ENCYCLOPEDIA OF MATERIALS CHARACTERIZATIONC phần 1 pdf

ENCYCLOPEDIA
OF
MATERIALS
CHARACTERIZATION
C.
Richard Brundle
Charles
A.
Evans, Jr.
Shaun
Wilson
a
MAT
E
R
I
A
LS
CHARACTER
SERIES
SURFACES, INTERFACES, THIN FILMS
+


ENCYCLOPEDIA
OF
MATERIALS CHARACTERIZATION
MATERIALS CHARACTERIZATION SERIES
Surfaces,
Interfaces, Thin Films
Series Editors: C. Richard Brundle and Charles

A.
Evans,
Jr.
Series Titles
Encyclopedia
of
Materiah Characterization,
C. Richard Brundle,
Characterization
of
Mekth and
Alloys,
Paul. H. Holloway and
P.
N.
Characterization
of
Ceramics,
Ronald E. Loehman
Characterimtion
of
Pobmers,
Ned
J.
Chou, Stephen P. Kowalczyk,
Characterization in Silicon Processing,
Yale Strausser
Characterization in Compound Semiconductor Processing,
Yale Strausser
Characterization

of
Integraed Circuit Packaging Materiah,
Thomas M. Moore and Robert
G.
McKenna
Characterization
of
Cadytic Materiah,
Israel E. Wachs
Characterization
of
Composite Materiah,
Hatsuo Ishida
Characterization
of
Optical Materiah,
Gregory
J.
Exarhos
Characterization
of
Tribological Materiah,
William
A.
Glaeser
Characterization
of
Organic Thin
Films,
Abraham

Ulman
Charles
k
Evans,
Jr.,
and Shaun Wilson
Vaidyanathan
Ravi
Sard,
and Ho-Ming Tong
ENCYCLOPEDIA
OF
MLATERIALS
CHARACTERIZATION
Surfaces, Interfaces,
Thin
Films
EDITORS
C
Ricbard Brundle
Charles
A.
Evans,
Jr.
Sbaun
Wihon
MANAGING EDITOR
Lee
E.
Fitzpatrick

BUTTERWORTH-HEINEMANN
Boston London Oxford Singapore Sydney Toronto Wellington
MANNING
Greenwich
This
book
was
acquired, developed,
and
produced
by
Manning Publications
Co.
Copyright
Q
1992
by
Butxetworch-Heinemann, a
division
of
Reed
Publishing
CUSA)
Inc
Au
rights
rad
No
parc
of

this
publicarion may
be
reproduced,
scored
in
a
retried
system,
or
transmitted,
in any
form
or
by
means. electronic, mechanical, photocopying,
or
orherwise,
without prior written permission
of
the publisher.
Recognizing the importance
of
preserving what has been written, it
is
the policy
of
Butterworth-Heinemann and
of
Manning to have

the
books
they publish printed on
acid-free paper,
and we exert
our
best
&m
to
that
end.
Library
of
Congress
Cataloging-in-Publication
Data
Brundle,
C.
R.
Encyclopedia
of
materials
characterization: surfaces, interfaces, thin films/C. Richard Brundle, Charles
A.
Evans,
Jr.,
Sham Wilson.
p. un (Materials characterization series)
Indudes
bibliographical

refrrenoa
and
index.
ISBN CL7506-9168-9
1.
Surfaces
(Tedmoology)-Tes~
I.
Evans,
Charlak
11.
Wilson,
Shaun.
111.
Title.
IV.
Series.
TA418.7.B73 I992 92-14999
620’.4Pdc20 CIP
Butterworth-Heinemann
80
Montvale Avenue
Stoneham,
MA02180
Manning Publications Co.
3
his Street
Greenwich,
CT
06830

109
8
7
6
5
4
3
Printed
in
the Unired States ofAmerica
Contents
Preface to Series
ix
Preface
x
Acronyms Glossary xi
Contributors xvi
INTRODUCTION AND SUMMARIES
1.0
Introduction
I
Technique Summaries
7-56
IMAGING
TECHNIQUES
(MICROSCOPY)
2.0
Introduction
57
2.1

Light Microscopy
60
2.2
Scanning Electron Microscopy, SEM
70
2.3
Scanning Tunneling Microscopy and
2.4
Transmission Electron Microscopy,
TEM
99
Scanning Force Microscopy, STM and SFM
85
ELECTRON
BEAM
INSTRUMENTS
3.0
Introduction
117
3.1
Energy-Dispersive X-Ray Spectroscopy, EDS
120
3.2
Electron Energy-Loss Spectroscopy in the
Transmission Electron Microscope,
EELS
135
3.3
Cathodoluminescence, CL
149

3.4
Scanning Transmission Electron Microscopy, STEM
161
3.5
Electron Probe X-Ray Microanalysis, EPMA
175
V
STRUCTURE DETERMINATION BY DIFFRACTION AND
SCATTERING
4.0
Introduction
193
4.1
X-Ray Diffraction,
XRD
198
4.2
Extended X-Ray Absorption Fine Structure,
EXAFS
214
4.3
Su&ce Extended X-Ray Absorption Fine Structure and
Near Edge X-Ray Absorption Fine Structure, SEXAFS/NEXAFS
Auger Electron Difiction, XPD and AED
227
4.4
X-Ray Photoelectron and
4.5
Low-Energy Electron Diffraction, LEED
252

4.6
Reflection High-Energy Electron Diffraction, WEED
264
240
ELECTRON EMISSION SPECTROSCOPIES
5.0
Introduction
279
5.1
X-Ray Photoelectron Spectroscopy,
XPS
282
5.2
Ultraviolet Photoelectron Spectroscopy,
UPS
300
5.3
Auger Electron Spectroscopy, AES
310
5.4
Reflected Electron Energy-loss Spectroscopy,
REELS
324
X-RAY EMISION TECHNIQUES
6.0
Introduction
335
6.1
X-Ray Fluorescence,
XRF

338
6.2
Total Reflection X-Ray Fluorescence Analysis,
TXRF
349
6.3
Particle-Induced X-Ray Emission,
PIXE
357
VISIBLE/W
EMISSION, REFLECTION,
AND
ABSORPTION
7.0
Introduction
371
7.1
Photoluminescence,
PL
373
7.2
Modulation Spectroscopy
385
7.3
Variable Angle Spectroscopic Ellipsometry, VASE
401
VIBRATIONAL SPECTROSCOPIES AND NMR
8.0
Introduction
413

8.1
Fourier Transform Infrared Spectroscopy, FTIR
416
8.2
RamanSpectroscopy
428
8.3
High-Resolution Electron Energy
Loss
Spectroscopy, HREELS
4-42
8.4
Solid State Nuclear Magnetic Resonance, NMR
460
vi
Contents
ION
SCATTERING
TECHNIQUFS
9.0
Introduction
473
9.1
Rutherford Backscattering Spectrometry,
RBS
476
9.2
Elastic Recoil Spectrometry, ERS
488
9.3

Medium-Energy Ion Scattering with
Channeling and Blocking, MEIS
502
9.4
Ion scattering Spectroscopy, Iss
514
MASS
AND
OPTICAL SPECTROSCOPIES
10.0
10.1
10.2
10.3
10.4
10.5
10.6
10.7
10.8
10.9
Introduction
527
Dynamic Secondary Ion
Mass
Spectrometry, Dynamic SIMS
Static Secondary Ion Mass Spectrometry, Static SIMS
549
Surfice Analysis by her Ionization, SAL1
Sputtered Neutral Mass Spectrometry, SNMS
Laser Ionization Mass Spectrometry, LIMS
Spark Source Mass Spectrometry, SSMS

598
Glow-Discharge Mass Spectrometry, GDMS
609
Inductively Coupled Plasma Mass Spectrometry, ICPMS
Inductively Coupled Plasma-Optical
Emission Spectroscopy, ICP-OES
633
532
559
586
571
624
NEUTRONANDNUCLEARTECHNIQUES
1'1.0
Introduction
645
1 1
.I
Neutron Diffraction
648
11.2
Neutron Reflectivity
660
11.3
Neutron Activation Analysis, NAA
671
11.4
Nuclear Reaction Analysis, NRA
680
PHYSICAL AND MAGNETIC PROPERTIES

12.0
Introduction
695
12.1
Surface Roughness: Measurement, Formation by
Sputtering, Impact on Depth Profiling
698
12.2
Optical Scatterometry
711
12.3
Magneto-optic Kerr Rotation, MOJSE
723
12.4
Physical and Chemical Adsorption Measurement of
Solid Surface
Areas
736
Contents
vii

Preface
to
Series
This
Materialj Characterization
Series
attempts to address the needs of the practi-
cal materials user, with an emphasis on the newer areas of surfice, interface, and
thin film microcharacterization. The Series is composed of the leading volume,

Enychpedia
of
Materialj Characterization,
and a set of about
10
subsequent vol-
umes concentrating on characterization
of
individual materials classes.
In the
Encyclopedia,
50
brief articles (each
10-18
pages in length) are presented
in a standard format designed for ease of reader access,
with
straightforward
technique descriptions and examples of their practical use. In addition to the arti-
cles, there are one-page summaries for every technique, introductory summaries
to groupings of related techniques, a complete glossary of acronyms, and a tabu-
lar comparison of the major features of
all
50
techniques.
The
10
volumes in the Series on characterization of particular materials classes
include volumes on silicon processing, metals
and

alloys, catalytic materials,
integrated circuit packaging, etc. Characterization is approached from the mate-
rials user’s point of view. Thus, in general, the format is based on properties, pro-
cessing steps, materials classification, etc., rather than on a technique. The
emphasis of
all
volumes is on surfaces, interfaces, and thin films, but the emphasis
varies depending on the relative importance of these areas for the materials class
concerned. Appendixes in each volume reproduce the relevant one-page summa-
ries from the
Encyclopedia
and provide longer summaries for any techniques
referred to that are not covered in the
Envcbpedia
The concept for
the
Series came firom discussion with Marjan Bace of Manning
Publications Comparly.
A
gap exists between the way materials characterization
is often presented and the needs of a large segment of the audience-the materials
user, process engineer, manager, or student. In our experience, when, at the end of
talks
or courses on analytical techniques, a question is asked on how a particular
material (or processing) characterization problem can be addressed the answer
often is that the speaker is “an expert
on
the technique, not the materials aspects,
and does not have experience with that particular situation.” This Series is an
attempt to bridge this gap by approaching characterization problems from the

side of the materials user rather than from that
of
the analytical techniques expert.
We would like to thank Marjan Bace for putting forward the original concept,
Shaun Wilson of Charles Evans and Associates and Yale Strausser of Surface Sci-
ence Laboratories fbr help in hrther defining the Series,
and
the
Editors
of
all
the
individual volumes for their efforts
to
produce practical, materials user based
volumes.
CR
Brundle
C.A.
Evans,Jr.
ix
This volume contains
50
articles describing analytical techniques for the charac-
terization of solid materials, with emphasis on surfaces, intedices, thin films,
and microanalytical approaches.
It
is part of the
Materzah Characterization Series,
copublished by Buttenvorth-Heinemann and Manning. This volume can serve

as
a
stand-alone reference
as
well
as
a companion to the other volumes in the Series
which deal with individual materials
classes.
Though authored by professional
characterization experts the articles are written to be easily accessible to
the
materials user, the process engineer, the manager,
the
student-in short to
all
those
who are not (and probably don’t intend to be) experts but who need to understand
the potential applications of the techniques to materials problems. Too often,
technique descriptions are written for
the
technique specialist.
With
50
articles, organization of the book was difficult; certain techniques
could equally well have appeared in more than one place. The organizational
intent of the Editors
was
to group techniques that have a similar physical basis,
or

that provide similar types
of
information. This is not the traditional organiza-
tion of an encyclopedia, where articles are ordered alphabetically. Such ordering
seemed less useful here, in part because many of the techniques have multiple pos-
sible acronyms (an
Acronym
Glossavy
is provided to help the reader).
The articles follow a standard format
for
each technique:
A
clear description
of the technique, the range of information it provides, the range of materials to
which it is applicable, a
few
typical examples,
and
some comparison to other
related techniques. Each technique
has
a “quick reference,” one-page summary in
Chapter
1
,
consisting
of
a descriptive paragraph and a tabular summary.
Some of

the
techniques included apply more broadly than just to
surhces,
interhces,
or
thin films; for example X-Ray Diffraction and Infrared Spectros-
copy, which have been used for
half
a
century in bulk solid and liquid analysis,
respectively. They are included here because they have by now been developed to
also
apply to surfaces.
A
fay
techniques that are applied almost entirely to bulk
materials (e.g., Neutron Diffraction) are included because they give complemen-
tary information to other methods
or
because they are referred to significantly in
the
10
materials volumes in the Series. Some techniques were left out because
they were considered to be too restricted to specific applications
or
materials.
We wish
to
thank
all

the
many contributors for their efforts, and their patience
and
restraint in dealing with the Editors who took a hirly demanding approach
to establishing the format, length, style, and content of the articles. We hope the
readers will consider our efforts worthwhile. Finally, we would like to thank Lee
Fitzpatrick
of
Manning Publications
Co.
for her professional help as Managing
Editor.
C.
R.
Brund.
CA.
Evans,
/r.
S.
Mhon
Acronyms
Glossary
This glossary lists
all
the acronyms referred to in the encyclopedia together with
their meanings. The major technique acronyms are listed alphabetically. Alter-
natives to these acronyms are listed immediately below each of these entries, if
they exist. Related acronyms (variations
or
subsets of techniques; terminology

used within the technique area) are grouped together below the major acronym
and indented to the right. Most, but not
all,
of
the techniques listed here are the
subject of individual articles in this volume.
AAS
AA
VPD-AAS
GFAA
FAA
AES
Auger
SAM
SAM
AED
ADAM
K.E
CMA
AIS
BET
BSDF
BRDF
BTDF
CL
CLSM
EDS
EDX
EDAX
EELS

HEELS
REELS
REELM
EELS
Atomic Absorption Spectroscopy
Atomic Absorption
Vapor Phase Decomposition-Atomic Absorption Spectroscopy
Graphite Furnace Atomic Absorption
Flame Atomic Absorption
Auger Electron Spectroscopy
Auger Electron Spectroscopy
Scanning Auger Microscopy
Scanning Auger Microprobe
Auger Electron Diffraction
Angular Distribution Auger Microscopy
Kinetic Energy
Cylindrical Mirror Analyzer
Atom Inelastic Scattering
Brunauer, Emmett, and Teller equation
Bidirectional Scattering Distribution Function
Bidirectional Reflective Distribution Function
Bidirectional Transmission Distribution Function
Cathodluminescence
Confocal Scanning Laser Microscope
Energy Dispersive (X-Ray) Spectroscopy
Energy Dispersive X-Ray Spectroscopy
Company selling EDX equipment
Electron Energy
Loss
Spectroscopy

High-Resolution Electron Energy-Loss Spectroscopy
Reflected Electron Energy-Loss Spectroscopy
Reflection Electron Energy-Loss Microscopy
Low-Energy Electron-Loss Spectroscopy
xi
PEELS
EXELFS
EELFS
CEELS
VEELS
EPMA
Electron Probe
ERS
HFS
HRS
FRS
ERDA
ERD
PRD
EXAFS
SEXAFS
NEXAFS
XANES
XAFS
FMR
FTIR
FT
Raman
HREELS
HRTEM

GDMS
GDQMS
Gloquad
ICP-MS
ICP
LA-ICP-MS
ICP-Optical
ICP
IETS
IR
FTIR
GC-FTIR
TGA-FTIR
ATR
Parallel (Detection) Electron Energy-Loss Spectrscopy
Extended Energy-Loss Fine Structure
Electron Energy-Loss Fine Structure
Core Electron Energy-Loss Spectroscopy
Valence Electron Energy-Loss Spectroscopy
Electron Probe Microanalysis
Electron Probe Microanalysis
Elastic Recoil Spectrometry
Hydrogen Forward Scattering
Hydrogen Recoil Spectrometry
Forward Recoil Spectrometry
Elastic Recoil Detection Analysis
Elastic
Recoil
Detection
Particle

Recoil
Detection
Extended X-Ray Absorption Fine Structure
Surface Extended X-Ray Absorption Fine Structure
Near-Edge X-Ray Absorption Fine Structure
X-Ray Absorption Near-Edge Structure
X-Ray Absorption Fine Structure
Ferromagnetic Resonance
See
IR
See
Raman
See
EELS
See TEM
Glow Discharge Mass Spectrometry
Glow Discharge
Mass
Spectrometry using
a
Quadruple
Mass
Analyser
Manufacturer name
Inductively Coupled Plasma Mass Spectrometry
Inductively Coupled Plasma
Laser
Ablation ICP-MS
Inductively Coupled
Plasma

Optical Emission
Inductively Coupled Plasma
Inelastic Electron Tunneling Spectroscopy
Infrared (Spectroscopy)
Fourier Transform Infra-Red (Spectroscopy)
Gas Chromatography FTIR
Thermo Gravimetric Analysis FTIR
Artenuated
Total
Reflection
xii
Acronyms Glossary
RA
IRAS
ISS
LEIS
RCE
LEED
LIMS
LAMMA
LAMMS
LIMA
NRMPI
MEISS
MEIS
MOKE
SMOKE
NAA
INAA
NEXAFS

XANES
NIS
NMR
MAS
NRA
OES
PAS
PIXE
HIXE
PL
PLE
PR
EBER
RDS
Raman
FT
Raman
RS
RRS
CARS
Reflection Absorption (Spectroscopy)
Infrared Reflection Absorption Spectroscopy
Ion Scattering Spectrometry
Low-Energy Ion Scattering
Resonance Charge Exchange
Low-Energy Electron Diffraction
Laser Ionization Mass Spectrometry
Laser Microprobe Mass Analysis
Laser Microprobe Mass Spectrometry
Laser Ionization Mass Analysis

Nonresonant Multi-Photon Ionization
Medium-Energy Ion Scattering Spectrometry
Medium-Energy Ion Scattering
Magneto-optic Kerr Rotation
Surface Magneto-optic Kerr Rotation
Neutron Activation Analysis
Instrumental Neutron Activation Analysis
Near Edge X-Ray Absorption Fine Structure
X-Ray Absorption Near Edge Structure
Neutron Inelastic Scattering
Nuclear Magnetic Resonance
Magic-Angle Spinning
Nuclear Reaction Analysis
Optical Emission Spectroscopy
Photoacoustic Spectroscopy
Particle Induced X-Ray Emission
Hydrogen/Helium Induced X-ray Emission
Photoluminescence
Photoluminescence Excitation
Photoreflectance
Electron Beam Electroreflectance
Reflection Difference Spectroscopy
Raman
Spectroscopy
Fourier Transform
Raman
Spectroscopy
Raman Scattering
Resonant Raman Scattering
Coherent Anti-Stokes Raman Scattering

Acronyms
Glossary
xiii
SERS
Surface Enhanced Raman Spectroscopy
Rutherford Backscattering Spectrometry
High-Energy Ion Scattering
Reflected High Energy Electron Diffraction
Scanning Reflection Electron Microscopy
Surfice
Analysis by her Ionization
Post-Ionization Secondary Ion Mass Spectrometry
Multi-Photon Nonresonant Post Ionization
Multiphoton Resonant Post Ionization
Resonant Post Ionization
Multi-Photon Ionization
Single-Photon Ionization
Sputter-Initiated Resonance Ionization Spectroscopy
Surface Analysii by Resonant Ionization Spectroscopy
Time-of-Flight Mass Spectrometer
See
AES
Scanning Electron Microscopy
Scanning Electron Microprobe
Secondary Electron Miscroscopy
Secondary Electron
Backscattered Electron
Secondary Electron Microscopy with Polarization Analysis
Scanning Force Microscopy
Scanning Force Microscope

Atomic Force Microscopy
Scanning Probe Microscopy
Secondary Ion
Mass
Spectrometry
Dynamic Secondary Ion Mass Spectrometry
Static Secondary Ion Mass Spectrometry
SIMS using a Quadruple
Mass
Spectrometer
SIMS using
a
Magnetic Sector
Mass
Spectrometer
See Magnetic SIMS
SIMS using Tune-of-Flight Mass Spectrometer
Post Ionization SIMS
Sputtered Neutrals Mass Spectrometry
Secondary Neutrals
Mass
Spectrometry
Direct Bombardment Electron
Gas
SNMS
Spark
Source
Mass Spectrometry
Spark Source Mass Spectrometry
See TEM

Scanning Tunneling Microscopy
RBS
HEIS
WEED
SREM
SAL1
PISIMS
MPNRPI
MRRPI
RPI
MPI
SPI
SINS
SARIS
TOFMS
SAM
SEM
SE
BSE
SEMPA
SFM
AFM
SPM
SIMS
Dynamic SIMS
Static SIMS
Magnetic SIMS
Sector SIMS
TOF-SIMS
PISIMS

Q-SIMS
SNMS
SNMSd
SSMS
Spark Source
STEM
STM
xiv
Acronyms
Glossary
SPM
Scanning Tunneling Microscope
Scanning Probe Microscopy
Thermal Energy Atom Scattering
Transmission Electron Microscopy
Transmission Electron Microscope
Conventional Transmission Electron Microscopy
Scanning Transmission Electron Microscopy
High Resolution Transmission Electron Microscopy
Selected
Area
Diffraction
Analytical Electron Microscopy
Convergent Beam Electron Diffraction
Lorentz Transmission Electron Microscopy
Thin Layer Chromatography
Tandem Scanning Reflected-Light Microscope
Tandem Scanning Reflected-Light Microscope
See
XRF

TEAS
TEM
CTEM
STEM
HRTEM
SAD
AEM
CBED
LTEM
TLC
TSRLM
TSM
TXRF
UPS
MPS
VASE
WDS
WDX
XAS
XPS
ESCA
XPD
PHD
KE
XRD
GIXD
GIXRD
DCD
XRF
XFS

TXRF
TRXFR
VPD-TXRF
Ultraviolet Photoelectron Spectroscopy
Ultraviolet Photoemission Spectroscopy
Molecular Photoelectron Spectroscopy
Variable Angle Spectroscopic Ellipsometry
Wavelength Dispersive &-Ray) Spectroscopy
Wavelength Dispersive X-Ray Spectroscopy
X-Ray Absorption Spectroscopy
X-Ray Photoelectron Spectroscopy
X-Ray Photoemission Spectroscopy
Electron Spectroscopy for Chemical Analysis
X-Ray Photoelectron Diffraction
Photoelectron Diffraction
Kinetic Energy
X-RayDiffraction
Grazing Incidence X-Ray Diffraction
Grazing Incidence X-Ray Diffraction
Double Crystal Diffractometer
X-Ray Fluorescence
X-Ray Fluorescence Spectroscopy
Total Reflection X-Ray Fluorescence
Total Reflection X-Ray Fluorescence
Vapor Phase Decomposition Total X-Ray Fluorescence
Acronyms
Glossan/
xv
Mark
R

Antonio
BP Research International
Cleveland,
OH
J.
E.
E.
Bagh
IBM Alrnaden Research Center
San
Jose,
CA
Scott Baumann
Charles Evans &Associates
Redwood City,
CA
Christopher
H.
Becker
SRI
International
Menlo Park,
CA
Albert
J. Bevolo
Ames Laboratory,
Iowa State University
Ames,
IA
J. B. Bindell

AT&T Bell Laboratories
Allentown,
PA
Filippo Radicati
di
Brozolo
Charles Evans &Associates
Redwood City,
CA
C.
R
Brundle
IBM Almaden Research Center
San
Jose,
CA
Daniele Cherniak
Rennsselaer Polytechnic Institute
Troy,
NY
Paul
Chu
Charles Evans
&
Associates
Redwood City,
CA
Carl Colvard
Charles
Evans

&
Assoociates
Redwood City,
CA
J. Neal Cox
INTEL, Components
Research
Santa Clara,
CA
John Gustav Delly
McCrone Research Institute
Chicago, IL
Extended X-Ray Absorption Fine Structure
Elastic Recoil Spectrometry
Rutherford Backscattering Spectrometry
Surface
Analysis by
Laser
Ionization
Reflected Electron Energy-Loss Spectro~copy
Scanning Electron Microscopy
Laser
Ionizarion Mass Spectrometry
X-Ray Photoelectron Spectroscopy;
Ultraviolet Photoelectron
Spectroscopy
Nuclear
Reaction
Analysis
Dynamic Secondary Ion

Mass
Spectrometry
Photoluminescence
Fourier Transform Infrared Spectroscopy
Light Microscopy
xvi
Hellmut F.ckert
University
of
California, Santa Barbara
Santa Barbara,
CA
Peter Eichinger
GeMeTec Analysis
Munich
P.
Fenter
Rutgers University
Piscataway, NJ
David
E.
Fowler
IBM Almaden Research Center
San Jose,
CA
S.
M.
Gaspar
University
of

New Mexico
Albuquerque,NM
ROY
H.
Geiss
IBM Almaden Research Center
San Jose,
CA
Torgny Gustafsson
Rutgers University
Piscataway, NJ
William
L.
Harrington
Evans
Fast
Plainsboro, NJ
Brent
D.
Hermsmeier
IBM Almaden Research Center
San Jose,
CA
K.C. Hidunan
University
of
New Mexico
Albuquerque, NM
Tim
Z.

Hossain
Cornell University
Ithica,
NY
Rebecca
S.
Howland
Park Scientific Instruments
Sunnyvale,
CA
John
C.
Huneke
Charles
Evans
&
Assodates
Redwood City,
CA
Ting C. Huang
IBM Almaden Research Center
San
Jose,
CA
William
Katz
Evans Central
Minnetonka, MN
Michael
D.

Kirk
Park Scientific Instruments
Sunnyvale,
CA
Solid State Nuclear Magnetic Resonance
Total
Reflection X-Ray Fluorescence
Medium-Energy Ion Scattering with
Channeling and Blocking
Magneto-optic
Kerr
Rotation
Optical Scatterometry
Energy-Dispersive X-Ray Spectroscopy
Medium-Energy Ion Scattefmg With
Channeling and Blocking
Spark
Source
Mass Spectromeuy
X-Ray Photoelectron and Auger
Electron Diffraction
Optical Scatterometry
Neutron Activation Analysis
Scanning Tunneling Microscopy
and
Scanning Force Microscorn
Sputtered Neutral
Mass
Spectrometry,
Glow-Discharge Mass Spectrometry

X-Ray Fluorescence
Static Secondary
Ion
Mass
Spectrometry
Scanning Tunneling Microscopy
and Scanning Force Microscopy
Contributors
xvii
Bruce E. Koel
University
of
Southern California
Los
Angles,
CA
Max G. Lagally
University
of
Wmnsin,
Madison,
WI
W.
A.
Lanford
State University
of
New York,
Albany,
NY

Charles E. Lyman
Lehigh University
Bethlehem, PA
Susan
MacKay
Perkin Elmer
Eden Prairie, MN
John
R
McNeil
University
of
New Mexico
Albuquerque, NM
Ronald G. Musket
Lawrence Livermore National Laboratory
Livermore,
(=A
S.
S.
H.
Naqvi
Universiy
of
New
Mexico
Albuquerque, NM
Dale E. Newbury
National Institutes
of

Science and Technology
Gairhersburg, MD
David Norman
SERC Daresbury Laboratory
Daresbury, Cheshire
John
W.
Olesik
Ohio State University
Columbus,
OH
Fred
H.
Pollak
Brooklyn
College, CUNY
New York,
NY
Thomas P. Russell
IBM Alden
Research Center
San Jose,
CA
Donald E. Savage
University
of
Wisconsin
Madison,
WI
Kurt

E. Si&
Los
Alamos
National Laboratory
LosAlamos,NM
Paul
G.
Snyder
University
of
Nebraska
Lincoln, NE
High-Resolution
Electron
Energy
Loss
Spectrometry
Low-Energy Electron Diffraction
Nudear Reaction Analysis
Scanning Transmission Electron Microscopy
Surface
Analysis by Laser Ionization
Optical Scatterometry
Partide-Induced X-Ray Emission
Optical Scatterometry
Electron Probe X-Ray Microanalysis
Surface
Extended X-Ray Absorption
Fine Structure, Near
Edge

X-Ray
Absorption Fine Structure
Inductively Coupled Plasma-Optical
Emission Spectroscopy
Modulation
spectroscopy
Neutron Reflectivity
Reflection High-Energy Electron Diffraction
Transmission Elmn Microscopy
Variable Angle Spectroscopic Ellipsometry
xviii Contributors
Gene Sparrow
Advanced R&D
St. Paul, MN
Fred
A.
Stevie
AT&T Bell Laboratories
Allentown, PA
Yale
E.
Strausser
Surface Science Laboratories
Mountainview,
CA
Barry J. Streusand
Applied Analytical
Austin,
TX
Raymond

G.
Teller
BP Research International
Cleveland,
OH
Michael F. Toney
IBM Almaden Research Center
San Jose,
CA
Wojciech Viech
Charles Evans
&
Assoociates
Redwood City,
CA
William B. White
Pennsylvania Skate UniVeI'Siq'
University Park, PA
S.R
Wilson
University of New Mexico
Albuquerque, NM
John A. Woollam
University of Nebraska
Lincoln, NE
Ben
G.
Yacobi
University of California at
Los

Angeles
Los
Angeles,
CA
David
J.
C. Yates
Consultant
Poway,
CA
Nestor
J.
Zaluzec
Argonne National Laboratory
Argonne, IL
Ion Scattering Spectroscopy
Surface Roughness: Measurement,
Formation by Sputtering, Impact on
Depth Profiling
Auger Electron Spectroscopy
Inductively Coupled Plasma Mass Spectrometry
Neutron Diffraction
X-Ray Diffraction
Glow-Discharge
Mass
Spectrometry
Raman Spectroscopy
Optical Scatterometry
Variable Angle Spectroscopic Ellipsometry
Cathodoluminescence

Physical and Chemical Adsorption for the
Measurement
of
Solid
Surface
Areas
Electron Energy-Loss Spectroscopy in the
Transmission Electron Microscope
Contributors
xix

I
INTRODUCTION AND
SUMMARIES
1.0
INTRODUCTION
Though a wide range of analytical techniques is covered in this volume there are
certain traits common to many of them. Most involve either electrons, photons,
or
ions
as
a
probe beam striking the material to be analyzed. The
beam
interacts
with
the material in some way, and in some of the
techniques
the
changes

induced
in
the
beam (energy, intensity, and angular distribution) are monitored after the inter-
action, and analytical information
is
derived from the observation of these
changes. In other techniques the information used for analysis comes from
elec-
trons, photons,
or
ions that are ejected from the sample under the stimulation of
the probe beam. In many situations several connected processes may be going on
more
or
less simultaneously, with a particular analytical technique picking out
only one aspect, e.g., the extent of absorption of incident light,
or
the kinetic
energy distribution of ejected electrons.
The range of information
provided
by the techniques
discussed
here
is
as0
wide,
but again there are common themes. What types of information are provided by
these techniques? Elemental composition is perhaps the most basic information,

followed by chemical state information, phase identification,
and
the determina-
tion
of
structure (atomic sites, bond lengths,
and
angles).
One
might
need
to
know
how
these
vary
as
a function of depth into the material,
or
spatially
across
the mate-
rial, and many techniques specialize
in
addressing these questions down to very fine
dimensions.
For
su&s,
interfaces, and thin films there is ofien very little
material

at
all
to
analyze,
hence
the presence of many microanalytical methods in this
vol-
ume. Within
this
field
(microanalysis) it
is
ob
necessary
to
identify trace
compo-
nents down
to
extremely low concentration (parts per trillion in some cases) and a
number of techniques specialize in this aspect. In other cases a high degree of accu-
racy
in measuring the presence of major components might be the issue. Usually
the techniques that are
good
fbr
trace
identification are not the same ones
used
to

accurately quantify
major
components. Most complete
analyses
require the use of
1
multiple techniques, the selection of which depends on the nature of the sample
and the desired information.
This
first
chapter contains onepage summaries of each of the
50
techniques cov-
ered in the following chapters.
All
summaries have the same format
to
allow easy
comparison and quick access to the information. Further comparative information
is
provided in the introductions to the chapters. Finally,
a
table is provided
at
the
end
of
this introduction, in which many
of
the important parameters describing the

capabilities
for
all
50
techniques are listed.
The subtitle of this Series
is
“Su&m, Interfices, and
Thin
Films.”
The
defi-
nition of a “surface”
or
of
a
“thin
film” varies considerably hm person
to
person
and with application
area.
The academic discipline of ‘‘Surfice Science”
is
largely concerned with chemistry and physics at the atomic monolayer level,
whereas the “surface
region”
in an engineering
or
applications sense

can
be much
more extensive. The same is true for interfaces between materials. The practical
consideration in distinguishing “sudace” from “bulk” or “thin” from “thick” is
usually connected to the property of interest in the application. Thus,
fbr
a cata-
lytic reaction the presence of
haf
a monolayer
of
extraneous
sulfur
atoms in the
top atomic layer of the catalyst material might be critical, whereas for
a
corro-
sion protection layer (for example,
Cr
segregation
to
the
surface region in steels)
the important region
of
depth may be several hundred
8,.
For interfaces the epi-
taxial relationship between he last atomic layer of
a

single crystal material and
the first layer of the adjoining material may be critical for the electrical proper-
ties of a device, whereas diffusion barrier interfaces elsewhere in the same device
may be
1000
A
thick. In thin-film technology requirements
can
range from layers
pm
thick, which
for
the majority
of
analytical techniques discussed
in
this volume
constitute bulk material, to layers
as
thin
as
50
8,
or
so
in thin-film magnetic
recording technology. Because of these different perceptions of “thick” and
“thin,” actual numbers are used whenever discussing the depth an analytical tech-
nique examines. Thus in Ion Scattering Spectroscopy the signals used in the anal-
ysis are generated fiom only the top atomic monolayer of material exposed

to
a
vacuum, whereas in X-ray photoemission up
to
100
8,
is probed, and in X-ray
flu-
orescence the signal can come from integrated depths ranging up to
10
pm.
Note
that in these three examples,
two
are
quoted
as
having
ranges
of
depths.
For
many
of
the techniques
it
is
impossible
to
assign

unique values because the depth from
which
a
signal
originates may depend both
on
the particular manner in which the
technique is
used,
and on the nature
of
the material being
examined.
Perfbrming
measurements at grazing
angles
of
incidence
of
the probe
beain,
or
grazing
exit
angles
fbr
the
detected
signal,
will

usually
make
the technique more
surface
sensi-
tive.
For
techniques where X-ray, electron,
or
high-energy ion scattering
is
the
critical
Factor
in determining the depth
analyzed,
materials consisting
of
light
elements are
always
probed more deeply
than
materials consisting of heavy ele-
ments.
2
INTRODUCTION AND SUMMARIES
Chapter
1