NI8T

NIST Special Publication 1043

Workshop oh Reliability Issues in

Nanomaterials

17-19 August 2004

Robert R. Keller

David T. Read

Roop Mahajan
he National Institute of Standards and Technology' was established in 1 988 by Congress to "assist industrv' in the de\ elopment of technology ... needed to improve product quality, to modernize manufacturing processes, to ensure product reliability ... and to facilitate rapid coimuercialization ... of products based on new scientific discoveries." NIST. originally founded as the National Bureau of Standards in 1901. works to strengthen U.S. industry 's competitiveness; advance science and engineering; and improv e public health, safety , and the environment. One of the agency's basic functions is to develop, maintain, and retain custody of the national standards of measurement, and provide the means and methods for comparing standards used in science, engineering, manufacturing, commerce, industry, and education

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'At Boulder. CO 80305 Some elements at Boulder, CO
NIST Special Publication 1043

Robert R. Keller

David T. Read

Materials Reliability Division

Materials Science and Engineering Laboratory

Roop Mahajan

Department ofMechanical Engineering

University of Colorado

Technology Administration

Robert C. Cresanti, Under Secretaiyfor Technology

National Institute of Standards and Technology

William A. Jeffrey, Director

ibility Issues in

Nanomaterials

January 2007

U.S. Department of Commerce

Carlos M. Gutierrez, Secretaiy
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.

National Institute of Standards and Technology Special Publication 1043

Natl. Inst. Stand. Technol. Spec. Publ. 1043, 31 pages (January 2007)

CODEN: NSPUE2

U.S. GOVERNMENT PRINTING OFFICE

WASHINGTON: 2007

For sale by the Superintendent of Documents, U.S. Government Printing Office

Internet: bookstore.gpo.gov — Phone: (202) 512-1800 — Fax: (202) 512-2250

Mail: Stop SSOP, Washington, DC 20402-0001
CONTENTS

EXECUTIVE SUMMARY v

1. INTRODUCTION 1

2. SCOPE 2

3. DEVELOPMENT OF NEEDS STATEMENTS 3

4. OUTLINE OF WORKSHOP REPORT 4

5. ASSESSMENT OF CURRENT KNOWLEDGE IN NANOMATERIALS FABRICATION

AND CHARACTERIZATION 4

5.1 Reliability Issues Pertinent to Nanomaterials 4

5.2 State of the Art in Measurement Technology for Reliability Studies of Nanomaterials 6

6. DETAILED SUMMARY OF NANOMATERIALS ISSUES 8

6.1 Nanomechanical challenges and needs in manufacturing and materials processing,

nanomaterial products, advanced interconnects, and active devices 8

6.1.1 Technological Challenges 8 6.2.2 Materials Challenges 8 6.1.3 Measurement Needs 9

6.1.4 More General Needs 10

6.2 Nanomechanical challenges and needs in characterization and testing 10

6.2.1 Technological Challenges 10

6.2.2 Materials Challenges 10

6.2.3 Measurement Needs 1

6.2.4 More General Needs 12

7. BRIEF SUMMARY OF ACTION ITEMS FOR METROLOGY DEVELOPMENT 12

8. GLOSSARY 13

ACKNOWLEDGMENTS 14

APPENDICES 15

Appendix A: Attendees 15 Appendix B: Plenary and Breakout Presentations 16 Appendix C: Workshop Program 17 Appendix D: Breakout Presentation Titles 22

Appendix E: Questions Posed to Plenary Session Speakers 24

Appendix F: Questions Posed to Breakout Session Speakers 25

Appendix G: NIST Lab Tours 25

iii
Workshop Organizers

Robert R. Keller

David T. Read

Materials Reliability Division, Materials Science and

Engineering Laboratory

National Institute of Standards and Technology

Roop Mahajan

Mechanical Engineering Department

University of Colorado

Venue

National Institute of Standards and Technology

Building 2, Room 0113

U. S. Department of Commerce Laboratories

325 Broadway

Boulder, Colorado 80305

IV
EXECUTIVE SUMMARY

The Workshop on Reliability Issues in Nanomaterials was held at the Boulder Laboratories of

the U. S. Department of Commerce on August 17-19, 2004. It was organized by the National

Institute of Standards and Technology (NIST) and was designed to promote a particular subset

of NIST's responsibilities under the National Nanbtechnology Initiative (NNI). Larger issues,

such as the definition, prospective uses, and impact of nanomaterials have been addressed

elsewhere and were not considered in this workshop. The goal was to achieve consensus on two

related topics: the identification of specific measurement-related barriers to successful

incorporation of reliable nanomaterials into widespread engineering practice in the next 5 to 10

years; and the identification of measurement methodologies, standards, data, and models that

might be appropriate for overcoming these barriers. 34 participants, representing cutting-edge

nanomechardcs-related research and development in industry, academia, and national

laboratories, attended and contributed. Adding NIST-Boulder staff who attended brings the

total to about 40. The workshop format promoted discussion on the intended topics, and

included

1. a pre-workshop questionnaire to be addressed by plenary and breakout speakers;

2. invitation of 10 plenary speakers who gave hour-long presentations and 23 breakout

speakers, who gave brief presentations addressing the points raised in the questionnaire.

Key Conclusions: Industrial, academic, and national laboratory consensus indicated that there

is always a need to understand fundamental causes of failure. Such understanding should then

lead to redesign that is more reliable and to improved manufacturing. The goal of accurate

performance and lifetime prediction for nanomaterials depends on the interplay between

accurate materials testing and characterization, and reliability models incorporating valid

measured data. Attendees agreed that while the synergy among industry, academia, and

national laboratories was effective, more fundamental materials research is needed, where the

actual division of labor would be determined by market forces and policy.

It was suggested that NIST could serve the unique role of developing metrology, standards, and

materials characterization methods for improving reliability of nanomaterials. The most

challenging and general metrology recommendation was the development of an "atom

imager," a hypothetical instrument capable of nondestructively measuring the chemical identity

and precise three-dimensional position of every atom within a nanomaterial. Such an

instrument was postulated to be the key tool for optimizing fabrication/manufacturing and

controlling reliability of nanomaterials. Nearer-term recommendations centered on improving

the metrological performance of scanned probe microscopy (SPM) and nanoindentation. A

secondary theme in many presentations was the need for modeling to be formally coupled with

physical measurement in any study of nanomaterials; however, no novel computational tool or dataset was identified as a need of high priority.

V
Acknowledgments: We are grateful for financial support from The National Science

Foundation Solid Mechanics and Materials Engineering Program, the NIST Office of

Microelectronics Programs, and the NIST Materials Reliability Division.

Robert R. Keller

David T. Read

Roop Mahajan

February 2005

VI
Workshop on Reliability Issues in Nanomaterials

Robert R. Keller and David T. Read

Materials Reliability Division

Materials Science and Engineering Laboratory

National Institute of Standards and Technology

Boulder, CO 80305

Roop Mahajan

Department of Mechanical Engineering

University of Colorado

Boulder, CO 80305

The Workshop on Reliability Issues in Nanomaterials was held at the Boulder

Laboratories of the U. S. Department of Commerce on August 17-19, 2004. It was

organized by the National Institute of Standards and Technology (NIST) and was

designed to promote a particular subset of NIST's responsibilities under the

National Nanotechnology Initiative (NNI). Attendees agreed that while the synergy

among industry, academia, and national laboratories was effective, more

fundamental materials research is needed, where the actual division of labor would

be determined by market forces and policy. It was suggested that NIST could serve

the unique role of developing metrology, standards, and materials characterization

methods for improving reliability of nanomaterials. The most challenging and

general metrology recommendation was the development of an "atom imager," a hypothetical instrument capable of nondestructively measuring the chemical identity

and precise three-dimensional position of every atom within a nanomaterial. Such

an instrument was postulated to be the key tool for optimizing

fabrication/manufacturing and controlling reliability of nanomaterials. Nearer-term

recommendations centered on improving the metrological performance of scanned

probe microscopy (SPM) and nanoindentation.

Keywords: design; experiment; fabrication; failure; lifetime prediction; material

characterization; metrology; modeling; processing

1. INTRODUCTION

Nanomaterials lie at the heart of the field of nanotechnology. The NNI projects this field to have

tremendous global impact, estimated to become a $1 trillion industry over the next 15 to 20

years, with one third of that focused on materials and materials processing. At present, with an

estimated $1 billion annual investment, U.S. government spending has doubled in the last 4

1
years and constitutes nearly one third of the world governments' annual investment of over $3

billion. Through the NNI, approximately 22 % of that U.S. investment addresses nanostructured

materials by design, and another 39 % addresses nano-electronics, -photonics, and -magnetics;

the rest cover other NNI grand challenges such as health care, environment, energy,

instrumentation and metrology, and manufacturing.

The introduction of nanomaterials into current and future technologies opens up an entirely

new suite of both materials science and measurement science challenges. Effects of dimensional

scaling play a stronger role in the reliability of nanomaterials than in any other materials known

to date. Surfaces and interfaces can easily dominate and change behaviors and properties

known to develop in bulk materials of the same chemical composition. As a result, one cannot

simply extrapolate what is known about bulk material behavior to the nanoscale and expect to predict structure or properties accurately.

The full realization of reliable devices at this scale is limited by a host of materials science and

engineering barriers centered on nanomechanics. For example, the development of accurate and

repeatable metrologies for determining mechanical properties of materials is key to understanding how issvies such as plasticity, fracture, adhesion, friction, stress/strain response,

micro- and nanostructure, and chemistry determine the mechanical response of materials at the

nanoscale. Further, nanomechanical response plays an important, yet sometimes indirect, role

in other types of reliability, such as thermal or electrical reliability. Valid measurements can

provide a foimdation for building predictive models of nanostructure and behavior that will be

based on materials science, as opposed to being purely empirical in nature.

It was the intent of this workshop to identify and discuss specific measurement-related barriers

to successful incorporation of reliable nanomaterials into widespread engineering practice in

the next 5 to 10 years, as determined by leading researchers in nanomechanics and reliability.

The workshop also intended to identify measurement methodologies, standards, data, and

models that might be appropriate for overcoming these barriers.

This report is also available online at http://www.boulder.nist.gov/div853/RIN .

2. SCOPE

These topics of discussion described the workshop for invitees considering attendance:

Nanomaterials processing and fabrication and their effects on mechanical reliability

" Methods and techniques for characterizing structure of nanomaterials

Methodologies for measuring mechanical properties in nanomaterials

Experimental and modeling approaches to understanding effects of structure and

dimensional scaling on mechanical behavior of nanomaterials, with emphasis on surface

and interface issues

Approaches to understanding what roles nanomechanics plays in other types of reliability

Structure, property, and lifetime prediction

2
Invitations to potential attendees informed them that we were seeking not only a description of

the present state of the art in nanomechanical reliability, but also a glimpse into the future of the

possible paths into which nanotechnology-based research could lead us in materials science and

engineering, and vice versa.

This workshop addressed some of the Grand Challenges identified during the Nanomechanics

Breakout Track of the NNI Interagency Workshop on Instrumentation and Metrology, held

January 2004 at NIST-Gaithersburg. Namely, we addressed many of the following issues:

Modeling of nanomechanical experiments;

Integration of multiple techniques for measurement and characterization

Experimentation/testing under real application conditions

Standardization and calibration

Instrument development for nanomechanics

High-throughput, automated nanomechanics measurements

3. DEVELOPMENT OF NEEDS STATEMENTS

The last two hours of the workshop were used to review a two-part summary, written by the

NIST organizers, of the measurement needs expressed by the attendees. One part was intended

to be a complete list of specific needs expressed by all speakers, grouped according to possible

metrological solutions. The other part was a shorter list of the consensus summary of the needs

identified at the workshop. It became clear during the course of the workshop that materials

researchers who are concerned with understanding and improving nanomechanical reliability

commonly use several main tools:

• Nanoindentation

• Micro- and nanotensile and compression testing

• Scanned probe microscopy

• Modeling

A number of other important tools were discussed, for example, reflectivity measurement, for reflective coatings on mirrors intended for switching light signals to and from optical fibers, and

scanned x-ray diffraction, for analysis of grain structure in copper on large silicon wafers; but

the degree of convergence on nanoindentation, scanned probe microscopy, and modeling was

neither intended nor anticipated in the planning of the workshop. As a result, most of the

detailed and consensus need statements center around these measurement instruments.

The idea of the measurement issues important to researchers from different industries being

addressed by a smaller suite of measurement tools was crystallized by one of the attendees in a breakout presentation. She said: "We care about different technologies and reliability concerns, but are addressing the same problems."

3
4. OUTLINE OF WORKSHOP REPORT

We present an assessment of current nanomaterials fabrication and characterization knowledge

in the context of reliabiHty, based on questionnaires and discussion during the plenary sessions,

and follow with a detailed summary of the issues of concern for making reliable nanomaterials,

as articulated by all workshop attendees. Plenary speakers reviewed this report prior to its distribution.

Two alternative definitions of the reliability of nanomaterials are considered, as used in the

context of this workshop:

1. the extent to which nanomaterials exhibit consistent mechanical behavior and associated

properties over a long period, such as during a device lifetime;

2. the extent to which nanomaterial behavior and properties can be predicted over a given

period.

The first definition is similar to the conventional use of the term "reliability." However, the

second definition must sometimes be used in the design of devices and products, in the event

that a material changes or degrades with increasing exposure to design stresses and

environments. If the material degrades over time, but the degradation can be well predicted, the

material may still be useful. In general, a "reliable" nanomaterial is one that can serve its purpose over the course of an intended device or designed product lifetime.

5. ASSESSMENT OF CURRENT KNOWLEDGE IN NANOMATERIALS

FABRICATION AND CHARACTERIZATION

5.1 Reliability Issues Pertinent to Nanomaterials

Successful incorporation of nanomaterials into widespread engineering use requires us to understand why, how, and when failure will occur. Basic research addressing the combination

of identification and measurement of failure mechanisms in these novel materials will provide

the framework necessary to develop reliability models that are able to accurately predict

changes in behavior and properties, and therefore lifetime, a key factor in successful

manufacturing.

A number of factors that compromise reliability were identified during the workshop. The

detailed lists as articulated by attendees follow in the next section, and are summarized here.

We have sorted the reliability problems into three categories:

Structures, behaviors, and resulting properties o Nanomaterials have much larger surface-to-volume ratios than bulk materials. This

affects friction and wear properties as well as stiction in nanomaterials.

o Polycrystalline nanomaterials contain a higher fraction of grain boundary volume, and

may be more susceptible to failure mechanisms involving such boundaries, including

4
high-temperature deformation modes becoming operative at lower temperatures or

failure mechanisms involving diffusion.

o Nanomaterials are almost always used as part of a materials system, and invariably come

into contact with other materials, creating interfaces. Failure mechanisms involving

delamination or chemical interdiffusion across an interface can be exacerbated. Diffusion

through interfaces can also contribute to failures.

o Defect stability differs from that observed in bulk materials due to stronger influences of

surfaces. Strain hardening may not follow the stages seen in bulk materials since

dislocations can easily escape. Internal stresses associated with defects can build up,

occupying the entire volume of a nanomaterial faster than might be expected from

observations of bulk materials. Dislocations may not be energetically favored to exist in

extremely small structures, forcing other mechanisms of plasticity or fracture to operate.

o Grain size is usually smaller in polycrystalline nanomaterials than in bulk materials,

causing defect behavior and properties such as strength to differ from those seen in bulk

materials.

o Localized behavior is much more important in nanomaterials. For example, an unusual

orientation of a single grain can compromise the reliability of an electronic interconnect.

Operation under extreme conditions

o Accelerated tests must be developed in manners that suitably reproduce expected

operating conditions, but sometimes the expected conditions can lead to behaviors not

yet well understood in nanomaterials.

o Area- or volume-normalized external loads can be much more intense than in the case of

bulk materials. Nanomaterials are often expected to withstand current densities, electric

fields, pressures, stresses, or optical power densities that far exceed the values typically

applied to bulk materials. Behaviors under such conditions are largely unknown.

o Time dependence of failure is very different from that observed in bulk materials, due to vastly different boundary conditions and length scales.

o Thermal management in nanomaterials is difficult, due to the high density of interfaces

in multi-material systems. This is exacerbated by very high temperatures often

undergone during thin- film or high-pressure processing.

Size, shape, and distribution control

o Ordered arrays or patterns of some nanostructures cannot presently be sufficiently

fabricated. Quantum dots or carbon nanotubes must be made uniformly over large areas

in order for many potential devices to be realized. Arrays and patterns must contain

well controlled size and structure distributions. Lithographic approaches may not be

5
feasible beyond certain dimensional limits, suggesting the need for self-assembly or other patterning processes.

o Stresses and strains can become very large in nanomaterials, and their management

becomes extremely difficult. Although lattice-mismatched quantum dots (QDs) require

high elastic strains (~7 % for InAs/GaAs) in order to exhibit their unique electronic

behaviors, plastic relaxation must be avoided.

5.2 State of the Art in Measurement Technology for Reliability Studies of

Nanomaterials

Reliability studies of nanomaterials depend on valid measurement of the properties and

behaviors of interest. Thorough understanding of mechanical properties and behavior of

nanomaterials requires accurate knowledge of the external forces and displacements applied to such materials, as well as the corresponding response of those materials.

Many test and characterization (i.e., measurement) methods were discussed during the

workshop. Some are now in use, while others are still under development. In general, high

performance tools for measuring bulk materials are commonly used for nanomaterials

characterization, with appropriate modifications. For example, high resolution imaging

methods such as atomic force microscopy (AFM), scanning tunneling microscopy (STM),

transmission electron microscopy (TEM), and scanning electron microscopy (SEM) are routinely

pushed to their limits. X-ray diffraction (XRD) is also used extensively for structural

characterization of both aggregates and individual nanostructures. Focused ion beam (FIB)

microscopy and manipulation has become a necessity for direct imaging, preparing specimens

for other types of imaging, and patterning. Advances in mechanical testing and characterization

have led to unprecedented resolutions in measurement and control of force and displacement.

We summarize these state of the art methods here, categorized by application. A detailed listing

of testing and characterization needs exceeding the present state of the art, as articulated by

attendees, follows in the next section.

MEMS/NEMS

o Nondestructive and/or noninvasive measures for mechanical displacement, both static and dynamic, using electrical or optical methods

o Automated systems for testing at high throughput

o Surface analysis and analytical tools for identifying impurities or contaminants, e.g.. Auger electron spectroscopy. X-ray photoelectron spectroscopy, secondary ion mass

spectroscopy (SIMS)

o Environmental chambers for accelerated testing

o Shock and vibration testing at the product level

o Thermal shock and cycling tests for delamination and crack growth

6
Nanoscale Manufacturing and Assembly

o STM methods for moving and removing atoms, to enable bottom-up fabrication

o Patterned atomic layer deposition (ALD) using STM for patterning (idea near

realization)

o Surface acoustic wave (SAW) devices, accelerometers for mechanical properties

o Indirect optical methods using lasers, deflection techniques for displacement

measurement

o Assembled micro-SEM columns to enable novel nanoscale characterization on a chip

o Assembled linear actuators to enable nanoscale testing on a chip

Advanced Electronic Interconnect

o Scanning XRD (four-circle goniometer) with area detector for simultaneous

measurement and mapping of crystallographic phases, texture, and film thickness on

200 mm wafers; includes 20 |im coUimation. Development is underway to make this system apply to films of thickness <10 nm, where electrical methods are invalid. Such a system can be used in-line during manufacturing.

Semiconductor Nanastructures

o Cleaving in situ within STM imder ultra-high vacuum for cross-sectional imaging with

atomic resolution

o Spectroscopy within STM for bandgap measurement as a function of position across a wafer

o Wafer curvature for average stress determination

o AFM-based patterned nanostructure fabrication using a nano-jet probe

o FIB nanopatteming for nanostructure position templates

Mechanical testing

o Young's modulus (E) and hardness (H) by continuous stiffness nanoindentation system

and hybrid tribology/nanoindentation system; measurements still not in good

agreement, with standard deviations as high as -75 to 125 GPa for E, -12 to 14 GPa for H

for the case of thermal plasma chemical vapor-deposited (CVD) silicon carbide;

o Calibration of tip shape by use of fused quartz (not optimal)

o Nanoindentation measurements for H from sub-500 nm grains

7
o

o

o

Modified nanoindentation measurements of sub-40 nm Si nanoparticles

Stressed overlayer and edge lift-off tests for adhesion;

Nanoscale scratch tests for adhesion

o Acoustic AFM for mapping of elastic properties

6. DETAILED SUMMARY OF NANOMATERIALS ISSUES

The organization of this summary follows the session titles as listed in the program. These lists were reviewed in detail at the final session of the workshop, and are sorted by topical area as presented in the workshop. There is no significance to the order in which the issues are listed.

6.1 Nanomechanical challenges and needs in manufacturing and materials

processing, nanomaterial products, advanced interconnects, and active devices

6.1.1 Technological Challenges

• Each device has its own unique reliability issues

• High yield and uniformity are required

• Reliability required over 20 year lifetimes

• Acceleration factor <10 desired in order to retain relevant physical mechanisms of

reliability degradation; accelerating stresses include: temperature, voltage, current,

humidity, strain, vibration, laser power

• Automated assembly manufacturing unavailable for parts of size <0.5 mm; all such

assembly now done by humans

6.1.2 Materials Challenges

• MEMS and NEMS:

- Stiction (key issue)

Possible solution: High-stiffness designs - Friction and wear (sliding and impact)

• Possible solution: Noncontacting parts - Hinge memory

- Fatigue and creep

Possible solution: Conservative design stress - Stress: need to absorb, balance, control - Structure uniformity, defects in coatings for MEMS

- Mechanical integrity of polysilicon vs. metals

• Carbon Nanotubes (CNTs): - Need dimensional uniformity, fewer defects - Separate by electronic structure - Can't make continuous fibers - Need much better process control and qualification

• CNTs and Nanoparticles:

8
- Separation, purification methods

• Nanocomposites: - Need better understanding, using both simulation and experiments, especially

CNT/matrix interface

• QDs:- Need uniform size distribution and spacing

Possible solution: Nanopatferning by FIB - Control plasticity

• General issues: - Make small things with more control over defects and uniformity of size - Structure/property relationships for monolayers (adhesion, friction, wear) - Effects of surface roughness - Develop process variables = f (residual stress, stress gradients, yield strength

(YS), ultimate strength (UTS)) - Need to know where all the atoms are located - Bulk property data on more materials, as foundation for nanomaterials:

Elastic, dielectric, density of states - Gradient characterization (chemical, physical), in complex matrices

6.1.3 Measiirement Needs

• Tools and/or techniques to measure nanometer motion, addressing six degrees-offreedom, faster than device resonance frequencies - Possible solution: optical surface profilometer, Doppler laser interferometer,

strobing methods

• Tools for atomically precise engineering - Possible solution: Patterned ALD, using STM

• Conversion of inherently two-dimensional measurement methods to three-dimensional

methods

• Metrology for micro- and nanostructure of low-level features, especially early in the

process

• Tools capable of multiple, coupled measurements with a single technique - Thickness, crystalline phase, texture - These must be done quickly - Possible solution: scanning XRD

• Tools or systems capable of coupled measurements of properties and behaviors, using

multiple techniques: - In- situ, coupled measurements

- Optical coupled to mechanical methods

- Electrical coupled to mechanical methods

• High resolution (in space and energy), fast methods for imaging, morphology, chemistry - Possible solution: improvements to SEM, AFM, TEM

• Methods for local measurement of:

9
- Strain - Electrical properties - Structure size and/or shape - Temperature, including spatially resolved, non-contact

Possible solution: micro-Raman

• Inline-capable techniques for measurements during CMP:

- Particle size, morphology, dispersion, aggregation, correlation to performance

• High-throughput adhesion measurement

• New tests and/or models for new material combinations

• Nondestructive measurement of defects

• Deconvolution of sample-probe interaction in nanoindentation and scanned probe

microscopy (SPM)

• Standards for: - Reflectivity - film thickness and texture

6.1.4 More General Needs

• Development of relationships between in situ tests and real failures

• More modeling coupled to experimental measurements

• Large-area temperature control during fabrication to promote structure uniformity

• More collaborations to stimulate development of relevant measurement needs: - Manufacturing development and materials characterization/metrology

development

• High-temperature interfacial reliability studies: - Segregation, voiding

6.2 Nanomechanical challenges and needs in characterization and testing

6.2.1 Technological Challenges

• Small length scales: - Difficult measurement problems even with state of the art instruments

• Need more than incremental advances in capabilities for mechanical behavior, beyond

modification of existing tests, i.e., revolutionary, not just evolutionary

6.2.2 Materials Challenges

• In general (from a session announced for the Fall 2004 Materials Research Society

Meeting), the dominant nanomaterial research problems at present include: - Size effects, temperature or viscoelasticity, multiscale modeling,

adhesion/surface energy

• Need good, repeatable test samples: - No dislocations, surface defects

10
• Rapid, fully automated fabrication methods suitable for production- and researchquality specimens

• Identification of specific problems and experimental approaches applicable to nanoscale

biological materials

6.2.3 Measurement Needs

• Scaling of mechanical test methods to sub micrometer samples: - Uniaxial, multiaxial, torsional stressing - Fracture toughness - Deformation mapping

- Gripping, manipulation

• Localized strain measurement

• Measurement of stress gradients, especially over small dimensions

• Valid methods for separating stress and temperature effects on stress-strain behavior

• Sub micrometer temperature measurement (direct)

• Improvements in spatially resolved characterization: - SEM, SIMS, in-situ TEM, microdiffraction, micro-Raman, FIB (SE imaging) - Single-atom resolution probes such as field ion microscopes

• "Desperately needed": - High-resolution, in situ deformation studies in electron microscopes

• Nanoindentation: - Instrument consistency for E, H

- Control of nanoindenter tip geometry - Microforce standards - Calibration standards for nano-test equipment - Direct imaging of contact areas - Improvements in position (x, y, z) control and measurement

• AFM:

- Ability to do simultaneous mechanical testing and imaging - Ability to do simultaneous nanodeposition and imaging

Possible solution: dual-head AFM

- Tip/sample interaction energies need to be understood:

Contact area effects Direct imaging of contact areas - Need better characterization of: AFM tips - Need sharp, durable, reproducible tips - Need AFM and model velocities to match

- "Accurate and proven AFM technology!" - Better control of SPM tip motion, i.e., no unintentional lateral motion

- Calibration standards for nano-test equipment - Improvements in position (x, y, z) control and measurement

11
- The "perfect" AFM:

• Accurate knowledge of F and d for AFM

F sensor perpendicular to surface

Sharp, durable tip

• F sensor with stiffness control for both mechanical properties and

topography

• Easy switch between F and d control

Wide range of operational frequencies, temperature

High-bandwidth, low-noise pre-amp - Standards for: Microforce, both axial and lateral AFM spring constant

AFM tip-specimen contact area

Test/calibration specimens for nanoindentation and AFM-based

mechanical testing

• Measurement of toughness and strength of thin films - Standard bulk property data, for which accepted measurement methods exist,

should be available for all relevant compositions and processes. (Needed as a basis for understanding properties of nanomaterials):

• Thin film and nanomaterial data should be disseminated as they become

available

6.2.4 More General Needs

• MUST combine experiment and modeling for mechanical testing and

adhesion/interfacial fracture.

7. BRIEF SUMMARY OF ACTION ITEMS FOR METROEOGY DEVELOPMENT

The lists of needs given above seem formidable at first glance. However, it became clear during

the course of the workshop that there are several main tools commonly used by materials

researchers who are concerned with understanding and improving nanomechanical reliability:

Nanoindentation

Micro- and nanotensile and compression testing

Scanned probe microscopy

Modeling

This short list of tools in no way diminishes the significance of others discussed during the

workshop, e.g., electron microscopy and X-ray diffraction; it simply reflects a larger consensus

about commonly used methods for nanomaterials. Attempts have been made to adapt these

tools to most of the measurements listed, but considerable additional research and development

are needed in order to meet the needs sufficiently. These "common-denominator" tools lead to the following action items for metrology development for nanomaterials reliability:

12
Near term: Improved metrological performance of scanned probe microscopy and

nanoindentation, for more quantitative measurements of position, displacement, force,

temperature, and other relevant quantities;

Longer term: The "atom imager," a hypothetical instrument capable of measuring

nondestructively the chemical identity and precise three-dimensional position of every atom in a nanomaterial. Nevv^er generation field ion microscopes capable of imaging with single-atom

resolution are under development, but are still subject to limitations such as difficult-to-control

tip (which also serves as the specimen) structure and loss of atoms upon imaging (30 to 40 %

losses are not uncommon). Such instruments are also capable of sub-nanometer chemical

spectroscopy.

8. GLOSSARY

AFM Atomic force microscope, atomic force microscopy

ALD Atomic layer deposition

CMP Chemical mechanical polishing

CNT Carbon nanotube

CVD Chemical vapor deposition

d Displacement

E Young's modulus

F Force

FIB Focused ion beam

G Stiain energy release rate H Hardness

M Modulus

MD Molecular dynamics

MEMS Micro-electromechanical system

NEMS Nano-electromechanical system

NIST National Institute of Standards and Technology

QD Quantum dot

SAW Surface acoustic wave

SE Secondary electron

SEM Scanning electron microscope, scanning electron microscopy

SIMS Secondary ion mass spectroscopy

SPM Scanned probe microscopy

STM Scanning tunneling microscope, scanning tunneling microscopy

TEM Transmission electron microscope, transmission electron microscopy

UTS Ultimate tensile strength

XRD X-ray diffraction

YS Yield strength

13
ACKNOWLEDGMENTS

The purpose of this Workshop was to gather and summarize the opinions of the attendees

regarding the important and timely issue of measurement needs for Reliability Issues in

Nanomaterials. The organizers gratefully acknowledge the preparation; travel time; attentive,

constructive, and cooperative participation; and informed opinions contributed by the

attendees. Special thanks are expressed to the majority of the attendees who stayed for the

summary and review of the measurement needs at the end of the workshop, as well as to those

who reviewed this final report. The organizers are grateful for critical reviews of the final report, provided by the plenary speakers.

This workshop was supported financially by The National Science Foundation Mechanics and

Structure of Materials Program through Program Director Ken Chong, the NIST Office of

Microelectronics Programs through director Steven Knight, and the NIST Materials Reliability

Division. The bulk of the expenses were cost-sharing for the travel expenses of the attendees.

Wendy McBride, NIST Boulder Conference Program Manager, carried out the bulk of the

arrangements for this workshop. The workshop benefited substantially from the well-organized

meeting room, refreshments, and al fresco lunches that Wendy arranged.

14
APPENDICES

The appendices to this report are intended to provide a historical record of the workshop to the extent practical. Most speakers have provided their presentations, mostly exactly as given at the

workshop, some with confidential information removed. The discussions were not recorded.

Appendix A: Attendees

Amey, Susanne

Boyce, Brad

Burnham, Nancy

Chandross, Michael

Chong, Ken

Datta, Subhendu

de Boer, Maarten

Dunn, Marty

Gerberich, William

Goldman, Rachel

Greenberg, Alan

HoU, Susan

Hsu, Stephen

Hurley, Donna

Johnson, Harley

Keller, Robert

Kopycinska-Mueller, Malgorzata

Mahajan, Roop

Moody, Neville

Pang, Mengzhi

Qi, H. Jerry

Randall, John

Read, David

Reimanis, Ivar Rodbell, Ken

Roshko, Alexana

Sbaizero, Orfeo

Schwaiger, Ruth

Sitaraman, Suresh

Smith, Douglas

Sokolov, Igor

Tewary, Vinod

Uchic, Michael

Volinsky, Alex

Yang, Bo

Zhu, Yong

Lucent Technologies Bell Labs and NJNC

Sandia National Laboratories

Worcester Polytechnic Institute

Sandia National Laboratories

National Science Foundation

University of Colorado

Sandia National Laboratories

University of Colorado

University of Minnesota

University of Michigan

University of Colorado

Intel Corporation

NIST

NIST

University of Illinois at Urbana-Champaign

NIST

NIST

University of Colorado

Sandia National Laboratories

Cornell University

University of Colorado

Zyvex Corporation

NIST

Colorado School of Mines

IBM Corporation

NIST

University of Trieste (Italy)

Forschungszentrum Karlsruhe -IMF2

Georgia Institute of Technology

NIST

Clarkson University

NIST

Air Force Research Laboratories

University of South Florida

Florida Institute of Technology

Northwestern University

15
Appendix B: Plenary and Breakout Presentations

Presentations from a majority of the speakers, both plenary and breakout, are included on the

attached CD. For a listing of titles, please refer to appendices C and D.

16
Appendix C: Workshop Program

Program, Day 1

Tuesday, August 17, 2004

8:00 a.m. Registration (coffee available)

8:30 a.m. Leslie Smith, Director, Materials Science and Engineering Laboratory, NIST - Welcome

Topical Area: Fabrication

Fabrication I: Nanomechanical Issues in Manufacturing

Session Chair: David Read, NIST

8:45 a.m. Susanne Amey, Lucent Technologies - Materials Requirements and

Measurements in Design and Manufacture of Micro- and NanoElectromechanical Systems for Performance and Reliability

9:45 a.m. Break - coffee

10:00 a.m. John Randall, Zyvex - Materials Requirements and Measurements in Nanoscale

Manufacturing and Assembly

11:00 a.m. Breakout 1:

Near-Term M/NEMS and Other Nanomaterial Products: Tools, Reliability, and

Metrology

Chair: Dudley Finch, NIST/University of Colorado

12:30 p.m. Lunch (box lunch supplied)

1:30- 2:00 p.m. Lab tours - Select ONE Tour

Tour 1. World Trade Center Investigation

Tour 2. Nanoscale Elastic-Property Imaging

Tour 3. Thin Film Mechanical Testing

Tour 4. MEMS for Testing of Biological Systems

17
Fabrication II: Nanomechanical Issues in Materials Processing

Session Chair: Robert Keller, NIST

2:00 p.m. Ken Rodbell, IBM - Materials Requirements and Measurements in Design and

Manufacture of Advanced Electronic Interconnect for Performance and

Reliability

3:00 p.m. Break

3:15 p.m. Rachel Goldman, University of Michigan - Materials Requirements and

Measurements in Design and Fabrication of Semiconductor Nanostructures for

Performance and Reliability

4:15 p.m. Breakout 2:

Advanced Interconnects and Active Devices: Reliability and Metrology

Chair: Alexana Roshko, NIST

5:45 p.m. Adjourn for the day

18
Program, Day 2

Wednesday, August 18, 2004

8:15 a.m. Ken Chong, National Science Foundation - NSF perspective on metrology

development for nanomaterials

Topical area: Characterization and Testing

Characterization and Testing I: Mechanics of Nanomaterials

Session Chair: Roop Mahajan, University of Colorado

8:30 a.m. William Gerberich, University of Minnesota - Significance of Mechanical

Behavior in Small Volumes to Design of Reliable Nanomaterials and Nanoscale

Devices

9:30 a.m. Break

9.45 a.m. Martin Dunn, University of Colorado - Necessary Reinterpretations of

Continuum Mechanics Concepts for Applicability to Nanomaterials

10:45 a.m. Breakout 3:

Unusual Mechanical Properties of Nanomaterials

Chair: Martin Dunn, University of Colorado

12:15 p.m. Lunch (box lunch supplied)

1:15 - 1:45 p.m. Lab tours - Select ONE Tour

Tour 1. World Trade Center Investigation

Tour 2. Nanoscale Elastic-Property Imaging

Tour 3. Thin Film Mechanical Testing

Tour 4. MEMS for Testing of Biological Systems

19
Characterization and Testing II: Mechanical Probing Methods for Characterizing

Nanomaterials

Session Chair: Donna Hurley, NIST

1:45 p.m. Nancy Burnham, Worcester Polytechnic Institute - Role of Atomic Force

Microscopy in Conception, Design, and Characterization of High-Performance

and Reliable Nanomaterials

2:45 p.m. Break

3:00 p.m. Neville Moody, Sandia National Laboratories - Significance of Adhesion and

Interfacial Fracture in Design of Reliable Nanomaterials and Nanoscale Devices

4:00 p.m. Breakout 4:

Atomic Force Microscopy and Nanoindentation

Chair: Ken Gall, University of Colorado

5:30 p.m. Adjourn technical sessions for day 2

5:45 p.m. Board bus for travel to Flagstaff Summit

6:00 p.m. Picnic, Flagstaff Stone Shelter (casual clothing suggested)

20
Program, Day 3

Thursday, August 19, 2004

Topical area: Nanomaterials metrology roadmap

Session Chair: Stephen Hsu, NIST

8:30 a.m. Stephen Hsu, National Institute of Standards and Technology - The

Nanomechanics Measurement Facility in the NIST Advanced Measurement

Laboratory (AML)

8:45 a.m. Douglas Smith, National Institute of Standards and Technology - Nanomechanics at NIST

9:45 a.m. Break

10:00 a.m. Robert Keller, National Institute of Standards and Technology - Summary of

nanomaterials reliability issues and measurement needs

11:00 a.m. David Read, National Institute of Standards and Technology - Challenges,

barriers, and priorities for nanomaterials metrology

12:00 noon Adjournment of the technical sessions of the workshop

1:00 p.m. Lab tours at University of Colorado, by request

1:00-5:00 p.m.

Report writing by volunteers

21
Appendix D: Breakout Presentation Titles

Breakout 1: Near-Term M/NEMS and Other Nanomaterial Products: Tools, Reliability, and

Metrology

DeBoer, Maarten

Greenberg, Alan

Sbaizero, Orfeo

Volinskv, Alex

Chair: Dudley Finch

III situ Property Measurement in MEMS

Mechanical and Gas Transport Behavior of Dense Polymer Films

The Center for Excellence in Nanotechnology at the University of Trieste

Thin Film Mechanical Reliability: Environmental Effects

Breakout 2: Advanced Interconnects and Active Devices: Reliability and Metrology

Sitaraman, Suresh

Johnson, Harley

Yang, Bo

Holl, Susan

Pang, Mengzhi

Chair: Alexana Roshko

Off-Chip Interconnects: Design, Fabrication, and Reliability

Mechanical and Electronic Coupling in Nanotubes and Quantum Dots

Energy Release Rate of Quantum Islands in Stranski-Krastanow Growth

CMOS to beyond CMOS, Novel Material Characterization Challenges

Adhesion Measurements of Thin Film Structures
Breakout 3: Unusual Mechanical Properties of Nanomaterials

Chair: Martin Dunn

Uchic, Michael

Schwaiger, Ruth

Datta, Subhendu

Qi, H. Jerry

Reimanis, Ivar

Boyce, Brad

Mechanical Testing at the Micron-Size Scale

Investigations of Nanostructured Materials - from Nanocrystalline to Nanoporous

Measurement and Modeling of Thermomechanical Properties of Thin

Layers

Biomolecule Unfolding and Mechanics of Nacre

Toughness Measurement of Thin Films: What Does it Tell Us and How

Reliable is That?

Measurement Challenges in Microtensile and Microfatigue Reliability

Studies

Breakout 4: Atomic Force Microscopy and Nanoindentation

Chair: Ken Gall

Sokolov, Igor The Need in a Standard for Small Force to Probe Interactions in

Nanoscale with the AFM

Zhu, Yong Novel Experiments to Assess the Mechanical Properties of Thin Films and

Nano-Scale Structures

Chandross, Michael Simulations of Nanotribology

23
Appendix E: Questions Posed to Plenary Session Speakers

Broad questions for all Plenary speakers; treat in terms of your area of expertise:

What is considered state-of-the-art, in terms of experiment/processing/characterization

and/or theory/modeling? (This may include some of your own work.)

What are the problems now under investigation?

What barriers (scientific and/or technological) do you foresee to advances in the coming 5 to 10 years? Please include barriers that may be addressed by improvements in materials

measurements.

What are possible approaches to solution? Please include how you might envision "division

of labor," i.e., roles of industry, DOE labs, NIST, universities.

Questions for Fabrication speakers (Day 1, Arney, Randall, Rodbell, Goldman):

How is mechanics/mechanical behavior important in terms of performance and reliability

required at product level?

How do you design-in performance and reliability, using principles of micro- and

nanostructure control? Please comment on adequacy of existing lifetime or performance

prediction methods.

How does industry measure performance of both the end product and the constituent

materials?

What are the limitations/barriers of the present measures/metrology?

Questions for Characterization and Testing speakers (Day 2, Gerberich, Dunn, Burnham,

Moody):

Measurements of which properties do you foresee to be critical for advancing

implementation of nanomaterials in the coming decade?

How sufficient are the existing test methods for nanoscale property measurement? Can

advances be made incrementally, or are revolutionary changes needed?

Please comment on the role of modeling in your work. What answers do you seek? What

type of modeling do you perform or refer to? What kind of information about materials structure is needed to guide the development of

property characterization and testing methods?

24
Appendix F: Questions Posed to Breakout Session Speakers

1. How does metrology affect your present work in nanomaterials?

2. What questions relating to reliability of nanomaterials would you like to see addressed

in this workshop and report/roadmap?

3. What metrology issues are of the most significance to you for your work in the coming 5

to 10 years?

Appendix G: NIST Lab Tours

Tour 1. World Trade Center investigation - David McColskey

In August of 2002, NIST took responsibility for the investigation of the World Trade Center

disaster. The investigation objectives include determining why the buildings collapsed; the

procedures and practices used in the design, construction, operation, and maintenance of the

buildings; and areas in codes and practices that warrant revision. The eight interdependent

projects include Project 3, "Analysis of Structural Steel," led by the Materials Science and

Engineering Laboratory. The objective of the project is to "determine and analyze the

mechanical and metallurgical properties and quality of steel, weldments, and connections from

steel recovered from WTC 1, 2, and 7."The lab tour/presentation will take place in the

Mechanical Properties Lab, where many specimens of steels from structural components of the

WTC towers are stored and evaluated.

Tour 2. Nanoscale Elastic-Property Imaging - Donna Hurley

We are developing AFM-based metrology for rapid, nondestructive measurement of

mechanical properties with true nanoscale spatial resolution. Our hybrid acoustic/AFM

approach involves the vibrational resonance of an AFM cantilever when its tip is in contact with

a sample. We have demonstrated how this approach can be used to determine the local indentation modulus of an unknown material or thin film. The AFM's scanning capabilities

mean that we can also obtain in-situ images of relative elastic stiffness with nanoscale spatial

resolution. Current research is aimed at combining the quantitative, single-point methods with

qualitative imaging in order to obtain quantitative maps of nanomechanical properties.

Complementary information obtained with scanning electron microscopy provides insight into

structure-property relations and helps to interpret the nanoscale contact-mechanics behavior.

Tour 3. Thin Film Mechanical Testing - David Read

We perform microtensile testing on thin films of metals, polymers, and ceramics. A typical gage

section is 1 jam thick by 10 jam wide by 200 |am long. The specimen is patterned by

25
photolithography on bare silicon. The silicon is etched from beneath the specimen, to a depth of

at least 60 |am, using xenon difluoride. This etch frees the gage section and a grip section with a hole for the loading pin. Tests are done under an optical microscope or inside the SEM. Using a

three-axis micromanipulator, the loading pin is placed in the 50 |am diameter hole in the grip

section of the specimen. As the load is applied, the displacement of a calibrated spring is recorded. A calibration factor, obtained using a force pendulum, is used to convert the

measured displacements to force values. Our noise level is tens of micronewtons; failure loads

for our specimens range upward from around 1 mN. Digital images are recorded every few

seconds during the test; digital image correlation is used to obtain the engineering strain in the

gage section. The gage section of the specimen is imaged over about 800 pixels of the digital

images, and the displacements are obtained with a precision of 0.01 to 0.05 pixels, for a strain

noise level of about 60 microstrain. Data are presented in the form of engineering stress-strain curves. Visitors to the lab will be able to see the optical testing station, the micromanipulator,

the xenon difluoride etching system, and posters showing typical specimens and results.

Tour 4. MEMS for Testing of Biological Systems - Andrew Slifka

We are developing MEMS-based mechanical test platforms and tools that can be integrated

with currently used biological techniques for the evaluation and measurement of cellular

response {e.g., gene expression, cell morphology, area of adhesion, etc.). These types of studies

are needed because the development of vascular smooth muscle cells in cardiovascular tissue, for example, is dependent on variations in the stress-strain environment that result from the

expansion and contraction of the vessel wall. The importance of the environment becomes

apparent when one considers that engineered tissues have mechanical properties inferior to those of naturally grown tissues. This is possibly a bulk effect, but is clearly related to processes

at the cellular level. Without a quantitative understanding of the mechanics and functionality of

the building blocks (cells and fibers), the bulk properties of the tissues cannot be fully

understood and modeled.

26
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