 

Data Storage 

Borg, H.J., Bussman, K., Egelhoff, W.F., Hesselink, L., 

Majetich, S.A., Murdock, E.S., Stadler, B.J.H., 

Vasquez, M., Wuttig, M., and Xaio, J.Q., “Applications 

of ferromagnetic and optical materials, storage, and 

magnetoelectronics.” MRS Symposium Proceedings, 

p. 674, 2001, Pittsburgh, PA, Materials Research 

Society Press. 

Araújo, A.E.P., Machado, F.L.A., Rodrigues, A.R., 

Azevedo, A., de Aguiar, F.M., de Almeida, J.R.L., 

Rezende, S.M., and Egelhoff, W.F., “Spin-glass and 

random-field effects in exchanged-biased NiFe film 

on a NiO single-crystal substrate.” Journal of Applied 

Physics, vol. 91, no. 10, pp. 7754–7756, 2002. 

Bae, S., Chen, P.J., Egelhoff, W.F., and Judy, J.H., 

“Effects of sputtering angle on surface roughness, 

chemical composition, and GMR behavior of NiO and 

α-Fe2O3 bottom spin-valves.” IEEE Transactions on 

Magnetics, 2002, (submitted). 

Bae, S., Chen, P.J., Egelhoff, W.F., Zurn, S., 

Sheppard, L., Torok, E.J., and Judy, J.H., 

“Magnetoelectronic characteristics of a GMR 

transpinnor and a magnetic random access memory 

using a closed-flux NiFe/Cu/CoFe/Cu/NiFe pseudo 

spin-valve.” Journal of Applied Physics, vol. 91, no. 10, 

pp. 8414 – 8416, 2002. 

Bae, S., Judy, J.H., Chen, P.J., Egelhoff, W.F., 

Shayne, Z., Sheppard, L., and Torok, E.J., 

“Application of α-Fe2O3 bottom GMR spin-valves for 

magnetoresistive random access memory (MRAM).” 

Japan Society of Powder and Powder Metallurgy, vol. 8 

pp. 1111, 2001. 

Bae, S., Judy, J.H., Chen, P.J., Gan, L., Egelhoff, W.F., 

Hautala, J., and Fenner, D.B., “Effects of Ar gas cluster 

ion beam (GCIB) processing on surface roughness, 

crystalline orientation texture, magnetic, and giant 

magnetoresistance (GMR) properties of reactively RF 

sputtered α-Fe2O3 bottom GMR spin valves.” IEEE 

Transactions on Magnetics, 2002, (in press). 

Bae, S., Zurn, S., Chen, P.J., Egelhoff, W.F., 

Sheppard, L., Torok, E.J., and Judy, J.H., “Fabrication 

and thermal-chemical stability of magnetoresistive 

random-access memory cells using α-Fe2O3 bottom 

spin valves.” IEEE Transactions on Magnetics, vol. 37, 

no. 6, pp. 3960–3968, 2001. 

Bae, S., Zurn, S., Egelhoff, W.F., Chen, P.J., 

Sheppard, L., Torok, E.J., and Judy, J.H., 

“Magnetoelectronic devices using α-Fe2O3 bottom 

GMR spin valves.” IEEE Transactions on Magnetics, 

vol. 37, no. 4–1, pp. 1986–1988, July 2001. 

Chopra, H.D., Yang, D.X., Chen, P.J., and 

Egelhoff, W.F., “Domain structure and magnetoelastic 

properties of Fe/Pd ferromagnetic thin films and 

multilayers.”Journal of Applied Physics, 2002,(submitted). 

Chopra, H.D., Yang, D.X., Chen, P.J., and 

Egelhoff, W.F., “Pb-Ag as a mixture-surfactant in atomic 

engineering of spin valves.” Journal of Applied Physics, 

2002, (submitted). 

Chopra, H.D., Yang, D.X., Chen, P.J., and 

Egelhoff, W.F., “Surfactant assisted atomic level 

engineering of spin valves.” Physical Review B, vol. 65, 

no. 9, pp. 094433-1–094433-7, Mar. 2002. 

Chung, S.H., García, N., Egelhoff, W.F., and 

Gomez, R.D., “Universal behavior of ballistic 

magnetoresistance versus scaled conductance in atomic 

nanocontacts.” Washington Editorial Review Board, 

2002, (in press). 

Egelhoff, W.F., Chen, P.J., Powell, C.J., and 

McMichael, R.D., “Surface and interface effects in 

the growth of giant magnetoresistance spin valves for 

ultrahigh-density data-storage applications.” Progress in 

Surface Science, vol. 67, no.1– 8, pp. 355–364, 2001. 

Egelhoff, W.F., Gan, L., Chen, P.J., Powell, C.J., 

McMichael, R.D., Fry, R.A., Beach, G., Martien, D., 

and Berkowitz, A.E., “Detection of pinholes in ultrathin 

films by magnetic coupling.” MRS Symposium 

Proceedings, p. 674, T1.2.1. 2001. 

Egelhoff, W.F., Stiles, M.J., Pappas, D.L., 

Pierce, D.T., Byers, J.M., Johnson, M.E., Jonker, B.T., 

Alvarado, S.F., Gregg, J.F., Bland, J.A.C., and 

Buhrman, R.A., “Spin polarization of injected 

electrons.” Science, vol. 296, no. 5571, pp. 1195, 

May 2002. 

Gan, L., Gomez, R.D., Castillo, A., Chen, P.J., 

Powell, C.J., and Egelhoff, W.F., “Ultra-thin aluminum 

oxide as a thermal oxidation barrier on metal films.” 

Thin Solid Films, 2002, (submitted). 

Gan, L., McMichael, R.D., Chen, P.J., Egelhoff, 

W.F., and Lee, C.G., “Al, Au, Cu, Ni, Ta, and Fe films as 

oxidation barriers for the Co surface in air.” Thin Solid 

Films, 2002, (in press). 

Gornakov, V.S., Nikitenko, V.I., Egelhoff, W.F., 

McMichael, R.D., Shapiro, A.J., and Shull, R.D., 

“Anomalous switching behavior of antiparallel-coupled 

Co layers separated by a super thin Ru spacer.” Journal 

of Applied Physics, vol. 91, no. 10, pp. 8272–8274, 

2002. 

Huang, H., Seu, K., Egelhoff, W.F., and Reilly, A., 

“Ultrafast pump-probe laser spectroscopy of the 

half-metal CrO2.” Journal of Applied Physics, 2002, 

(submitted). 

58 
Metallurgy Division FY02 Annual Report Publication List


Lee, C.G., Jung, J.G., McMichael, R.D., Fry, R.A., 

Chen, A., Egelhoff, W.F., and Gornakov, V.S., 

“Structural, magnetic, and thermal stability of IrMn 

exchange biased layers.” Journal of Applied Physics, 

vol. 91, no. 10, pp. 8566–8568, 2002. 

Menyhard, M., Zsolt, G., Chen, P.J., Powell, C.J., 

McMichael, R.D., and Egelhoff, W.F., “Structural effects 

in the growth of giant magnetoresistance (GMR) spin 

valves.” Applied Surface Science, vol. 180, no. 3–4, 

pp. 315–321, Aug. 2001. 

McMichael, R.D., Twisselmann, D.J., Bonevich, J.E., 

Chen, P.J., Egelhoff, W.F., and Russek, S.E., 

“Ferromagnetic resonance mode interactions in 

periodically perturbed films.” Journal of Applied Physics, 

vol. 91, no. 10, pp. 8647– 8649, May 2002. 

Moffat, T.P., Baker, B.C., Wheeler, D., Bonevich, J.E., 

Edelstein, M., Kelley, D.R., Gan, L., Stafford, G.R., 

Chen, P.J., Egelhoff, W.F., and Josell, D., “Superconformal 

electrodeposition of silver in submicron features.” 

Journal of the Electrochemical Society, vol. 149, no. 8, 

pp. C423–C428, 2002. 

Muñoz, M., Qian, G.G., Karar, N., Cheng, H., 

Saveliev, I.G., García, N., Moffat, T.P., Chen, P.J., 

Gan, L., and Egelhoff, W.F., “Ballistic magnetoresistance 

in a nanocontact between a Ni cluster and a magnetic 

thin film.” Applied Physics Letters, vol. 79, no. 18, 

pp. 2946–2948, 2001. 

Repetski, E.J., Yang, D.X., Chopra, H.D., Chen, P.J., 

and Egelhoff, W.F., “Improved interfaces and magnetic 

properties in spin valves using a Ni80Fe20 seed layer.” 

Journal of Applied Physics, vol. 91, no. 6, pp. 3891–3895, 

2002. 

Repetski, E.J., Yang, D.X., Chopra, H.D., Chen, P.J., 

and Egelhoff, W.F., “Modification of interface and magnetic 

properties in giant magnetoresistance spin valves using 

seed layers.” Acta Materialia, 2002, (submitted). 

Rezende, S.M., Azevedo, A., de Aguiar, F.M., 

Fermin, J.R., Egelhoff, W.F., and Parkin, S.S.P., 

“Three-layer model for exchange anisotropy.” 

Washington Editorial Review Board, 2002, (in press). 

Sanz, M., Papageorgopoulos, A., Egelhoff, W.F., 

Nieto-Vesperinas, M., and García, N., “Wedge-shaped 

absorbing samples look left handed: the problem of 

interpreting negative refraction, and it’s solution.” 

Science, 2002, (submitted). 

Seu, K., Huang, H., Showman, J.L., Showman, H., 

and Egelhoff, W.F., “Magneto-optical Kerr effect studies 

of Co layer thickness dependence of exchange biasing of 

IrMn/Co and FeMn/Co.” Journal of Applied Physics, 

2002, (submitted). 

Shapiro, A.J., Gornakov, V.S., Nikitenko, V.I., 

McMichael, R.D., Egelhoff, W.F., Tahk, Y.W., Shull, R.D., 

and Gan, L., “Features of domain nucleation and 

growth in Co/Ru/Co synthetic antiferromagnets 

deposited on obliquely sputtered Ta underlayers.” 

Journal of Magnetism and Magnetic Materials, vol. 240, 

no. 1–3, pp. 70–72, Feb. 2002. 

Siu, I.L., Egelhoff, W.F., Chopra, H.D., and 

Wang, D.X., “Magnetization reversal in epitaxial CrO2 

films.” Journal of Applied Physics, 2002, (in press). 

Torok, E.J., Zurn, S., Bae, S., Chen, P.J., 

Egelhoff, W.F., Sheppard, L., Spitzer, R., and Judy, J.H., 

“Transpinnor: a new giant magnetoresistive spin-valve 

device.” IEEE Transactions on Magnetics, 2002,(in press). 

Yang, D.X., Chopra, H.D., Shashishekar, B., 

Chen, P.J., and Egelhoff, W.F., “Carbon, a bane for 

giant magnetoresistance magnetic multilayers.” Applied 

Physics Letters, vol. 80, no. 16, pp. 2943–2945, 2002. 

Yang, D.X., Repetski, E.J., Chopra, H.D., 

Spencer, B.J., Parks, D.C., Chen, P.J., and Egelhoff, W.F., 

“Pinhole coupling strength in giant magnetoresistance spin 

valves: a statistical approach.” Physical Review B, 2002, 

(submitted). 

Hardness Standardization: 

Rockwell, Vickers, Knoop 

Low, S.R., “An empirical approach to determining 

Rockwell hardness measurement uncertainty,” 2002, 

Celle, Germany. Joint International Conference of 

IMEKO TC3/TC5/TC20. 

Low, S.R. and Song, J., “Worldwide comparisons of 

Rockwell hardness scales that use a diamond indenter,” 

2002, San Diego, CA. NCSL International 2002 

Workshop & Symposium. 

Ma, L., Low, S.R., and Song, J., “Comparison of 

Rockwell B hardness (HRB) tests using steel and 

tungsten carbide ball indentation,” 2002, Celle, 

Germany. IMEKO TC3/TC5/TC20 Joint International 

Conference. 

Ma, L., Low, S.R., Zhou, J., Song, J., and deWit, 

R., “Simulation and prediction of hardness performance 

of Rockwell diamond indenters using finite element 

analysis.” Journal of Testing and Evaluation, 2002, 

(in press). 

Ma, L., Zhou, J., Lau, A., Low, S.R., and deWit, R., 

“Self-similarity simplification approaches for the 

modeling and analysis of Rockwell hardness 

indentation.” Journal of Applied Mechanics, 2002. 

Ma, L., Zhou, J., Low, S.R., and Song, J., “FEA 

modeling and hardness performance prediction of 

Rockwell diamond indenters,” 2001, Washington, D.C. 

2001 NCSL Workshop and Symposium. 

59 
Metallurgy Division FY02 Annual Report Publication List


Song, J.F., Low, S.R., and Ma, L., “Tolerancing 

form deviations for Rockwell diamond indenters,” 2002, 

Celle, Germany. Joint International Conference of 

IMEKO TC3/TC5/TC20. 

Deformation Mechanisms and


Constitutive Laws in Thin Film Superlattices


Foecke, T., “A new sample geometry for in situ 

TEM tensile testing of brittle materials.” 

Ultramicroscopy, 2002, (in press). 

Foecke, T. and Kramer, D.E., “Observations of 

deformation and fracture mechanisms in nanolayered 

metallic structures,” pp. 370–373, 2002, Fulton, MD, 

NEAT Press. Proceedings of Plasticity ’02: Plasticity, 

Damage and Fracture at Macro, Micro and Nano Scales. 

Khan, A.S. and Lopez–Pamies, O. 

Josell, D., Weihs, T.P., and Gao, H., “Diffusional 

creep: stress and strain rate in thin films and multilayers.” 

Materials Research Bulletin, vol. 27, no. 1, pp. 39–44, 

Jan. 2002. 

Kramer, D.E. and Foecke, T., “Observations of 

deformation and fracture in metallic nanolaminates.” 

Philosophical Magazine A, 2002, (in press). 

Mann, A.B., Tapson, J., van Heerden, D., Lewis, A.C., 

Josell, D., and Weihs, T.P., “Apparatus to measure wafer 

curvature for multilayer systems in a vacuum furnace.” 

Review of Scientific Instruments, vol. 73, no. 4, 

pp. 1821–1827, 2002. 

Nanoscale Characterization: 

Electron Microscopy 

Armstrong, N., Kalceff, W., Cline, J.P., and 

Bonevich, J.E., “Bayesian inference of nanoparticlebroadened x-ray line profiles.” Journal of Research of 

the National Institute of Standards and Technology, 

2002, (in press). 

Bendersky, L.A. and Gayle, F.W., “Electron 

diffraction at NIST: Transmission electron microscopy.” 

Journal of Research of the National Institute of Standards 

and Technology, vol. 106, no. 6, pp. 997, 2002. 

Bendersky, L.A., Krajewski, J.J., and Cava, R.J., 

“Dielectric properties and microstructure of 

Ca5Nb2TiO12 and Ca5Ta2TiO12 compounds.” 

Journal of European Ceramic Society, vol. 12, no. 14, 

pp. 2653–2658, 2001. 

Bendersky, L.A., Levin, I., Roth, R.S., and 

Shapiro, A.J., “Ca4Nb2O9-CaTiO3: Phase equilibria 

and microstructures.” Journal of Solid State Chemistry, 

vol. 160, pp. 257– 271, 2001. 

Chen, R., Greenblatt, M., and Bendersky, L.A., 

“Stabilization of the n=3 Ruddlesden– Popper phases: 

Sr4Mn3-xFexO10-δ and Sr4-yCayMn3O10-δ.” Chemistry 

of Materials, vol. 13, no. 11, pp. 4094–4100, 2001. 

Cresswell, M.W., Bonevich, J.E., Headley, T.J., 

Allen, R.A., Guillaume, N.M.P., Giannuzzi, L.A., 

Everist, S.C., Murabito, C.E., Shea, P.J., and 

Linholm, L.W., “Electrical linewidth test structures 

patterned in (100) silicon-on-insulator for use as CD 

standards.” IEEE Transactions on Semiconductor 

Manufacturing, vol. 14, no. 4, pp. 356–364, Nov. 2001. 

Fry, R.A., McMichael, R.D., Bonevich, J.E., 

Chen, P.J., Egelhoff, W.F., and Lee, C.G., “Thermal 

stability of Ta-pinned spin valves.” Journal of Applied 

Physics, vol. 89, no. 11, pp. 6825– 6827, 2001. 

Grey, I.E., Roth, R.S., Mumme, W.G., Planes, J., 

Bendersky, L.A., Li, C., and Chenavas, J., “Characterization 

of new 5M and 7M polytypes of Niobia-doped Ca2Ta2O7.” 

Journal of Solid State Chemistry, vol. 161, pp. 274, 2001. 

Higginson, K.A., Bonevich, J.E., Mattoussi, H., 

Qadri, S.B., Yousuf, M., and Kuno, M., “Synthesis and 

Characterization of Colloidal β-HgS Quantum Dots.” 

Journal of the American Chemical Society, 2002, (in 

press). 

Josell, D., Wheeler, D., Huber, W.H., Bonevich, J.E., 

and Moffat, T.P., “A simple equation for predicting 

superconformal electrodeposition in submicrometer 

trenches.” Journal of the Electrochemical Society, 

vol. 148, no. 12, pp. C767– C773, 2001. 

McMichael, R.D., Twisselmann, D.J., Bonevich, J.E., 

Chen, P.J., Egelhoff, W.F., and Russek, S.E., 

“Ferromagnetic resonance mode interactions in 

periodically perturbed films.” Journal of Applied Physics, 

vol. 91, no. 10, pp. 8647–8649, May 2002. 

Moffat, T.P., Baker, B.C., Wheeler, D., Bonevich, J.E., 

Edelstein, M., Kelley, D.R., Gan, L., Stafford, G.R., 

Chen, P.J., Egelhoff, W.F., and Josell, D., “Superconformal 

electrodeposition of silver in submicron features.” 

Journal of the Electrochemical Society, vol. 149, 

no. 8, pp. C423–C428, 2002. 

Punnoose, A., Magnone, H., Seehra, M.S., and 

Bonevich, J.E., “Bulk to nanoscale magnetism and 

exchange bias in CuO nanoparticles.” Physical Review 

B, vol. 64, no. 17, pp. 174420-1–174420-8, 2001. 

Stoudt, M.R., Ricker, R.E., and Cammarata, R.C., 

“The influence of a multilayered metallic coating on 

fatigue crack nucleation.” International Journal of 

Fatigue, vol. 23, no. 1001, pp. 215–223, 2001. 

Other 

Foecke, T. and Gerberich, W.W., “Emission of both 

blunting and jogging dislocations at crack tips in alkali 

halide single crystals.” Journal of Materials Research, 

2002. 

Hooper, J.J., Graham, L., Foecke, T., and Weihs, T.P., 

“The relationship between microstructure and mechanical 

properties of late 19th/early 20th century wrought iron 

using the generalized method of cells,” 2001. Materials 

Research Society. Symposium on Materials Conservation. 

60 
Metallurgy Division FY02 Annual Report Publication List


Hooper, J.J., Graham, L., Foecke, T., and Weihs, T.P., 

“The relationship between microstructure and mechanical 

properties of late 19th/early 20th century wrought iron 

using the generalized method of mells.” Scripta Materialia. 

2002, (submitted). 

Jovic, V., Jovic, B., and Stafford, G.R., “Composition 

and morphology changes and their influence on 

hydrogen evolution on Ni-Mo and Fe-Mo alloys 

electrodeposited by DC and pulsed current.” Surface 

Finishing (CD-ROM), 2002. 

Kass, M., Brooks, C.R., Falcon, D., and Basak, D., 

“The formation of defects in Fe-Al alloys: electrical 

resistivity and specific heat measurements.” 

Intermetallics, 2002, (in press). 

McCowan, C.N., Read, D.T., and Ricker, R.E., 

“Materials issues for replacement gates at Folsom dam,” 

2002. Bureau of Reclamation, Department of the 

Interior, (submitted). 

Ricker, R.E., “Modeling the influence of crack path 

deviations on the propagation of stress corrosion cracks.” 

Washington Editorial Review Board, 2002, (in press). 

Ricker, R.E. and Vasudevan, A.K., “The influence of 

grain boundary precipitation on the stress corrosion 

cracking of Al-Li and Al-Li-Cu alloys.” Washington 

Editorial Review Board, 2002, (in press). 

Shepherd, D.A. and Vasudevan, V.K., “The effect 

of molybdenum on the creep behavior of orthorhombic 

titanium aluminides,” 2002, Amsterdam, The Netherlands. 

Turbo Expo 2002 ASME and International Gas Turbine 

Institute (IGTI) Joint Conference. 

Shin, K., Wang, H., Satija, S.K., Han, C.C., and 

Josell, D., “X-ray reflectivity study of gold nanoparticles 

in a polymer matrix.” Materials Research Society 

Proceedings, 2001, (in press). 

61 

Metallurgy Division


Metallurgy Division


Chief


Carol A. Handwerker


Phone: 301–975–6158


E-mail: carol.handwerker@nist.gov


Deputy Chief 

Frank W. Gayle 

Phone: 301–975–6161 

E-mail: frank.gayle@nist.gov 

NIST Fellows 

William J. Boettinger 

Phone: 301–975–6160


E-mail: william.boettinger@nist.gov


John W. Cahn 

Phone: 301–975–5664 

E-mail: john.cahn@nist.gov 

Group Leaders 

Electrochemical Processing Group 

Gery R. Stafford 

Phone: 301–975–6412 

E-mail: gery.stafford@nist.gov 

Magnetic Materials Group 

Robert D. Shull 

Phone: 301–975–6035 

E-mail: robert.shull@nist.gov 

Materials Performance Group 

Stephen D. Ridder 

Phone: 301–975–6175


E-mail: stephen.ridder@nist.gov


Materials Structure and Characterization Group 

Frank W. Gayle 

Phone: 301–975–6161 

E-mail: frank.gayle@nist.gov 

Metallurgical Processing Group 

Stephen D. Ridder 

Phone: 301–975–6175


E-mail: stephen.ridder@nist.gov


63 
Research Staff


Research Staff


Banovic, Stephen W. 

E-mail:	 stephen.banovic@nist.gov 

Metal forming 

Mechanical properties 

Texture analysis 

Beauchamp, Carlos R. 

E-mail:	 carlos.beauchamp@nist.gov 

Compositionally modulated alloys 

Standard reference materials 

Baker, Brett C. 

E-mail: brett.baker@nist.gov 

Deposition of metals/alloys 

Bendersky, Leonid A. 

E-mail:	 leonid.bendersky@nist.gov 

Functional ceramics 

Analytical and high-resolution TEM 

High-temperature intermetallics 

Combinatorial methods 

Biancaniello, Frank S. 

E-mail:	 frank.biancaniello@nist.gov 

Spray deposition measurements and diagnostics 

Inert gas atomization: metal powder 

measurements and consolidation 

Nitrogenated steels, standard reference materials 

Special alloys, bulk metallic glasses 

Biomaterials 

Boettinger, William J. 

E-mail: william.boettinger@nist.gov 

Relation of alloy microstructures to processing 

conditions; solidification 

Thermal analysis 

Solder 

Bonevich, John E. 

E-mail:	 john.bonevich@nist.gov 

Electron holography 

Interfacial structure and chemistry 

High resolution/analytical electron microscopy 

Magnetic materials 

Boyer, Paul A. 

E-mail:	 paul.boyer@nist.gov 

Powder analysis 

Data management 

Vacuum technology 

Plasma spray 

Campbell, Carelyn E. 

E-mail:	 carelyn.campbell@nist.gov 

Transient liquid phase bonding 

Multicomponent diffusions simulations 

Alloy design methodology 

Claggett, Sandra W. 

E-mail:	 sandra.claggett@nist.gov 

Specimen preparation for electron microscopy 

Digital imaging 

Specimen preparation for scanning electron 

microscopy 

Image analysis 

Metallography of materials 

Specimen preparation for transmission of 

electron microscopy 

Drew, Rosetta V. 

E-mail:	 rosetta.drew@nist.gov 

Magnetometry 

Database maintenance 

Egelhoff Jr., William F. 

E-mail:	 william.egelhoff@nist.gov 

Giant magnetoresistance 

Molecular beam epitaxy 

Surface physics 

Ultrahigh density data storage 

Fields, Richard J. 

E-mail:	 richard fields@nist.gov 

Mechanical properties 

Mechanical testing 

Powder consolidation 

Metal forming 

Fink, James L. 

E-mail:	 james fink@nist.gov 

Hardness standards 

Hardness testing 

Mechanical properties measurement 

Metal powder consolidation 

Environmental corrosion 

Metallography 

Foecke, Timothy J. 

E-mail:	 timothy.foecke@nist.gov 

Metal forming standards 

Nanostructured materials 

Experimental fracture physics 

SEM, TEM, SPM 

Micro- and nano-mechanics of materials 

Dislocation-based deformation mechanisms 

Historical metallurgy and failure analysis 

Fry, Richard A. 

E-mail:	 richard. fry@nist.gov 

SQUID magnetometry 

Ferromagnetic resonance 

Magnetic dendrimer nanocomposites 

Giant magnetoresistance 

64 
Research Staff


Gates, Hilary G. 

E-mail: hilary.gates@nist.gov 

Standard reference materials 

Gayle, Frank W. 

E-mail:	 frank.gayle@nist.gov 

Structure/property relationships 

Transmission electron microscopy 

Aluminum metallurgy 

Solder science 

Guyer, Jonathan E. 

E-mail:	 jonathan.guyer@nist.gov 

III-V semiconductors 

Molecular beam epitaxy 

Alloy film deposition 

Stress-induced mass transport 

Handwerker, Carol A. 

E-mail:	 carol.handwerker@nist.gov 

Interface thermodynamics and kinetics 

Solder science 

Microstructure evolution 

Jiggetts, Rodney D. 

E-mail:	 rodney.jiggetts@nist.gov 

Substrate analysis 

Grit blasting 

Roughness measurements 

Metallography of coatings 

Image analysis 

Micro analysis/characterization 

Hot isostatic processing 

Johnson, Christian E. 

E-mail:	 christian.johnson@nist.gov 

Ultra-black coatings 

Electroless deposition processes 

Metallic glass alloy deposition 

Microhardness SRM research 

Chromium deposition 

Pulse alloy deposition 

Lead-free solder 

Josell, Daniel 

E-mail: daniel.josell@nist.gov 

Mechanical and thermal properties of 

multilayer materials 

Measurement and modeling of solder joint 

geometries 

Filling of sub-0.1mm features by 

electrodeposition 

Kattner, Ursula R. 

E-mail:	 ursula.kattner@nist.gov 

Computational thermodynamics 

Alloy phase equilibria evaluations 

Solder alloy systems 

Superalloy systems 

Kelley, David R. 

E-mail:	 david.kelley@nist.gov 

Microhardness SRM development 

Dye penetrant SRM development 

Precious metal electrodeposition 

Plating on aluminum 

Electroplating 

Kramer, Donald E. 

E-mail:	 donald.kramer@nist.gov 

Nanoindentation 

Atomic force microscopy 

Thin film mechanical behavior 

Transmission electron microscopy 

Nanostructured material 

Kunz, Andrew W. 

E-mail: akunz@nist.gov 

Micromagnetic calculations 

Levine, Lyle E. 

E-mail:	 lyle.levine@nist.gov 

Diffraction theory 

Dislocation-based deformation 

Synchrotron x-ray techniques 

Percolation theory 

TEM, SEM, SPM 

Lewis, Daniel J. 

E-mail:	 daniel.lewis@nist.gov 

Modeling of eutectic solidification 

Electric packaging 

Lobkovsky, Alexander E. 

E-mail:	 alexander.lobkovsky@nist.gov 

Formation and evolution of microstructure 

Plasticity 

Dynamics of crystalline defects 

Thermodynamics of fluid membranes 

Low II, Samuel R. 

E-mail:	 samuel.low@nist.gov 

Hardness standards 

Hardness testing 

Mechanical properties of materials 

Mechanical testing of materials 

Mates, Steven P. 

E-mail:	 steven.mates@nist.gov 

Compressible fluid flow 

Metal sprays 

Fluid flow visualization 

McMichael, Robert D. 

E-mail:	 robert mcmichael@nist.gov 

Giant magnetoresistance 

Micromagnetic modeling 

Ferromagnetic resonance 

Nanocomposites 

65 
Research Staff


Moffat, Thomas P. 

E-mail:	 thomas.moffat@nist.gov 

Electrochemistry 

Scanning probe microscopy 

Nanostructures 

Pierce Jr., Thomas A. 

E-mail:	 tpierce@nist.gov 

Hardness measurements 

Metallography 

Pitchure, David J. 

E-mail:	 david.pitchure@nist.gov 

Mechanical testing 

Computer-aided design 

Mechanical engineering 

Ricker, Richard E. 

E-mail:	 richard.ricker@nist.gov 

Corrosion 

Deformation mechanisms 

Fracture mechanisms (SCC, CF HE) 

TEM, SEM 

Ridder, Stephen D. 

E-mail:	 stephen.ridder@nist.gov 

Spray dynamics and deposition 

Thermal spray processes 

Process modeling and control 

Savage, Michael F. 

E-mail:	 michael.savage@nist.gov 

Mechanical behavior 

Dislocation deformation mechanisms 

Transmisssion electron microscopy 

Titanium alloys and intermetallics 

Shapiro, Alexander J. 

E-mail:	 alexander.shapiro@nist.gov 

MOIF method microscopy 

Mössbauer effect 

Scanning electron microscopy (SEM) and 

X-ray microanalysis 

Image analysis 

Shepherd, Dominique, A. 

E-mail:	 dominique.shepherd@nist.gov 

Titanium alloys 

Mechanical testing 

Mechanical properties 

SEM, TEM 

Shull, Robert D. 

E-mail:	 robert shull@nist.gov 

Nanocomposites 

Magnetic susceptibility 

Mössbauer effect 

X-ray and neutron diffraction 

Magneto-caloric and magneto-optical effects 

Magnetic domain imaging 

Siu, I-Liang 

E-mail:	 iliang.siu@nist.gov 

Thin film processing 

Giant magnetoresistance 

Magnetization dynamics 

Slutsker, Julia 

E-mail:	 julia.slutsker@nist.gov 

Smart composites 

Shape memory alloy 

Massive transformations 

Superelastic material 

Stafford, Gery R. 

E-mail:	 gery.stafford@nist.gov 

Electrochemical transients 

Electrodeposition 

Molten salt electrochemistry 

Stoudt, Mark R. 

E-mail:	 mark.stoudt@nist.gov 

Metal fatigue 

Thin films 

Mechanical properties 

Environmentally assisted cracking 

Twisselmann, Douglas J. 

E-mail:	 douglas.twisselmann@nist.gov 

Ferromagnetic resonance 

Magnetometry 

Warren, James A. 

E-mail:	 james.warren@nist.gov 

Computer simulations of solidification 

Dendrite pattern formation 

Modeling of solder/substrate wetting processes 

Modeling grain boundaries 

Williams, Maureen E. 

E-mail:	 maureen.williams@nist.gov 

Differential thermal analysis 

Powder x-ray diffraction 

Solder wettability 

SEM 

66 
Organizational Charts


Organizational Charts


Materials Science and Engineering Laboratory


Polymers 

E.J. Amis, Chief 

C.R. Snyder, Deputy 

Metallurgy 

C.A. Handwerker, Chief 

F.W. Gayle, Deputy 

Ceramics 

G.G. Long, Chief (Acting) 

(Vacant), Deputy 

Materials Reliability 

F.R. Fickett, Chief 

T.A. Siewert, Deputy 

NIST Center for 

Neutron Research 

J.M. Rowe, Director 

L.E. Smith, Director 

S.W. Freiman, Deputy Director 

National Institute of Standards and Technology


Director 

Deputy Director Director 

Boulder Laboratories 

Baldrige National Quality 

Program 

Director for 

Administration 

& Chief Financial 

Officer 

Technology 

Services 

Advanced 

Technology 

Program 

Manufacturing 

Extension 

Partnership 

Manufacturing 

Engineering 

Laboratory 

Chemical Science 

and Technology 

Laboratory 

Materials Science 

and Engineering 

Laboratory 

Electronics and 

Electrical Engineering 

Laboratory 

Information 

Technology 

Laboratory 

Physics 

Laboratory 

Building and 

Fire Research 

Laboratory 

67