Kazuhisa Miyoshi

Glenn Research Center, Cleveland, Ohio

Surface Analysis and Tools

NASA/TM—2002-211815

August 2002
The NASA STI Program Office . . . in Profile

Since its founding, NASA has been dedicated to

the advancement of aeronautics and space

science. The NASA Scientific and Technical

Information (STI) Program Office plays a key part

in helping NASA maintain this important role.

The NASA STI Program Office is operated by

Langley Research Center, the Lead Center for

NASA’s scientific and technical information. The

NASA STI Program Office provides access to the

NASA STI Database, the largest collection of

aeronautical and space science STI in the world.

The Program Office is also NASA’s institutional

mechanism for disseminating the results of its

research and development activities. These results

are published by NASA in the NASA STI Report

Series, which includes the following report types:

• TECHNICAL PUBLICATION. Reports of

completed research or a major significant

phase of research that present the results of

NASA programs and include extensive data

or theoretical analysis. Includes compilations

of significant scientific and technical data and

information deemed to be of continuing

reference value. NASA’s counterpart of peerreviewed formal professional papers but

has less stringent limitations on manuscript

length and extent of graphic presentations.

• TECHNICAL MEMORANDUM. Scientific

and technical findings that are preliminary or

of specialized interest, e.g., quick release

reports, working papers, and bibliographies

that contain minimal annotation. Does not

contain extensive analysis.

• CONTRACTOR REPORT. Scientific and

technical findings by NASA-sponsored

contractors and grantees.

• CONFERENCE PUBLICATION. Collected

papers from scientific and technical

conferences, symposia, seminars, or other

meetings sponsored or cosponsored by

NASA.

• SPECIAL PUBLICATION. Scientific,

technical, or historical information from

NASA programs, projects, and missions,

often concerned with subjects having

substantial public interest.

• TECHNICAL TRANSLATION. Englishlanguage translations of foreign scientific

and technical material pertinent to NASA’s

mission.

Specialized services that complement the STI

Program Office’s diverse offerings include

creating custom thesauri, building customized

data bases, organizing and publishing research

results . . . even providing videos.

For more information about the NASA STI

Program Office, see the following:

• Access the NASA STI Program Home Page

at http://www.sti.nasa.gov

• E-mail your question via the Internet to

help@sti.nasa.gov

• Fax your question to the NASA Access

Help Desk at 301–621–0134

• Telephone the NASA Access Help Desk at

301–621–0390

• Write to:

 NASA Access Help Desk

 NASA Center for AeroSpace Information

 7121 Standard Drive

 Hanover, MD 21076
Kazuhisa Miyoshi

Glenn Research Center, Cleveland, Ohio

Surface Analysis and Tools

NASA/TM—2002-211815

August 2002

National Aeronautics and

Space Administration

Glenn Research Center
Available from

NASA Center for Aerospace Information

7121 Standard Drive

Hanover, MD 21076

National Technical Information Service

5285 Port Royal Road

Springfield, VA 22100

Available electronically at http://gltrs.grc.nasa.gov
NASA/TM—2002-211815 1

Surface Analysis and Tools

Kazuhisa Miyoshi

National Aeronautics and Space Administration

Glenn Research Center

Cleveland, Ohio 44135

Introduction

Many material properties are actually surface properties. For example, erosion, abrasion, wear,

oxidation, corrosion, adhesion, bonding, friction, fatigue, and cracking are all affected by surface properties [1–3]. By modifying surfaces, depositing thin films, or producing multiple-layered coatings, the

designer can enhance performance, such as resistance to erosion, abrasion, wear, oxidation, corrosion,

and cracking, as well as biocompatibility or environmental compatibility [4–7].

In order to understand surface properties, and ultimately to provide better surfaces, it is necessary

to study the physical and chemical characteristics of the material surface obtained by a given process.

A number of tools are now available for surface analysis of any solid surface [8–10]. Because the surface

plays such a crucial role in many processes, surface analysis and its tools have established their importance in a number of scientific, industrial, and commercial fields [11–21]. For example, the editors of

Research & Development Magazine surveyed the thin-film research community in August 2001 to determine the level of involvement with thin-film characterization tools and the immediate research concerns

[22]. The survey indicated that thin films and coatings are commonly used in components and devices

to improve mechanical properties, material performance, durability, strength, and resistance in basic

industries, such as industrial coatings (21% of researchers’ responses), nanotechnology (19%), optical

components (19%), plastics (17%), ceramics (15%), biomedical technology (10%), instrumentation

(10%), microelectromechanical systems (10%), and disk drives (6%). Further, according to the survey,

the most widely used tools for examining thin films and coatings are optical microscopy (60%), scanning

electron microscopy (56%), energy-dispersive x-ray spectroscopy (29%), Fourier transform infrared spectroscopy (29%), surface profilometry (29%), x-ray diffraction (27%), Auger electron spectroscopy (25%),

ellipsometry (23%), scanning probe microscopy (19%), transmission electron microscopy (19%), thermal

analysis (15%), x-ray photoelectron spectroscopy (12%), confocal microscopy (10%), and secondary

ion mass spectroscopy (8%).

Surface analysis is important for verifying the success of the surface preparation process including

a coating process or surface treatment, for controlling the surface quality, and for identifying the surface

contamination that can either enhance or inhibit the surface effects of the material. Selecting the proper

analytical tool and method is crucial to obtaining the right information. To select the proper tool, the

researcher must know the size of the specimen, the sampling area, the sampling depth, the spatial resolution, the detection sensitivity, whether quantitative or qualitative results and destructive or nondestructive

analysis are desired, and many other factors. Each technique has its strengths and weaknesses. Therefore,

no single tool can provide the answers to all problems. In many cases, it will be necessary to use multiple

tools to reach an answer.

This chapter describes selected surface analytical tools that are being used in understanding phenomena and mechanisms of oxidation, adhesion, bonding, friction, erosion, abrasion, and wear and in defining

the problems. The reader will find the basic principles and instrumentation details for a wide range of analytical tools in the literature [8–10, 19]. However, the analytical instrumentation field is moving rapidly,

and within a year current spatial resolutions, sensitivities, imaging and mapping capabilities, accuracies,

and instrument cost and size are likely to be out of date. Therefore, these references should be viewed

with caution.
NASA/TM—2002-211815 2

Nature of Surface Analysis

A surface, by definition, is an interface, a marked discontinuity from one material to another. Because

no change in nature is ever instantaneous, any real surface has a finite depth, and in characterizing a surface one must at some point consider just what this depth is.

The elemental and chemical state, phase, microstructure, crystalline structure, and defects of a solid

often vary as a function of depth into the material or

spatially across the material. Many tools specialize

in addressing these variations down to extremely fine

dimensions (on the order of angstroms in some cases).

Requests are made for physical and chemical information as a function of depth to depths of 1 mm or so

(materials have about 3 million atomic layers per

millimeter of depth), as shown in fig. 1. It is this

region that affects a broad spectrum of physical,

chemical, mechanical, and structural properties.

Knowledge of these variations is of great importance

to the selection and use of bulk materials, thin films,

and modified surfaces.

Tables 1 to 3 briefly summarize the selected

common tools available to surface engineers and

tribologists today in studying the properties and

behavior of solid surfaces. They give the commonly

used tools, the information that can be obtained from

the analysis, the vertical (depth) and the lateral (spatial) resolution that can be probed, and the form of

the required specimen. For surfaces, interfaces, and

thin films there is often little material to analyze—

hence, the presence of many microanalytical methods in tables 1 to 3. Within microanalysis it is

often necessary to identify trace components down

to extremely low concentrations (parts per trillion in

some cases), and a number of tools specialize in this

aspect.

In other cases a high degree of accuracy in measuring the presence of major components might be

the issue. Usually, the tools that are good for trace

identification do not accurately quantify major

components. Most complete analyses require the

use of multiple analytical tools, the selection of

which depends on the nature of the specimen and

the desired information.

Figure 1.—Schematic diagram showing regimes 

 of (a) surface analysis, (b) thin-film analysis, 

 (c) interface analysis, and (d) bulk substrate 

 analysis.

1 to 3 nm

(b)

10 to 30 nm

(c)

1 mm

100 nm to 1m

(d)

Sampling

depth

from 

surface

Contaminant

Solid

surface

(a)
NASA/TM—2002-211815 3

Surface Chemistry

Tools included in table 1 primarily provide elemental and chemical information on surfaces, interfaces, and thin films. The surface tools usually require a high vacuum. In most analyses the specimen is

subjected to some kind of radiation beam: electrons, photons (light), ions, x rays, and neutral species. As

a result of interactions between the solid surface and the incoming radiation, a beam of a similar (or a

different) nature will emerge from the specimen. Measurement of the physical and/or chemical attributes

of this emerging radiation will yield qualitative, and often quantitative, information about the chemistry,

topography and morphology, and structure of the surface being probed.

TABLE 1.— SELECTED ANALYTICAL TOOLS FOR SURFACE CHEMISTRY

Technique Main information Vertical resolution

(depth probed)

(typical)*

Lateral resolution

(typical)

Types of solid

specimen

(typical)

Auger electron

spectroscopy (AES)

Elements (all except

hydrogen and helium)

Chemical state

Depth profiling

Image and mapping

0.5 nm to several

nanometers

A few tens of

nanometer or less

Ultra-highvacuumcompatible

solids

X-ray photoelectron

spectroscopy (XPS)

Elements (all except

hydrogen and helium)

Chemical state

Bonding

Organic compounds

Depth profiling

Imaging and mapping

0.5 nm to several

nanometers

5 mm to 5 mm Ultra-highvacuumcompatible

solids

Secondary ion mass

spectroscopy

(SIMS)

Chemical state

Elements (hydrogen to

uranium)

Isotopes

Depth profiling

Imaging

0.1 mm to 1 mm 0.5 nm to 10 mm All; vacuumcompatible

solids

Rutherford

backscattering

spectrometry (RBS)

Elements

Structure

Defects

2 nm to 30 nm 1 mm to 4 mm; 1 mm

in specialized case

Ultra-highvacuumcompatible

solids

Electron probe x-ray

microanalysis

(EPMA)

Elements (beryllium to the

actinides)

SEM imaging

Compositional mapping

1 mm 0.5 mm to 1 mm All; vacuumcompatible

solids

Energy-dispersive or

wavelengthdispersive X-ray

spectroscopy (EDS

or WDS)

Elements (Z≥5; boron to

uranium)

Spectroscopy

Imaging/mapping

0.02 mm to 1 mm 0.5 mm to 1 mm for

bulk specimens; as

small as 1 nm for thin

specimens

All; vacuumcompatible

solids

Fourier transform

infrared

spectroscopy (FTIR)

Elements (all but not element

specific)

Chemical bonds

Stress

Structure order

Defects

Imaging and mapping

10 nm to

micrometers

20 mm to 5 mm All; solid,

liquid, or gas in

all forms

Raman spectroscopy Identification of unknown

compounds

Elements (all but not element

specific)

Chemical state

Bonding state

Structural order

Phase transitions

Few micrometers

to millimeters

1 mm Solids, liquids,

gases, and thin

films

* The vertical resolution is a measurement of the technique’s ability to clearly distinguish a property as a function of

depth.
NASA/TM—2002-211815 4

Auger electron spectroscopy (AES), x-ray photoelectron spectroscopy (XPS) or electron spectroscopy

for chemical analysis (ESCA), secondary ion mass spectroscopy (SIMS), and Rutherford backscattering

spectroscopy (RBS) have become the standard set of surface, thin-film, and interface analytical tools.

Each has its own strengths and weaknesses and mostly they are complementary. AES and XPS each can

determine the elemental composition (except for hydrogen and helium) and the chemical state of the outermost atomic layers of a surface [1, 2, 15–19]. SIMS can detect hydrogen and helium and has a much

higher absolute sensitivity in many cases, but it seldom gives any chemical information and does not

identify bonding characteristics as would XPS. SIMS, by its nature, has to remove material to do its

analysis. RBS readily produces good quantitative results and does nondestructive depth profiling, but it

lacks the absolute sensitivity of AES to many of the important elements and its depth resolution is not as

good as AES can produce, in many cases.

AES and XPS both are surface-sensitive tools for probing the surface chemistry of solids. There are,

however, a number of practical differences between the two tools (e.g., detection speed, background,

and spatial resolution). XPS is more often selected to determine chemical information than is AES. The

particular strengths of XPS are quantitative chemical state analysis and elemental analysis of surfaces

(without standards). Although these techniques derive their usefulness from their intrinsic surface sensitivity, they can also be used to determine the composition of deeper layers. Such a determination is

normally achieved through controlled surface erosion by ion bombardment. AES or XPS analyzes the

residual surface left after a certain sputtering time with rare gas ions. In this way composition depth

profiles can be obtained that provide a powerful means for analyzing worked layers, modified layers, thin

films, multiple-layered coatings, lubricants, reaction film products, transferred films, and their interfaces.

AES is generally more advantageous in composition depth profiling than is XPS.

AES—AES uses a focused electron beam to create secondary electrons near a solid surface. Some

of these electrons (the Auger electrons) have the characteristic energies of the elements. AES has the

attributes of high lateral resolution (10 nm with a field emission electron source) and an analysis depth

to 10 nm, relatively high sensitivity, and standardless semi-quantitative elemental analysis. In addition,

some of the Auger electrons detected have energies characteristic, in many cases, of the chemical bonding

of the atoms from which they are released. Because of their characteristic energies and the shallow depths

from which they escape without energy loss, Auger electrons can characterize the elemental composition

and, at times, the chemistry (chemical bonding information in some cases) of surfaces. The Auger peaks

of many elements show significant changes in position or shape in different chemical conditions and environments. Further, the high spatial resolution of the electron beam and the sputter etching process allow

microanalysis of three-dimensional regions of solid specimens.

A study of aluminum is an example of effective AES analysis. Figure 2(a) presents an AES spectrum

of a chemically polished surface of a single-crystal aluminum pin specimen examined in ultrahigh

vacuum (10–9 Pa). A carbon contamination peak is evident as well as an oxygen contamination peak.

Carbon and water are ubiquitous on any solid surface. Even a supposedly “clean” surface will show a

significant carbon and water contribution to the AES spectrum because of the presence of one or more

layers of adsorbed hydrocarbons. The surfaces of metals and ceramics usually contain, in addition to the

constituent atoms, adsorbed films of water vapor, carbon monoxide and dioxide, and other oxide layers.

A contaminant layer will attenuate the electron signal from the underlying surface and may mask important features in the spectrum. In fig. 2(a) the aluminum and oxygen peaks indicate that the surface was

covered with aluminum oxide (Al2O3) as well as a simple adsorbed oxygen film. In addition to the major

AES peaks the chemically polished aluminum surface could contain small amounts of contaminant species, such as silicon and nitrogen.

In a vacuum environment sputtering with rare gas ions or heating can remove contaminants adsorbed

on the surfaces of materials [23]. Figure 2(b) presents the AES spectrum taken after the aluminum pin

specimen had been argon ion sputter cleaned. After the sputtering the contamination peaks became very

small, and the relative peak intensity of aluminum increased markedly. Each contaminant was less than

1%, on the order of typical AES trace capability.
NASA/TM—2002-211815 5

Figure 3 presents the AES spectra of an as-received surface and an argon-ion-sputter-cleaned surface

of a sapphire flat specimen. A carbon contamination peak is evident on the as-received sapphire surface.

The cleaned sapphire surface consisted of Al2O3 and small amounts of carbon and implanted argon. The

contaminants on the cleaned sapphire surface were on the order of typical AES trace capability.

When the contaminated surface of the chemically polished aluminum pin specimen was brought into

contact with the argon-ion-sputter-cleaned surface of the sapphire flat specimen in ultrahigh vacuum, the

pull-off forces (adhesion) required to separate the two surfaces in contact were small. The mean value and

standard deviation of these pull-off forces were 231 and 241 μN (fig. 4), respectively. On the other hand,

300

S1

1.7%

C1

17.6%

N1

1.5%

O1

11.3%

Fe2

1.1%

Zn1

0.9%

Al2

65.8%

600

Kinetic energy, eV

900 1200 1500

(a)

0

dN(E)/dE

Ar1

0.3%

C1

0.7%

N1

0.3%

O1

0.4%

Fe2

0.7%

Al2

97.7%

300 600

Kinetic energy, eV

900 1200 1500

(b)

0

dN(E)/dE

Figure 2.—AES spectra of single-crystal aluminum pin surfaces. (a) Chemically 

 polished surface; 3-keV electron beam. (b) Argon-ion-sputter-cleaned surface; 

 3-keV electron beam.
NASA/TM—2002-211815 6

when the argon-ion-sputter-cleaned aluminum pin specimen was brought into contact with the argon-ionsputter-cleaned sapphire flat specimen in ultrahigh vacuum, strong bonds formed between the two materials. The mean value and standard deviation of the pull-off forces required to separate the two surfaces in

contact were 3015 and 298 μN, respectively (fig. 4). The presence of a contaminant film on an aluminum

surface reduced adhesion by a factor of 13. Clearly, the importance of surface chemistry on the adhesion

behavior of two solid surfaces in contact is demonstrated in the data of fig. 4.

XPS—In XPS monoenergetic soft x rays bombard a specimen material, causing electrons to be

ejected. The elements present in the specimen can be identified directly from the kinetic energies of these

ejected photoelectrons. Electron binding energies are sensitive to the chemical state of the atom. Although

C1

0.9%

300 600

Kinetic energy, eV

900 1200 1500

(b)

0

dN(E)/dE

Ar1

1.6%

O1

27.8%

Al2

69.7%

300

C1

40.9% O1

25.3%

600

Kinetic energy, eV

900 1200 1500

(a)

0

dN(E)/dE

Figure 3.—AES spectra of single-crystal sapphire flat surfaces. (a) As-received surface; 

 2-keV electron beam. (b) Argon-ion-sputter-cleaned surface; 3-keV electron beam.

Al2

33.5%
NASA/TM—2002-211815 7

XPS is designed to deal with solids, specimens can be

gaseous, liquid, or solid. XPS is applicable to metals,

ceramics, semiconductors, and organic, biological, and

polymeric materials. Although x-ray beam damage can

sometimes be significant, especially in organic materials, XPS is the least destructive of all the electron or

ion spectroscopy methods. The depth of solid material

probed by XPS varies from the top 2 atomic layers to

15 to 20 layers (an analysis depth to 0.5 to 5 nm). XPS

has the lateral resolution of 5 mm to 75 μm (5 μm in

special instruments). This surface sensitivity, combined

with quantitative and chemical analysis capabilities, has

made XPS the most broadly applicable general surface

analysis tool used today, especially in the field of surface engineering and tribology. The main advantage of

XPS is its ability to provide chemical information from

the shifts in binding energy.

One classic study of single-crystal silicon carbide

(SiC) heat treated at 1500 °C in vacuum is an example

of effective XPS analysis [23, 24]. In the study in situ

XPS analyses were conducted with the heat-treated

SiC. Also, single-pass sliding experiments were conducted with the heat-treated SiC in contact with iron

at various temperatures from room temperature to 1200 °C in ultrahigh vacuum. As depicted in fig. 5

the XPS spectra of the heat-treated SiC surface indicate distinguishable kinds of carbon (i.e., a large

graphite peak and a small carbide peak associated with the SiC as a result of the chemical shifts). XPS

analysis revealed that, concurrently, graphitic carbon replaced carbidic carbon at the topmost layers of Pull-off (adhesion) force, 

μ

N

3500

3000

2500

2000

1500

1000

500

0 Clean

aluminum

surface

Contaminated

aluminum

surface

Surface condition

Figure 4.—Pull-off force (adhesion) for clean 

 aluminum pin in contact with clean sapphire 

 flat at normal load of 135 μN and for contam- 

 inated aluminum pin in contact with clean 

 sapphire flat at 1063 μN in ultrahigh vacuum. Coefficient of friction

0.6

0.4

0.2 0 400 800 1200

Sliding temperature, °C

Figure 5.—XPS spectra of silicon carbide surface heat-treated to 1500 °C 

 and measured coefficients of friction on that surface to 1200 °C after 

 heat treatment.

(b)

Sliding

direction

<1010>

<1120>

Intensity, N(E)

104 102 100 98 96

Binding energy, eV

(a)

Si2p XPS peak

Si

Intensity, N(E)

292 290 288 286 276 284 282 280 278

Binding energy, eV

C1S XPS peaks

Graphite

Carbide
NASA/TM—2002-211815 8

SiC, as a result of the evaporation of silicon. The outermost surficial graphite layer on the SiC heat

treated at 1500 °C was 1.5 to 2.4 nm in depth. The coefficients of friction for the graphitized SiC in

vacuum were generally low. The heat-treated SiC had lower coefficients of friction, by more than onehalf, than those for nongraphitized, clean SiC surfaces. The coefficient of friction dropped from 0.8 for

the nongraphitized, clean SiC surfaces to 0.2 for the graphitized surfaces. Note that the carbide peak

obtained from the nongraphitized, clean SiC surface dominated in the XPS spectrum. Thus, this study

demonstrated that heat treatment of SiC at 1500 °C converted the surface exhibiting high friction to low

friction and identified the surface chemical changes responsible for the friction behavior. The results of

fig. 5 illustrate the value of surface analytical approaches in friction investigations [23, 25].

Topography and Morphology

Surface imaging analyses (e.g., table 2) are important for assessing the preparation process, phase,

damage, defects, or morphological characteristics of solid surfaces. They provide a visual feel for the surface of a device and can quickly identify problem areas. Observation and topography measurement of the

physical attributes will yield qualitative, and often quantitative, information about the morphology of the

surface being probed. Scanning electron microscopy (SEM), optical interferometry (optical profilometry),

and atomic force microscopy (AFM) have become the standard set of imaging analytical tools. Each has

its own strengths and mostly they are complementary.

SEM—SEM is an excellent first-look analytical tool when conventional light microscopy no longer

provides adequate spatial resolution or depth of focus. SEM is the most common surface imaging tool to

materials engineers, surface engineers, and tribologists interested in studying the morphology, defects,

fractures, erosion, and wear of material surfaces.

In SEM an electron beam is focused into a fine probe and subsequently raster scanned over a small

rectangular area. As the electron beam interacts with the specimen, it creates various signals, such as

secondary electrons, internal currents, and photon emissions, all of which can be collected by appropriate

detectors. The use of electron microprobe tools in SEM is now a well-established procedure. Especially,

the combination of SEM and x-ray analysis utilizing either energy-dispersive x-ray spectroscopy (EDS)

or wavelength-dispersive x-ray spectroscopy (WDS) provides a powerful tool for local microanalysis.

SEM–EDS or SEM–WDS produces three principal images: secondary electron images, backscattered

electron images, and elemental x-ray energy maps or x-ray energy histograms. Secondary electrons carry

information about surface topography and morphology. Backscattered primary electrons carry information about atomic number and topographic contrast. X-rays carry information about elemental composition and an element’s concentration distribution. Three modes of analysis are commonly used: spectrum

acquisition, spatial distribution or dot-mapping of the elements, and element line scans. X-rays are

generated over a larger volume than are either the backscattered or secondary electrons detected. Thus,

the spatial resolution of x-ray maps (0.5 to 1 μm) is much larger than that of secondary electron images

(~1.5 nm with a field emission electron source) or backscattered electron images.

One example of SEM–EDS analysis is a study of titanium-6% aluminum-4% vanadium (Ti-6Al-4V)

in vacuum. In the study multiple-pass sliding friction experiments were conducted with the Ti-6Al-4V in

contact with a typical nickel-base superalloy in vacuum at room temperature. Substantial plastic deformation and severe surface damage occurred on the Ti-6Al-4V surface when sliding against the superalloy

in vacuum [26]. Figure 6 presents a secondary electron SEM image, a backscattered electron SEM image,

and an x-ray energy histogram of the wear surface produced on the superalloy after 100 passes at a load

of 2.5 N. Figure 6 shows a Ti-6Al-4V patch on the wear track of the superalloy surface. The interfacial

bonds (adhesion) between the two materials in contact in vacuum are generally strong, and seizure

between the two contacting materials can occur. Seizure (or galling) increased the coefficient of friction

to 1.4. Failure of Ti-6Al-4V generally occurs either in tension or in shear because some of the interfacial
NASA/TM—2002-211815 9

TABLE 2.— SELECTED IMAGING ANALYTICAL TOOLS FOR TOPOGRAPHY AND MORPHOLOGY

Technique Main information

obtained

Vertical resolution (depth

probed) (typical)*

Lateral resolution (typical) Types of solid

specimen

(typical)

Scanning

electron

microscopy

(SEM)

Imaging

Morphology

Elements

Damages

Defects

Crystallography

Grain structure

Magnetic domains

Variable from a few

nanometers to a few

micrometers

1 to 50 nm in secondary

electron mode

Conductors and

coated insulators

Optical profiler

and laser

interferometry

3D and 2D imaging

Morphology

Profilometry

Topography

Film thickness

Wear volume

Scar and crater depth

Surface defects

~0.1 nm A few submicrometers to a

few tens of micrometers

All but

transparent films

and materials

Atomic force

microscopy

(AFM) or

scanning force

microscopy

(SFM)

Topography

Friction force mapping

Morphology

Profilometry

Film thickness

Wear volume

Scar and crater depth

Structure

Surface defects

<0.03 nm to 0.05 nm Atomic to 1 nm All

Stylus

profilometry

Profilometry

Topography

Film thickness

Morphology

Scar and crater depth

Wear volume

Surface defects

0.5 nm 100 nm Almost all;

flat smooth films

Confocal

microscopy

3D and 2D imaging

Morphology

Profilometry

Topography

Film thickness

Wear volume

Scar and crater depth

Surface defects

Live cells

Variable from a few

nanometers to a few

micrometers

Variable; optical, 0.5 mm to

4 mm; SEM, 1 mm to

50 mm

Almost all

Transmission

electron

microscopy

(TEM)

Atomic structure

Microstructure

Crystallography defects

Imaging and mapping

Morphology

None £0.2 nm Conductors,

semiconductors,

coated insulators

Light

microscopy

(general)

Imaging

Morphology

Damages

Defects

Phase

Magnetic flux and field

Variable Variable All

* The vertical resolution is a measurement of the technique’s ability to clearly distinguish a property as a function of

depth.
NASA/TM—2002-211815 10 Counts

Al

Au Au

V and 

Cr Fe Ni

Ti and V

Ti

Energy, keV

(c)

(a)

(b)

Figure 6.—Large transferred patch of Ti-6Al-4V on nickel-base superalloy disk 

 specimen after sliding by Ti-6Al-4V pin specimen at 2.5 N in vacuum, showing

 transfer patches of Ti-6Al-4V. (a) Secondary electron SEM image. (b) Backscattered

 electron SEM image. (c) EDS spectrum of transferred film on disk. (Data taken at

 point indicated in part (a). Thin gold film used to reduce charging of mount is

 responsible for gold signal in spectrum.)
NASA/TM—2002-211815 11

bonds are generally stronger than the cohesive bonds within the cohesively weaker Ti-6Al-4V. The failed

Ti-6Al-4V subsequently transfers Ti-6Al-4V patches to the contacting superalloy surface. The transfer

patches shown in fig. 6 occupied a large area fraction of the overall wear track. Thus, severe damage,

often called scuffing, scoring, or galling, occurred in the unlubricated contact between the Ti-6Al-4V

and the nickel-base superalloy superalloy in vacuum. The results illustrate the value of the SEM and EDS

surface analytical approaches in seizure (galling) and wear investigations.

Optical interferometry—Optical interferometry is a useful tool available today to surface engineers

and tribologists interested in studying surface topography. Optical interferometry (also called an optical

profiler; a non-contact, vertical-scanning, white-light interferometer; or a non-contact, vertical-scanning,

laser interferometer) can profile an extremely wide range of surface heights and can measure surface

features without contact [27]. It characterizes and quantifies surface roughness, step height, bearing ratio,

height distribution, critical dimensions such as area and volume of damage, eroded craters, wear scars,

and other topographical features. It has three-dimensional profiling capability with excellent precision

and accuracy; for example, profile heights ranging from <1 nm to 5000 μm at speeds to 10 μm/sec with

0.1-nm height resolution and large profile areas to 50 mm by 50 mm or 100 mm by 100 mm.

In optical interferometry light reflected from the surface of interest interferes with light from an

optically flat reference surface. Deviations in the fringe pattern of bright and dark lines produced by the

interference are related to differences in surface height. If an imaging array is used, three-dimensional

information can be provided. In general, optical profilers have some advantages—non-destructive measurement, no specimen preparation, and short analysis time under ambient conditions—but also some

disadvantages. If the surface is too rough (roughness greater than 1.5 mm), the interference fringes can

be scattered to the extent that topography cannot be determined. If more than one matrix is involved (e.g.,

multiple thin films on a substrate) or if the specimen is partially or totally transparent to the wavelength

of the measurement system, measurement errors can be introduced. Multiple-matrix specimens can be

measured if coated with a layer that is not transparent to the wavelength of light used.

The shape of a surface can be displayed by a computer-generated map developed from digital data

derived from a three-dimensional interferogram of the surface. Computer processing and frequency domain analysis result in a quantitative three-dimensional image. Such a map shows details of individual

features and also the general topography over an area and describes surfaces. For example, fig. 7(a)

shows a three-dimensional view of an optical interferometry image taken at the beginning of a wear track

(groove) produced on a gamma titanium aluminide flat (Ti-48Al-2Cr-2Nb in atomic percent) with a

rounded diamond pin (a Rockwell cone diamond with a tip radius of 0.2 mm) in air at room temperature.

In the experiment the surfaces of the Ti-48Al-2Cr-2Nb flat and the diamond pin were brought into contact

and loaded at 100 N, and the single-pass sliding was begun at a sliding velocity of 12 mm/min. Clearly, a

plastically deformed permanent groove was formed on the Ti-48Al-2Cr-2Nb surface where the diamond

began to slide. The plastically deformed Ti-48Al-2Cr-2Nb was subsequently piled onto the sides of the

groove. The quantitative volume, height, and depth of the displaced Ti-48Al-2Cr-2Nb were directly

processed by the computer. In the view of this particular groove the volume and the maximum height,

calculated from the three-dimensional image, of the piled Ti-48Al-2Cr-2Nb on the sides of groove

were 1.64106 μm3 and 30.81 μm, respectively, whereas the volume loss and the groove depth were

1.63106 μm3 and 42.94 μm, respectively. The sliding action also produced cracks, which generally

propagate perpendicular to the sliding direction. The combination of data taken from optical profilometry

and scanning electron microscopy (SEM) verified that the cracks did propagate perpendicular to the sliding direction. The Ti-48Al-2Cr-2Nb failed either in tension or in shear.

Another study was done of a polymer matrix composite (PMC). Erosion tests were conducted with

the PMC in an air-sand erosion rig. Substantial erosion occurred on the PMC surface. Figure 7(b), as

an example, shows a three-dimensional view of an optical interferometry image of an erosion crater for

PMC (vane specimen) eroded at an impact angle of 20° by using 15 g of Arizona road dust as the erodent.

In this particular case the volume loss and maximum depth, calculated from the three-dimensional image,

of the eroded crater were 3.001010 μm3 and 69.42 μm, respectively.
NASA/TM—2002-211815 12

Figure 7.—Optical interferometry images. (a) Three-dimensional view of wear track 

 (groove) produced on gamma titanium aluminide (Ti-48Al-2Cr-2Nb in atomic percent) 

 flat surface with rounded diamond (Rockwell cone diamond with tip radius of 0.2 mm) 

 in air. Volume of material grooved, 1.63106 μm3; depth of groove, 42.94 μm.

 (b) Erosion crater produced on polymer matrix composite vane specimen. Volume 

 loss of material eroded, 3.001010 μm3; depth of eroded crater, 69.42 μm.

459.9

604.2 μm

(a)

μm

31.8

25.0

20.0

15.0

10.0

5.0

0.0

–5.0

–10.0

–15.0

–20.0

–25.0

–30.0

–35.0

–41.9

288

250

200

150

100

50

0

–50

–100

–170 (b)

23.1 mm

11.4

μm
NASA/TM—2002-211815 13

The results of the studies shown in fig. 7 demonstrated that optical interferometry can be a powerful

analytical tool for measuring critical dimensions, such as the volume, depth, and area of the wear scar and

eroded crater, respectively.

AFM—One popular variant of scanning probe microscopy is atomic force microscopy (AFM), also

called scanning force microscopy (SFM). AFM can measure the force of interaction between a specimen

surface and a sharp probe tip [28]. The tip, a couple of micrometers long and often less than 10 nm in

diameter, is located at the free end of a cantilever 100 mm to 200 mm long. When the tip comes within a

few angstroms of the specimen surface, repulsive van der Waals forces between the atoms on the tip and

those on the specimen cause the cantilever to deflect, or bend. A detector, such as the position-sensitive

photodetector, measures the cantilever deflection as the tip is scanned over the specimen or the specimen

is scanned under the tip. As a piezoelectric scanner gently traces the tip across the specimen (or the specimen under the tip), the contact force causes the cantilever to bend to accommodate changes in topography. The measured cantilever deflections allow a computer to generate a map of surface topography.

Atomic force microscopes can be used to study insulating and semiconducting materials as well as electrical conducting materials. Most atomic force microscopes currently used detect the position of the cantilever with optical techniques. The position-sensitive photodetector itself can measure light displacements as

small as 1 nm. The ratio of the path length between cantilever and detector to the length of the cantilever

itself produces a mechanical amplification. As a result the system can detect even 0.1-nm vertical movements of the cantilever tip. Other methods of detecting cantilever deflection rely on optical interference,

a scanning tunneling microscope tip, or piezoresistive detection (fabricating the cantilever from a

piezoresistive material). In addition to having higher spatial resolution than SEM, AFM requires little

or no sample preparation and can analyze specimens in ambient or even hydrated conditions.

The shape of a surface can be displayed by a computer-generated map developed from digital data

derived from many closely spaced parallel profiles taken by this process. Such a map shows details of

individual features and also the general topography over an area and describes surfaces. Many engineering surfaces have height distributions that are approximately Gaussian (i.e., they can be described by the

normal probability function). It is also useful to describe surfaces in terms of the integral of the distribution (bearing ratio), which gives the fraction of the surface at or below each height. The well-known

Abbott’s bearing curve, which gives the contact area that would exist if the hills were worn down to the

given height by an ideally flat body, is the fraction of the surface at or above each height. Many modern

surface analyzers provide chart or video displays of height histogram and bearing ratio (Abbott’s bearing

curve or bearing area curve) as standard features [29]. Figure 8 gives examples of AFM images of an

ion-beam-deposited, diamondlike carbon (DLC) film and a chemical-vapor-deposited (CVD), fine-grain

diamond film, both deposited on mirror-polished silicon substrates (DLC on silicon and CVD diamond

on silicon). The DLC film surface has a smooth, flat morphology. The CVD diamond surface has a granulated or spherulitic morphology: the surface contains spherical asperities of different sizes [30]. The surface roughness of the DLC on silicon is 0.49 nm root-mean-square (rms), and the surface roughness of

the CVD diamond on silicon is 58.8 nm rms. Also, figs. 8(a) and (b) show actual three-dimensional

height profiles, histograms, and bearing ratios for the DLC on silicon and the CVD diamond on silicon,

respectively.

Structure and Crystallography

Three tools included in table 3 all have diffraction in their names and give long-range order information on atomic positions from diffraction patterns. They are nondestructive techniques because of the

specimen preparation methods. Their role is to provide structural information on surfaces, interfaces,

and thin films. Low-energy electron diffraction (LEED) and reflection high-energy electron diffraction

(RHEED) use electrons in high vacuum, whereas x-ray diffraction (XRD) uses x rays in most environments. LEED and RHEED are surface sensitive and provide surface crystallographic information,
NASA/TM—2002-211815 14

0 0

1

2

3

0.00

0.20

1

2

3

μm

μm

μm

1000

Sampling rate, counts/sec

0

2000

3000

4000

5000

Height, nm

Histogram

0 100 200 300 400

Bearing ratio

20

0

Concentration, at.%

0 100 200 300 400

40

60

80

100

Height, nm (b)

0 0

1

2

0

50

100

1

2

nm

μm

μm

5 000

0 0

Sampling rate, counts/sec

4 8 12

10 000

15 000

20 000

25 000

Height, nm

Histogram Bearing ratio

20

0

Concentration, at.%

0 4 8 12

40

60

80

100

Height, nm (a)

Figure 8.—Atomic force micrographs of carbon films deposited on mirror-polished 

 silicon substrates. (a) Ion-beam-deposited, diamondlike carbon film. (b) Chemical-

 vapor-deposited, fine-grain diamond film.
NASA/TM—2002-211815 15

whereas XRD is a bulk method and provides bulk crystallographic and structural information. In standard

form LEED and RHEED do not have much spatial resolution, beam spot sizes being a fraction of a millimeter. Microscopic modes using beam columns exist, however. Usually, XRD does not provide spatial

resolution, but for special applications, resolution of greater than ~10 μm can be obtained with a

microfocus source and a suitably thin film (~1 μm). One of the disadvantages of XRD, compared with

electron diffraction, is the low intensity of diffracted x rays, particularly for low-atomic number (Z) materials. Typical intensities for electron diffraction are ~108 times larger than for XRD.

LEED is the best known and most widely used tool for investigating the crystallography of surfaces

and overlayers or films adsorbed on surfaces. LEED is a standard tool in the analysis of single-crystal

surfaces. LEED uses normal incidence, with electron energies between 10 eV and 1000 eV, whereas

RHEED uses grazing incidence and detection, with electron energies between 5 keV and 50 keV. The

diffraction pattern and the intensity distribution in the diffracted beams from rows of atoms can provide

information on the positions of atoms in the surface and on the existence of various kinds of crystallographic disorder in the periodic arrangement of surface atoms. LEED gives information on surface order

and cleanliness, surface atomic structure, adsorbed gas or oxide, phase transition in overlayers or surfaces,

and chemical reactions of surfaces.

RHEED is the most similar to LEED, differing mainly by using grazing incidence instead of normal

incidence. It is a surface-sensitive tool for probing surface structures and is ideally suited for the study

of single-crystal surfaces. Although RHEED is a standard tool in the analysis of single-crystal surfaces, it

can be used to study disordered real crystal surfaces and polycrystalline surfaces. When used to examine

a real crystal surface, RHEED gives information on surface crystalline structure, crystallographic orientation, surface reconstruction (the rearrangement of surface atoms to minimize the surface energy), degree

of surface disorder, and degree of surface roughness.

TABLE 3.— SELECTED ANALYTICAL TOOLS FOR STRUCTURE AND CRYSTALLOGRAPHY

Technique Main information Vertical resolution

(depth probed)

(typical)*

Lateral resolution

(typical)

Types of solid

specimen (typical)

and use

(popularity)

Low-energy electron

diffraction (LEED)

Crystallography

Structure

Surface cleanliness

Surface disorder

Defects

Adsorbed gas

Oxide

Chemical reaction

Phase transition

Imaging

~0.4 nm 0.1 mm (~10 mm

available)

Single crystal

(conductors,

semiconductors,

and insulators);

polycrystalline

specimens under

special

circumstances

Reflection highenergy electron

diffraction

(RHEED)

Crystallography

Structure

Surface cleanliness

Surface disorder

Defects

Surface roughness

Deposited film growth

Phase transition

Imaging

2 nm to 10 nm 200 mm by 4 mm Single crystal

(conductors and

semiconductors);

polycrystalline

specimens under

special

circumstances

X-ray diffraction

(XRD)

Crystalline phases

Strain state

Diffusion

Atomic spacings

Atomic arrangements

Crystallite orientation

Grain size

Defects

Film thickness

A few

micrometers;

~5 nm achievable

with laboratorybased equipment

Normally none;

although ~10 mm

with microfocus

All

* The vertical resolution is a measurement of the technique’s ability to clearly distinguish a property as a function of

depth.
NASA/TM—2002-211815 16

Figure 9 shows classic examples of crystal structural damage in manganese-zinc (Mn-Zn) ferrite as

verified by RHEED and the effect of the damage on its magnetic properties [31]. On a magnetic tape

recorder the sliding of the magnetic tape abrades the Mn-Zn ferrite head and scratches its surface. Considerable surficial plastic flow occurs on the ferrite surface, and the large number of defects produced can

drastically change the crystalline state of the ferrite head and produce a worked layer on its surface. The

worked layer decreases readback signal amplitude and degrades the signal obtained in short-wavelength

recording. Figure 9(a) shows the readback signals from a new, chemically etched single-crystal Mn-Zn

ferrite magnetic head in sliding contact with a magnetic tape as a function of sliding distance. Figures 9(b)

and (c) show the electron diffraction patterns taken from the magnetic head surface before and after sliding. Clearly, the sliding action changed the crystalline state of the magnetic head’s surficial layer from a

single-crystal structure to a nearly amorphous one. That crystallographic change in Mn-Zn ferrite is a

critical factor in the readback signal losses shown in fig. 9(a).

When RHEED is used to study film growth on crystalline surfaces, it gives information on the nucleation, growth, and growth rate of epitaxial films (e.g., molecular beam epitaxy (MBE); structural changes

as a function of temperature or time; the deposited film growth mode (i.e., whether it grows layer by layer

or as three-dimensional crystallites); the crystalline structure; and the film’s orientation with respect to the

substrate).

XRD is the classical, most widely used tool for general crystalline material characterization. With

the use of high-brightness x-ray sources the surface structure also can be determined by grazing incidence

methods. XRD offers unparalleled accuracy in measuring atomic spacings. It identifies crystalline phases

present in materials and measures the structural properties of these phases, such as strain state, crystallite

size, grain size, epitaxy, phase formation and composition, preferred orientation, diffusion, and defect

structure. XRD is also used to determine the thickness of thin films and multiple layers and the atomic

arrangements in amorphous materials including polymers and at interfaces.

(b) (c)

198

165

122

52

Head

displacement,

μm

Readback signal, dB –5

0 10

–4

20 30 40 50 60

–3

–2

–1

0

Sliding distance, km

Estimated signal

loss due to tape wear

(a)

Figure 9.—Crystal structure and magnetic signal as function of sliding distance. Sliding 

 materials, chemically etched Mn-Zn ferrite and magnetic tape. (a) Readback signal.

 Electron diffraction patterns of (b) highly strained single-crystal structure before

 sliding and (c) nearly amorphous structure after 60 km of sliding.
NASA/TM—2002-211815 17

Concluding Remarks

Surface modifications, thin films, and multiple-layered coatings designed for engineering materials

will become more important in the future. To understand the benefits that surface engineering techniques

provide, and ultimately to devise better ones, researchers must study the chemical, physical, and structural

characteristics of material surfaces obtained by a given process. Therefore, the use of surface analyses and

surface characterization tools will grow in importance.

A wide variety of analytical tools are available for diagnosing the chemical, physical, and structural

characteristics of surfaces. Each surface analysis technique and its tool provides unique chemical, physical, and structural information. Each technique has its strengths and weaknesses. Therefore, no single tool

can provide the answers to all problems. In many cases, multiple tools must be used to reach an answer.

It should be possible to coordinate the different pieces of information provided by these surface analyses

and tools into a coherent, self-consistent description of surfaces and their bulk characteristics.

References

 1. Miyoshi, K., 2001, Solid Lubrication: Fundamentals and Applications, Marcel Dekker, New York.

 2. Miyoshi, K., and Chung, Y–W., eds., 1993, Surface Diagnostics in Tribology: Fundamental

Principles and Applications, World Scientific Publishing Co., River Edge, NJ.

 3. Burnnell-Gray, J.S., and Datta, P.K., eds., 1996, Surface Engineering Casebook, Solutions to

Corrosion and Wear-Related Failures, Woodhead Publishing Limited, Cambridge, UK.

 4. Bunshah B., et al, eds., 1982, Deposition Technologies for Films and Coatings: Developments

and Applications, Noyes Publications, Park Ridge, NJ.

 5. Mort, J., and Jansen, F., eds., 1988, Plasma Deposited Thin Films, CRC Press, Inc., Boca Raton,

FL.

 6. Holmberg, K., and Matthews, A., 1994, Coatings Tribology: Properties, Techniques, and Applications in Surface Engineering, Tribology Series 28, D. Dowson, ed., Elsevier, Amsterdam.

 7. Kumar, A. , Chung, Y–W., Moore, J.J., and Smugeresky, J.E., eds., 1999, Surface Engineering:

Science and Technology 1, The Minerals, Metals, & Materials Society, Warrendale, PA.

 8. Amelinckx, S., Gevers, R., Remaut, G., and Landuyt, J.V., eds., 1970, Modern Diffraction and

Imaging Techniques in Materials Science, North-Holland Publishing Co., Amsterdam-London.

 9. Briggs, D., Seah, M.P., and Grant, J. T., eds., 1988, Surface and Interface Analysis, ECASIA 87,

Proceedings of the European Conference on Applications of Surface and Interface Analysis,

SIANDQ, Vol. 12, Nos. 1–12, John Wiley & Sons, New York.

10. Brundle, C.R., Evans, C.A., Jr., and Wilson, S., eds., 1992, Encyclopedia of Materials Characterization, Butterworth-Heinemann, Stoneham, MA.

11. Brewis, D.M., ed., 1982, Surface Analysis and Pretreatment of Plastics and Metals, Macmillan,

New York.

12. Miyoshi, K., and Buckley, D.H., 1979, “Friction, Deformation, and Fracture of Single-Crystal

Silicon Carbide,” ASLE Transactions, 22, pp. 79–90.

13. Norton, J.T., and Cameron, G.T., Sr., eds., 1986, “Electron Optical and X-ray Instrumentation for

Research, Product Assurance and Quality Control,” Amray Technical Bulletins, Vol. 2, No. 1,

Amray, Inc., Bedford, MA.

14. Chung, Y–W., and Cheng, H.S., eds., 1991, Advances in Engineering Tribology, STLE SP–31,

Society of Tribologists and Lubrication Engineers, Park Ridge, IL.

15. Chung, Y–W., Homola, A.M., and Street, G.B., eds., 1992, Surface Science Investigations in

Tribology: Experimental Approaches, ACS Symposium Series 485, American Chemical Society,

Washington, DC.
NASA/TM—2002-211815 18

16. Buckley, D.H., 1981, Surface Effects in Adhesion, Friction, Wear, and Lubrication, Tribology

Series 5, Elsevier, Amsterdam.

17. Quinn, T.F.J., 1991, Physical Analysis for Tribology, Cambridge University Press, Cambridge, UK.

18. Glaeser, W.A., ed., 1993, Characterization of Tribological Materials, Butterworth-Heinemann,

Stoneham, MA.

19. Briggs, D., and Seah, M.P., 1983, Practical Surface Analysis: By Auger and X-Ray Photo-Electron

Spectroscopy, Vol. 1, John Wiley & Sons, New York.

20. Tsukizoe, T., 1970, Precision Metrology, Yokkendo Publishing, Tokyo, Japan, pp. 180–199.

21. Williamson, J.B.P., 1984, “The Shape of Surfaces,” CRC Handbook of Lubrication, E.R. Booser,

ed., CRC Press Inc., Boca Raton, FL, Vol. II, pp. 3–16.

22. Studt, T., editor-in-chief, 2001, “Thin-Film Survey, Vacuum/Thin Films,” Research & Development Magazine, 43, 9, p. 84.

23. Miyoshi, K., 1991, “Uses of Auger and X-ray Photoelectron Spectroscopy in the Study of Adhesion

and Friction,” Advances in Engineering Tribology, STLE SP–31, Y–W. Chung and H.S. Cheng,

eds. Society of Tribologists and Lubrication Engineers, Park Ridge, IL, pp. 3–12.

24. Miyoshi, K., and Buckley, D.H., 1983, “Tribological Properties and Surface Chemistry of Silicon

Carbide at Temperatures to 1500 °C,” ASLE Transactions, 26, 1, pp. 53–63.

25. Singer, I.L., 1991, “Solid Lubrication Processes,” Fundamentals of Friction: Macroscopic and

Microscopic Processes, I.L. Singer and H.M. Pollock, eds., Kluwer Academic Publishers,

Dordrecht, pp. 237–261.

26. Miyoshi, K., 1999, “Aerospace Mechanisms and Tribology Technology, Case Study,” Tribology

International, 32, pp. 673–685.

27. Caber, P.J., Martinek, S.J., and Niemann, R.J., 1993, “A New Interferometric Profiler for Smooth

and Rough Surfaces,” WYKO Technical Bulletin 1993–27A, WYKO, Tucson, AZ, pp. 1–14.

28. Howland, R.S., Okagaki, J., and Mitobe, L., 1993, “How to Buy a Scanning Probe Microscope,”

Park Scientific Instruments, Sunnyvale, CA.

29. Miyoshi, K., 2001, “Characterization of Solid Surfaces,” Solid Lubrication: Fundamentals and

Applications, Marcel Dekker, New York, pp. 23–97.

30. Miyoshi, K., and Wu, R.L.C., 2001, “Measurements and Diagnostics of Diamond Films and Coatings,” Measurement, 29, pp. 113–126.

31. Miyoshi, K., Buckley, D.H., and Tanaka, K., 1986, Effect of Crystallographical and Geometrical

Changes of a Ferrite Head on Magnetic Signals During the Sliding Process With Magnetic Tape,

ASLE Special Publication SP–21, pp. 50–56.
This publication is available from the NASA Center for AeroSpace Information, 301–621–0390.

REPORT DOCUMENTATION PAGE

2. REPORT DATE

19. SECURITY CLASSIFICATION

 OF ABSTRACT

18. SECURITY CLASSIFICATION

 OF THIS PAGE

Public reporting burden for this collection of information is estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources,

gathering and maintaining the data needed, and completing and reviewing the collection of information. Send comments regarding this burden estimate or any other aspect of this

collection of information, including suggestions for reducing this burden, to Washington Headquarters Services, Directorate for Information Operations and Reports, 1215 Jefferson

Davis Highway, Suite 1204, Arlington, VA 22202-4302, and to the Office of Management and Budget, Paperwork Reduction Project (0704-0188), Washington, DC 20503.

NSN 7540-01-280-5500 Standard Form 298 (Rev. 2-89)

Prescribed by ANSI Std. Z39-18

298-102

Form Approved

OMB No. 0704-0188

12b. DISTRIBUTION CODE

8. PERFORMING ORGANIZATION

 REPORT NUMBER

5. FUNDING NUMBERS

3. REPORT TYPE AND DATES COVERED

4. TITLE AND SUBTITLE

6. AUTHOR(S)

7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES)

11. SUPPLEMENTARY NOTES

12a. DISTRIBUTION/AVAILABILITY STATEMENT

13. ABSTRACT (Maximum 200 words)

14. SUBJECT TERMS

17. SECURITY CLASSIFICATION

 OF REPORT

16. PRICE CODE

15. NUMBER OF PAGES

20. LIMITATION OF ABSTRACT

Unclassified Unclassified

Technical Memorandum

Unclassified

National Aeronautics and Space Administration

John H. Glenn Research Center at Lewis Field

Cleveland, Ohio 44135–3191

1. AGENCY USE ONLY (Leave blank)

10. SPONSORING/MONITORING

 AGENCY REPORT NUMBER

9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES)

National Aeronautics and Space Administration

Washington, DC 20546–0001

Available electronically at http://gltrs.grc.nasa.gov

August 2002

NASA TM—2002-211815

E–13165–1

WU–297–60–10–00

24

Surface Analysis and Tools

Kazuhisa Miyoshi

Surface properties

Unclassified -Unlimited

Subject Category: 27 Distribution: Nonstandard

Responsible person, Kazuhisa Miyoshi, organization code 5160, 216–433–6078.

This article is a chapter of the book entitled, “Tribology of Mechanical Systems,” to be published by ASME Press,

New York, NY. It describes selected analytical techniques, which are being used in understanding phenomena and

mechanisms of oxidation, adhesion, bonding, friction, erosion, abrasion, and wear, and in defining the problems.

The primary emphasis is on microanalytical approaches to engineering surfaces.