vickerman - surface analysis the principal techniques
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S urface A n alys is
The Pr incipal
Techniques
2nd Edition
Editors
JOHNC.VICKERMAN
Man chester Interdisciplinary
Biocentre
niv rsityof
Manchester
UK
IA N S . GILMORE
National PhysicalLaboratory
Teddington UK
W I L Y
A John Wiley and Sons, Ltd., Pu blication
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Contents
List of Contribu tors xv
Preface xvi i
1 Intro d uction 1
John
C
Vickerman
1.1
1.2
1.3
1.4
1.5
1.6
How do we Define the Surface?
How Many Atoms in a Surface?
Information Required
Surface Sensitivity
Radiation Effects - Surface Damage
Com plexity of the Data
2 Auger E lectron Spectro sco py
Hans
2.1
2.2
2.3
;
JorgMathieu
Introduction
Principle of the Aug er Process
2.2.1 Kinetic Energies of Auger Peaks
2.2.2 Ionization Cross-Section ;
2.2.3 Comparison of Auger and Photon Emission
2.2.4 Electron Backscattering
2.2.5 Escape Depth
2.2.6 Chemical Shifts
Instrumentation
2.3.1 Electron Sources
2.3.2 Spectrometers
2.3.3 Modes of Acquisition
2.3.4 Detection Limits
2.3.5 Instrument Calibration
1
2
3
5
7
8
9
9
10
11
15
16
17
18
19
21
22
24
24
29
30
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V I ONTENTS
2.4 Quantitative Analysis 31
2.5 Depth Profile Analysis 33
2.5.1 Thin Film Calibration Standard 34
2.5.2 Depth Resolution 36
2.5.3 Sputter Rates 37
2.5.4 Preferential Sputtering 40
2.5.5 X-Correction 41
2.5.6 Chemical Shifts in AES Profiles 42
2.6 Summary 43
References 44
Problems 45
Electron Spectroscopy
for
Chemical nalysis
7
BuddyD .Rattiera nd David
G
Castner
3.1 Overview 47
3.1.1 The Basic ESCA Experiment 48
3.1.2 A History of the Photoelectric Effect and ESCA 48
3.1.3 Information Provided by ESCA 49
3.2 X-ray Interaction with Matter, the Photoelectron Effect
and Photoemission from Solids 50
3.3 Binding Energy and the Chemical Shift 52
3.3.1 Koopmans' Theorem 53
3.3.2 Initial State Effects 53
3.3.3 Final State Effects 57
3.3.4 Binding Energy Referencing 58
3.3.5 Charge Compensation in Insulators 60
3.3.6 Peak Widths 61
3.3.7 Peak Fitting 62
3.4 Inelastic Mean Free Path and Sampling Depth 63
3.5 Quantification 67
3.5.1 Quantification Methods 68
3.5.2 Quantification Standards 70
3.5.3 Quantification Example 71
3.6 Spectral Features 73
3.7 Instrumentation 80
3.7.1 Vacuum Systems for ESCA Experiments 80
3.7.2 X-ray Sources 82
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CONTENTS
3.8
3.9
3.10
3.11
3.12
-- ' 3.13
3.14
3.7.3 Analyzers
3.7.4 Data Systems
3.7.5 Accessories
Spectral Q uality
Depth Profiling
X-Y M apping and Imaging
Chemical Derivatization
Valence Band
Perspectives
Conclusions
Acknowledgements
References
Problems
4 Mo lecular Surface M ass Spectr o metr y by SIMS
JohnC
4.1
4.2
4.3
4.4
>
4.5
4.6
Z. Vickerman
Introduction
Basic Concepts
4.2.1 The Basic Equation
4.2.2 Sputtering
4.2.3 Ionization
4.2.4 The Static Limit and Depth Profiling
4.2.5 Surface Charging
Experimental R equirements
4.3.1 Primary Beam
4.3.2 Mass Analysers
Secondary Ion Formation
4.4.1 Introduction
4.4.2 Models of Sputtering
4.4.3 Ionization
4.4.4 Influence of the Matrix Effect in Organic
Materials A nalysis
M odes of A nalysis
4.5.1 Spectral Analysis
4.5.2 SIMSImaging or Scanning SIMS
4.5.3 Depth Profiling and 3D Imaging
Ionization of the Sputtered Neutrals
VII
84
86
88
88
89
94
96
96
99
100
101
101
109
113
113
116
116
116
121
123
124
125
125
131
140
140
143
149
151
155
155
166
173
183
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VIM
4.7
4.6.1
4.6.2
CONTENTS
Photon Induced Post-Ionization
Photon Post-Ionization and SIMS
Ambient Methods of Desorption Mass Spectrometry
References
Problems
5 Dynamic SIMS
David
McPhail
and Mark Dowsett
5:1
5.2
5.3
5.4
5.5
-
' Fundamentals and Attributes
5.1.1
5.1.2
5.1.3
5.1.4
5.1.5
Areas
5.2.1
5.2.2
5.2.3
5.2.4
Introduction
Variations on a Theme
The Interaction of the Primary Beam
with the Sample
Depth Profiling
Complimentary Techniques and D ata
Comparison
and Methods of Application
Dopant and Impurity Profiling
Profiling High Concentration Species
Use ofSIMSin Near Surface Regions
Applications of
SIMS
Depth Profiling
in M aterials Science
Quantification of Data
5.3.1
5.3.2
5.3.3
5.3.4
Novel
5.4.1
5.4.2
5.4.3
Quantification of Depth Profiles
Fabrication of S tandards
Depth Measurement and Calibration of the
Depth Scale
Sources of Error in Depth Profiles
Approaches
Bevelling and Imaging or Line Scanning
Reverse-Side Depth Profiling
Two-Dimensional Analysis
Instrumentation
5.5.1
5.5.2
5.5.3
5.5.4
Overview
Secondary Ion Optics
Dual Beam M ethods and ToF
Gating
184
190
194
199
203
2 0 7
207
207
211
214
217
224
226
226
227
230
233
233
233
239
241
242
246
246
250
251
252
252
253
254
254
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CONTENTS IX
5.6
Conclusions
References
Problems
6 Low E nergy Ion Scatt er ing and Rutherford Backscatt ering
Edmund
Taglauer
6.1
6.2
6.3
6.4
Introduction
Physical Basis
6.2.1 The Scattering Process
6.2.2 Collision Kinem atics
6.2.3 Interaction Potentials and Cross-sections
6.2.4 Shadow Cone
6.2.5 Computer Simulation
Rutherford Backscattering
6.3.1 Energy Loss
6.3.2 Apparatus
6.3.3 Beam Effects
6.3.4 Quantitative Layer Analysis
6.3.5 Structure Analysis
6.3.6 Medium-Energy Ion Scattering (MEIS)
6.3.7 The Value of RBS and Com parison to Related
Techniques
Low-Energy Ion Scattering
6.4.1 Neutralization
6.4.2 Apparatus
6.4.3 Surface Com position Analysis
6.4.4 Structure Analysis
6.4.5 Conclusions
Acknowledgement
References
Problems
Key Facts
256
257
267
269
269
271
271
272
275
278
281
284
284
287
289
290
293
297
298
300
300
303
307
316
323
324
324
330
330
7 Vib rationa l Spectroscopy from Surfaces
MartynE.Pemble and Peter Gardner
7.1 Intro duction 333
7.2 Infrared Spectroscopy from Surfaces 334
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CONTENTS
7.2.1 Tran sm ission IR Spec troscopy
335
7.2.2 Pho toacou stic Spectrosc opy
340
7.2.3 Reflectance M eth od s
342
7.3 Elec tron En erg y Loss Sp ectro sco py (EELS) 361
7.3.1 Inelastic
or
'Imp act ' Scattering
362
7.3.2 Elasticor 'Dipole' Scattering 365
7.3.3 Th e EELS (HREELS) Ex pe rim en t 367
7.4 TheG r o u p T h e o r yofSurface V ibrat ions 368
7*.4.1
General Approach
368
7.4.2 G rou p Theory AnalysisofEthyne Ad sorbedat a
Flat, Featureless Surface
369
7.4.3 G rou p Theo ry AnalysisofEthyne A dsorbedat a
(100) Surface
of an
FCC Metal
373
7.4.4 The Expected Formof the RAIRSand Dipolar
EELS (HREELS) Sp ectra 374
7.5 Laser Ra m an Spec troscopy from Surfaces 375
7.5.1 TheoryofRa ma n Scattering 376
7.5.2 The Stu dyofCollective Surface Vib rations
(Phonons) using Raman Spectroscopy 377
7.5.3 Ra m an Spectrosc opy from M etal Surfaces 379
7.5.4 Sp atial Re solu tion
in
Surface Ra m an
Spectroscopy 380
7.5.5 Fou rier Transfo rm Surface Ra m an Tec hniq ues 380
7.6 Inelast ic N eu tro n Scat ter ing (INS) 381
7.6.1 IntroductiontoIN S 381
7.6.2 The INS Sp ectru m
382
7.6.3 INS Spe ctraofHydrodesesulfurizat ion Catalysts 382
7 7
Sum-Frequency Generation Methods 383
References 386
Problems 389
8 Su r face S tructure Determinat ion
by
In te r fe r e n c e T e c h n iq u e s
39
hristopher
A . Lucas
8.1 Int roduct ion
391
8.1.1 Basic Th eo ryofD iffraction - Three Dimensions 392
8.1.2 ExtensiontoSurfaces- Two Dimensions 398
8.2 Elec tron Diffraction Te ch niq ue s 402
8.2.1 Ge nera l Intro du ction 402
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CONTENTS XI
8.2.2 Lo w En erg y Electro n Diffraction 403
8.2.3 Reflection H ig h En erg y Elec tron Diffraction
(RHEED) 418
8.3 X-ray Tec hn ique s 424
8.3.1 Ge nera l Intro du ction 424
8.3.2 X-ray A ds orp tion Spec troscopy 427
8.3.3 Surface X-ray Diffraction (SXRD) 447
8.3.4 X-ray Sta nd ing W ave s (XSWs) 456
-... -
8.4 Ph oto ele ctro n Diffraction 464
8.4.1 Intro du ctio n 464
8.4.2 Theo retical Co nsid eratio ns 465
8.4.3 Ex perim ental Details 469
8.4.4 Ap plicatio ns of XPD an d Ph D 470
References 474
9 Scanning Probe Microscopy 479
Graham
J Leggett
9.1 Intr od uc t ion 479
9.2 Scann ing Tun nel l ing M icroscopy 480
9.2.1 Basic Prin cip les of the STM 481
9.2.2 Instrum entatio n and Basic Op eration Param eters 487
9.2.3 Atom ic Reso lution an d Spectrosco py: Surface
Crystal an d Electronic Struc ture 489
9.3 Ato m ic Force M icrosco py 511
9.3.1 Basic Prin ciple s of the AFM 511
9.3.2 Ch em ical Force M icroscopy 524
9.3.3 Friction Force M icros cop y 526
9.3.4 Biological A pp lica tion s of the AFM 532
9.4 Sca nnin g Ne ar-Field Op tical M icrosco py 537
9.4.1 Op tical Fibre Ne ar-Field M icroscopy 537
9.4.2 Ap ertu reless SNO M 541
9.5 O ther Scanning Probe M icroscopy Techn iques 542
9.6 L i thog raphy Us ing P robe Mic roscopy M ethod s 544
9.6.1 STM Lith og rap hy 544
9.6.2 AFM Lith og rap hy 545
9.6.3 Nea r-Field Ph oto litho gra ph y 549
9.6.4 The 'M illipe de ' 550
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XII CONTENTS
9.7 Co nclusio ns 551
References 552
Problems 559
10 T h e A p p l ic a t io n of Mu l t iv a r i a t e D a ta A n a l y s i s T e c h n i q u e s in
S u r fa c e A n a l y s i s 5 63
Joanna
L.S.
Lee and
Ian S. Gilmore
10.1 Int ro duc t ion 563
10.2 Basic C on ce pt s 565
10.2.1 M atrix an d Vector R epr ese nta tion of Data 565
10.2.2 Dim ens iona lity an d Ra nk 567
10.2.3 Relation to M ultiv aria te An alysis 568
10.2.4 Ch oosing the A pp rop riate M ultivariate M ethod 568
10.3 Facto r A na lys is for Iden tification 569
10.3.1 Term inolo gy 570
10.3.2 M athe m atical Ba ckg roun d 570
10.3.3 Principal C om po ne nt An alysis 571
10.3.4 M ultiva riate C ur ve Re solu tion 579
10.3.5 An alysis of M ultiv ariate Im age s 582
10.4 Re gress ion M eth od s for Qu antif icat ion 591
10.4.1 Term inolog y 591
10.4.2 M athe m atical Ba ckg roun d 592
10.4.3 Principal C om po ne nt Regression 594
10.4.4 Partial Least Sq uare s Reg ression 595
10.4.5 Calibration, Validation an d Pred iction 596
10.4.6 Exam ple - Co rrelating ToF -SIM S Spectra w ith
Polym er W ettability Using PLS 598
10.5 M et h o d s for Classification 600
10.5.1 D iscrim inan t Fu nction An alysis 601
10.5.2 H ierarc hal Clu ster An alysis 602
10.5.3 Artificial N eu ra l N etw or ks 603
10.6 Su m m ary an d Co nclusion 606
A c know l e dge me n t s 608
References 608
Problems 611
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CONTENTS XIII
Ap pen dix 1 VacuumTec hn ology forAp p l ied Sur face Sc ience
6 3
Rod W ilson
Al.l Introduction: Gases and Vapours 613
A1.2 The Pressure Regions of Vacuum Technology and
their Characteristics 619
A1.3 Production of a Vacuum 622
Al.3.1 Types of Pump 622
Al.3.2 Evacuation of a Chamber 634
* - ' Al.3.3 Choice of Pumping System 635
Al.3.4 Determination of the Size of Backing Pumps 636
Al.3.5 Flanges and their Seals 636
A1.4 Measurement of Low Pressures 637
Al.4.1 Gauges for Direct Pressure Measurement 638
Al.4.2 Gauges Using Indirect Means of Pressure
Measurement 640
Al.4.3 Partial Pressure Measuring Instruments 644
Acknowledgement 647
References 647
A p p e n d i x
2
Un i ts Fundame nta l Ph ys ica l Constants
and
Conversions 649
A2.1 Base Units of the SI 649
A2.2 Fundamental Physical Constants 650
A2.3 Other Units and Conversions to SI 651
References 652
Index 653
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