Surface Analysis Methods in Materials Science

by O'Connor, D. J.; Sexton, B. A.; Smart, R. St. C.

Edition: 2nd

ISBN13: 9783540413301

ISBN10: 3540413308

Format: Hardcover

Pub. Date: 2003-06-01

Publisher(s): Springer Verlag

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Summary

This guide to the use of surface analysis techniques, now in its second edition, has expanded to include more techniques, current applications and updated references. It outlines the application of surface analysis techniques to a broad range of studies in materials science and engineering. The book consists of three parts: an extensive introduction, a techniques section and a section on applications. Each chapter has been written by specialists in the field. This book is aimed at industrial scientists and engineers in R&D seeking a description of available techniques in a concise but informative style. It is invaluable as a comprehensive text for scientists and engineers attending training courses and workshops. The level and content of this book make it ideal as a course text for senior undergraduate and postgraduate students in materials science, materials engineering, physics, chemistry and metallurgy.

Part I Introduction

1 Solid Surfaces, Their Structure and Composition

C. Klauber, R. St. C. Smart

(4)

1.1 Importance of the Surface

(4)

1.2 Solid Surfaces of Different Materials

(5)

1.2.1 A Material Under Attack: Aluminium

(1)

1.3 Methods of Surface Analysis

(1)

1.3.1 Variety of Surface Analytical Techniques

(1)

1.4 Structural Imaging

(10)

1.4.1 Direct Physical Imaging

(15)

1.4.2 Indirect Structural Imaging - Relaxation and Reconstruction

1.5 Composition of the Surface Selvedge

(19)

1.5.1 Electron Inelastic Meun Free Paths

(4)

1.5.2 Variation of Elemental Sensitivities

(3)

1.5.3 Practical Detection Limits

(1)

1.5.4 Practical Bpatial Lömite

(5)

1.5.5 Chemical State Information

(4)

1.5.6 Laboratory Standards

(1)

1.5.7 Inter-laboratory Errors

(1)

1.6 Defect and Reaction Sites at Surfaces

(4)

1.7 Electronic Structure at Surfaces

(3)

1.8 Structures of Adsorbed Layers

(2)

1.9 Structure in Depth Profiles Through Surfaces

(4)

1.10 Specific Structures

(6)

1.10.1 Grain Structures, Phase Distributions and Inclusions

(1)

1.10.2 Fracture Faces and Intergranular Regions

(2)

1.10.3 Pore Structures

(3)

1.10.4 Precipitates, Reaction Products and Recrystallised Particles on Surfaces

(1)

1.10.5 Magnetic Domains

(1)

1.11 Technique-Induced Artifacts

(4)

1.11.1 Radiation Damage 6l

1.11.2 Electrostatic Charging

(1)

References

2 UHV Basics

C. Klauber

(78)

2.1 The Need for Ultrahigh Vacuum

(3)

2.2 Achieving UHV

(2)

2.3 Specimen Handling

(2)

2.4 Specimen Handling: ASTM Standards

(3)

References

(4)

PART II Techniques

3 Electron Microscope Techniques for Surface Characterization

P.S.Turner, C.E. Nockolds, S. Bullock

(22)

3.1 What Do We Need to Know About Surface Structures?

(1)

3.2 Electron Optical Imaging Systems

(4)

3.2.1 Electron Sources

(1)

3.2.2 Electron Lenses

3.2.3 Detection Systems

(1)

3.3 Scanning Electron Microscopy of Surfaces

(8)

3.3.1 The SEM

(1)

3.3.2 The Signals and Detectors

(1)

3.3.3 Resolution and Contrast in SEM Images

(4)

3.3.4 Variable Pressure SEM and Envrionmental SEM

(1)

3.3.5 Energy Dispersive X-Ray Spectrometry

(1)

3.4 Transmission Electron Microscopy of Surfaces

(4)

3.4.1 The Transmission Electron Microscope

(2)

3.4.2 Electron Diffraction

101

(1)

3.4.3 Image Contrast and Resolution in the TEM

101

(1)

3.4.4 Imaging Surface Structures in the TEM

102

(1)

3.4.5 Reflection Electron Microscopy

103

(1)

3.5 Other Developments

103

(1)

References

104

(3)

4 Sputter Depth Profiling

B.V. King

107

(20)

4.1 Analysis of a Sputter Depth Profile

108

(7)

4.1.1 Calibration of the Depth Scale

108

(4)

4.1.2 Calibration of the Concentration Scale

112

(3)

4.2 The Depth Resolution of Sputter Profiling

115

(8)

4.2.1 Specification of the Depth Resolution

115

(2)

4.2.2 Instrumental Factors Determining the Depth Resolution

117

(2)

4.2.3 Surface Effects Determining the Depth Resolution

119

(1)

4.2.4 Bulk Effects Affecting the Depth Resolution

120

(1)

4.2.5 Minimisation of the Depth Resolution

121

(2)

4.3 Conclusion

123

(1)

References

123

(4)

5 SIMS - Secondary Ion Mass Spectrometry

R.J. MacDonald, B.V. King

127

(28)

5.1 The Practice of SIMS

128

(10)

5.1.1 Overview

128

(2)

5.1.2 Advantages and Disadvantages of SIMS

130

(1)

5.1.3 The Yield of Secondary Ions

131

(7)

5.2 Construction of a Secondary Ion Mass Spectrometer

138

(7)

5.3 Topics in SIMS Analysis

145

(5)

5.3.1 Signal Enhancement by Surface Adsorption

145

(2)

5.3.2 Using Secondary Ion Energies in SIMS Analysis

147

(2)

5.3.3 The Relative Sensitivity Factor

149

(1)

5.4 Static SIMS Analysis

150

(3)

References

153

(2)

6 Auger Electron Spectroscopy and Microscopy - Techniques and Applications

P.C. Dastoor

155

(20)

6.l Introduction

155

(1)

6.2 Fundamentals

155

(3)

6.3 Instrumentation

158

(1)

6.4 Quantification

159

(1)

6.5 Techniques

160

(9)

6.5.1 Spot Analysis Mode

161

(1)

6.5.2 Line Scan Mode

162

(1)

6.5.3 Scanning Mode

163

(1)

6.5.4 Scanning Auger Microscopy

164

(3)

6.5.5 Depth Profiling Mode

167

(1)

6.5.6 Preferential Sputtering

167

(1)

6.5.7 Attenuation Length

168

(1)

6.5.8 Chemical Effects

168

(1)

6.6 Applications

169

(2)

6.6.1 Thin Film Analysis

169

(1)

6.6.2 Surface Diffusion and Segregation

170

(1)

6.7 Future

171

(1)

References

171

(4)

7 X-Ray Photoelectron Spectroscopy

M.H. Kibel

175

(28)

7.1 Basic Principles

175

(4)

7.1.1 Theory

175

(1)

7.1.2 Typical Spectrum

176

(2)

7.1.3 Surface Specificity

178

(1)

7.2 Instrumentation

179

(5)

7.2.1 Essential Components

179

(3)

7.2.2 Optional Components

182

(1)

7.2.3 Synchrotron Radiation

183

(1)

7.2.4 Imaging XPS

183

(1)

7.3 Spectral Information

184

(5)

7.3.1 Spin-Orbit Splitting

184

(1)

7.3.2 Chemical Shifts

185

(1)

7.3.3 Auger Chemical Shifts in XPS

186

(1)

7.3.4 X-Ray Line Satellites

187

(1)

7.3.5 "Shake-up" Lines

187

(1)

7.3.6 Ghost Lines

188

(1)

7.3.7 Plasmon Loss Lines

189

(1)

7.4 Quantitative Analysis

189

(2)

7.5 Experimental Techniques

191

(4)

7.5.1 Variation of X-Ray Sources

191

(1)

7.5.2 Depth Profiles

191

(3)

7.5.3 Angular Variations

194

(1)

7.5.4 Sample Charging

194

(1)

7.6 Comparison with Other Techniques

195

(2)

7.7 Applications

197

(1)

7.8 Conclusion

197

(1)

References

198

(5)

8 Vibrational Spectroscopy of Surfaces

R.L. Frost, N.K. Roberts

203

(26)

8.1 Introduction

203

(3)

8.2 Surface Techniques

206

(15)

8.2.1 Diffuse Reflectance Infrared Fourier Transform (DRIFT)

207

(2)

8.2.2 Attenuated Total Reflectance Spectroscopy (ATR)

209

(7)

8.2.3 Photoacoustic Spectroscopy (PAS)

216

(3)

8.2.4 Infrared Emission Spectroscopy (IES)

219

(2)

8.3 Fourier transform Raman spectroscopy

221

(3)

8.4 Raman Microscopy

224

(3)

References

227

(2)

9 Rutherford Backscattering Spectrometry end Nuclear Reaction Analysis

S.H. Sie

229

(18)

9.1 Introduction

229

(2)

9.2 Principles

231

(3)

9.2.1 Stopping Power

232

(1)

9.2.2 Straggling

233

(1)

9.3 Rutherford Backscattering Spectrometry

234

(6)

9.3.1 Experimental Considerations

236

(1)

9.3.2 Examples

236

(2)

9.3.3 Special Cases

238

(2)

9.4 Nuclear Reaction Analysis

240

(5)

9.4.1 Formalism

241

(1)

9.4.2 Experimental Considerations

242

(1)

9.4.3 Examples

243

(2)

9.5 Summary

245

(1)

References

246

(1)

10 Materials Characterization by Scanned Probe Analysis

S. Myhra

247

(40)

10.1 Introduction

247

(4)

10.2 The Surface Analytical Context

251

(1)

10.3 Generic SPM Systems

251

(2)

10.4 Physical Principles

253

(9)

10.4.1 STM/STS

253

(3)

10.4.2 Scanning Force Microscopy (SFM)

256

(1)

10.4.3 Intermittent Contact Mode

257

(1)

10.4.4 F d Analysis

258

(2)

10.4.5 Lateral Force Microscopy (LFM)

260

(2)

10.5 Procedures for 'Best Practice'

262

(5)

10.5.1 Spatial Characteristics of Scanners

263

(1)

10.5.2 Determination of cN and cT

264

(1)

10.5.3 Determination of Spring Constants

265

(1)

10.5.4 Determination of Actual Tip Parameters in the Mesoscopic Regime

266

(1)

10.6 Illustrative Case Studies

267

(16)

10.6.1 Surface and Defect Structures of WTe2 Investigated by UHV-STM

267

(2)

10.6.2 Organic Thin Film and Surface Mechanical Characterization

269

(4)

10.6.3 AFM Analysis of 'Soft' Biological Materials

273

(5)

10.6.4 Nanotribology of Solid Lubricants

278

(5)

References

283

(4)

11 Low Energy Ion Scattering

D.J. O'Connor

287

(20)

11.1 Qualitative Surface Analysis

287

(2)

11.2 Advantage of Recoil Detection

289

(2)

11.3 Quantitative Analysis

291

(8)

11.3.1 Scattered Ion Yield

291

(1)

11.3.2 Differential Scattering Cross Section

291

(1)

11.3.3 Charge Exchange

292

(3)

11.3.4 Relative Measurements

295

(2)

11.3.5 Standards

297

(2)

11.4 Surface Structural Analysis

299

(3)

11.4.1 Multiple Scattering

299

(1)

11.4.2 Impact Collision Ion Surface Scattering (ICISS)

300

(2)

11.5 Experimental Apparatus

302

(2)

References

304

(3)

12 Reflection High Energy Electron Diffraction

G.L. Price

307

(12)

12.1 Theory

309

(3)

12.2 Applications

312

(6)

References

318

(1)

13 Low Energy Electron Diffraction

P.J. Jennings, C.Q. Sun

319

(18)

13.1 The Development of LEED

319

(1)

13.2 The LEED Experiment

320

(4)

13.2.1 Sample Preparation

323

(1)

13.2.2 Data Collection

323

(1)

13.3 Diffraction from a Surface

324

(2)

13.3.1 Bragg Peaks in LEED Spectra

325

(1)

13.4 LEED Intensity Analysis

326

(2)

13.5 LEED Fine Structure

328

(1)

13.6 Applications of LEED

329

(4)

13.6.1 Determination of the Symmetry and Size of the Unit Mesh

329

(1)

13.6.2 Unit Meshes for Chemisorbed Systems

330

(1)

13.6.3 LEED Intensity Analysis

330

(2)

13.6.4 Surface Barrier Analysis

332

(1)

13.7 Conclusion

333

(1)

References

334

(3)

14 Ultraviolet Photoelectron Spectroscopy of Solids

R. Leckey

337

(10)

14.1 Experimental Considerations

339

(1)

14.2 Angle Resolved UPS

340

(4)

14.3 Fermi Surface Studies

344

(1)

References

345

(2)

15 EXAFS

R.F. Garrett, G.J. Foran

347

(30)

15.1 Introduction

347

(1)

15.2 Experimental Details

348

(11)

15.2.1 Synchrotron Radiation

350

(2)

15.2.2 Synchrotron Beamlines for EXAFS

352

(2)

15.2.3 Detectors

354

(1)

15.2.4 The Sample

355

(2)

15.2.5 Acquiring EXAFS Data

357

(2)

15.3 Theory of X-ray Absorption

359

(3)

15.3.1 EXAFS

359

(2)

15.3.2 XANES

361

(1)

15.4 EXAFS Analysis

362

(4)

15.4.1 Data Reduction

362

(1)

15.4.2 Conversion to k-space

363

(1)

15.4.3 Background Subtraction

363

(1)

15.4.4 Fourier Transformation

364

(1)

15.4.5 Fourier Filtering and Back Transformation

364

(1)

15.4.6 Modelling and Least Squares Fitting to the EXAFS Equation

365

(1)

15.5 Case Studies

366

(11)

15.5.1 Surface EXAFS of Titanium Nanostructure Thin Films

366

(4)

15.5.2 Ion-Implantation Induced Amorphisation of Germanium

370

(1)

References

371

(6)

Part III Processes and Applications

16 Minerals, Ceramics and Glasses

R.St.C. Smart

377

(28)

16.1 Minerals

380

(9)

16.1.1 Iron Oxides in Mineral Mixtures

380

(1)

16.1.2 Surface Layers on Minerals

381

(1)

16.1.3 Mineral Processing of Sulfide Ores

381

(5)

16.1.4 Adsorption and Reaction of Oxide and Clay Minerals

386

(1)

16.1.5 Surface Modification of Minerals

387

(2)

16.2 Ceramics

389

(6)

16.2.1 Leaching and Dissolution

390

(2)

16.2.2 Ceramic Surface Layers: Bioceramics

392

(3)

16.3 Glasses

395

(10)

16.3.1 Leached and Recrystallised surfaces

395

(3)

16.3.2 Surface Modification of Glass Surfaces

398

(2)

References

400

(5)

17 Characterization of Catalysts by Surface Analysis

N.K. Singh, B.G. Baker

405

(30)

17.1 Examples of Catalytic Systems Studied by XPS

408

(12)

17.1.1 Alumina

408

(1)

17.1.2 Tungsten Oxide Catalysts

409

(3)

17.1.3 Palladium on Magnesia

412

(2)

17.1.4 Cobalt on Kieselguhr Catalysts

414

(2)

17.1.5 Iron Catalysts

416

(4)

17.2 Examples of Catalytic Systems Studied by FT-Infrared Spectroscopy

420

(12)

17.2.1 ZSM-5 Zeolites

420

(6)

17.2.2 Thin Alumina Films

426

(2)

17.2.3 Rhodium Supported Alumina Films

428

(1)

17.2.4 Copper Supported Silica Films

429

(3)

17.3 Conclusion

432

(1)

References

432

(3)

18 Application to Semiconductor Devices

P.W. Leech, P. Ressel

435

(20)

18.1 Micro and Nano-Analysis of Integrated Circuits

436

(7)

18.2 Analytical Techniques in the Characterisation of Ohmic Metal/Semiconductor Contacts

443

(9)

18.3 Summary

452

(1)

References

452

(3)

19 Characterisation of Oxidised Surfaces

J.L. Cocking, G.R. Johnston

455

(18)

19.1 The Oxidation Problem

456

(1)

19.2 Oxidation of Co-22Cr-11A1

457

(7)

19.2.1 Chemical Characterisation

458

(1)

19.2.2 Scanning Auger Microscopy

458

(1)

19.2.3 Rutherford Backscattering Analysis

459

(5)

19.3 Oxidation of Ni-18Cr-6A1 0.5Y

464

(9)

19.3.1 Extended X-Ray Absorption Fine Structure

466

(5)

References

471

(2)

20 Coated Steel

R.Payling

473

(16)

20.1 Applications

474

(12)

20.1.1 Grain Boundaries in Steel

474

(1)

20.1.2 Steel Surface

475

(3)

20.1.3 Alloy Region

478

(1)

20.1.4 Metallic Coatings

478

(5)

20.1.5 Treated Metallic Coating Surface

483

(1)

20.1.6 Metal Polymer Interface

483

(1)

20.1.7 Polymer Surface

484

(2)

20.2 Conclusion

486

(1)

References

486

(3)

21 Thin Film Analysis

G.C. Morris

489

(16)

21.1 Thin Film Photovoltaics

490

(2)

21.1.1 Use for Solar Electricity

490

(1)

21.1.2 The Thin Film Solar Cell: Glass/ITO/mCdS/pCdTe/Au

491

(1)

21.2 Film Purity

492

(4)

21.2.1 Low Level Impurities Qualitative

492

(2)

21.2.2 Low Level Impurities Quantitative

494

(1)

21.2.3 Doping Profiles in Thin Films

495

(1)

21.3 Composition and Thickness of Layered Films

496

(5)

21.3.1 Composition Gradation in Films, e.g. CdxHg1-xTe Films on Platinum

496

(1)

21.3.2 Thin Overlayers on Films

497

(4)

21.4 Beam Effects in Thin Film Analysis

501

(1)

21.5 Conclusion

502

(3)

22 Identification of Adsorbed Species

B.G. Baker

505

(14)

22.1 Examples of Adsorption Studies

505

(13)

22.1.1 Nitric Oxide Adsorption on Metals

505

(6)

22.1.2 Aurocyanide Adsorption on Carbon

511

(3)

22.1.3 Adsorbed Methoxy on Copper and Platinum

514

(4)

22.2 Conclusion

518

(1)

References

518

(1)

23 Surface Analysis of Polymers

H.A.W. StJohn, T.R. Gengenbach, P.G. Hartley, H.J. Griesser

519

(34)

23.1 Specific Properties of Polymers

520

(5)

23.2 Surface Contamination and Additives

525

(4)

23.3 Contact Angle Measurements

529

(1)

23.4 X-Ray Photoelectron Spectroscopy (XPS)

529

(8)

23.4.1 General Aspects

529

(2)

23.4.2 Angle-Resolved XPS

531

(1)

23.4.3 Inelastic Mean Free Path in Polymers

532

(1)

23.4.4 Cold Stage XPS

533

(1)

23.4.5 Derivatization of Chemical Groups

534

(3)

23.5 Secondary Ion Mass Spectrometry (SIMS)

537

(3)

23.6 Scanning Probe Microscopy Methods: Scanning Tunneling Microscopy (STM) and Atomic Force Microscopy (AFM)

540

(3)

23.7 Specimen Damage

543

(4)

23.8 Charge Correction

547

(1)

23.9 Grazing Angle Infrared Spectroscopy

548

(1)

References

549

(4)

24 Glow Discharge Optical Emission Spectrometry

T. Neus, R. Payling

553

(3)

24.1 Instrument

553

(2)

24.2 Theory

555

(1)

24.3 Applications

556

(1)

24.3.1 Near Surface

556

(1)

24.3.2 Coatings

556

(1)

24.3.3 Semiconductor Processing

557

(2)

References

559

Part IV Appendix

Acronyms Used in Surface and Thin Film Analysis

563

(6)

Surface Science Bibliography

569

(8)

Index

577

Surface Analysis Methods in Materials Science

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