Glow Discharge Optical Emission Spectrometry

, by Payling, Richard; Jones, Delwyn; Bengtson, Arne

Note: Supplemental materials are not guaranteed with Rental or Used book purchases.

ISBN: 9780471966838 | 0471966835
Cover: Hardcover
Copyright: 12/8/1997

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Glow Discharge Optical Emission Spectrometry (GD-OES) is rapidly becoming one of the most important techniques for the direct analysis of solids. This, the first book entirely devoted to the subject, represents the combined contributions of over 30 specialists from around the world. All contributors are active in the field and recognised internationally for their expertise and knowledge in GD-OES. The book begins with an introductory overview of the subjects, deals with the design of the instrument, its operation and analytical methods and describes in detail the complex plasma processes which occur inside the glow discharge source. The second part of the book is more practically orientated, showing the full range of uses for GD-OES from the bulk analysis of virtually any solid material to depth profiling within the first tens of micrometres of a variety of surfaces and coatings. Glow Discharge Optical Emission Spectrometry is intended for a wide audience of scientists, engineers and postgraduate students and will be a valuable and challenging reference work for both experienced users of the technique and newcomers alike.

List of Contributors

xix

(4)

Biographies of Contributors

xxiii

(8)

Preface

xxxi

(4)

R. Payling

D. G. Jones

A. Bengtson

Acknowledgements

xxxv

(2)

Abbreviations

xxxvii

(2)

Nomenclature

xxxix

1. Introduction

(48)

1.1 Background

(9)

A. Bengtson

D.G. Jones

R. Payling

1.1.1 Definitions

(2)

1.1.2 Historical Background

(7)

1.2 A Historical Perspective

(8)

C.S. Lazik

1.2.1 Introduction

(2)

1.2.2 Modifications to the Grimm Design

(1)

1.2.3 Development of Depth Profiling Applications

(1)

1.2.4 Developments in Hollow Cathode Lamps

(1)

1.2.5 Boosted GD Sources

(1)

1.2.6 Development of the Radio Frequency Glow Discharge

(3)

1.3 An Overview of GD-OES

(29)

R. Payling

1.3.1 Introduction

(2)

1.3.2 Instrumentation

(4)

1.3.3 Glow Discharge

(1)

1.3.4 Sputtering and Crater Effects

(3)

1.3.5 Quantitative Analysis

(5)

1.3.6 Bulk Analysis

(1)

1.3.7 Quantitative Depth Profiles

(2)

1.3.8 Applications of GD-OES to Bulk Analysis

(1)

1.3.9 Applications of GD-OES to Coatings and Surfaces

(5)

1.3.10 Conclusion

(6)

2. Glow Discharge Sources

(42)

2.1 Introduction

(3)

M. Bouchacourt

F. Schwoehrer

2.2 Grimm Source

(8)

M. Bouchacourt

F. Schwoehrer

2.2.1 Source Components

(1)

2.2.2 Ancillary Components

(1)

2.2.3 Pressure Measurement in the Discharge

(3)

2.2.4 Sequences Used for Analysis

(2)

2.3 dc Operation

(5)

M. Bouchacourt

F. Schwoehrer

2.3.1 Defining the Conditions of Analysis

(1)

2.3.2 Determination of Characteristic Curves

(3)

2.4 rf Operation

(3)

M.S. Marychurch

R. Payling

2.4.1 Definition of the Condition of Analysis

(3)

2.5 Other Sources

(7)

R. Payling

2.5.1 Variations on the Grimm Source

(2)

2.5.2 Boosted Sources

(2)

2.5.3 Radio Frequency

(3)

2.6 Gas Jet Boosted GD-OES

(14)

H.J. Kim

E.H. Piepmeier

2.6.1 Introduction

(2)

2.6.2 Fundamental Characteristics

(7)

2.6.3 Analytical Performance

(2)

2.6.4 Future Study

(3)

3. Instrumentation and Operation

(74)

3.1 Optics

(8)

T. Nelis

3.1.1 Basic Concepts

(1)

3.1.2 Gratings

(3)

3.1.3 Spectrometer Design

(2)

3.1.4 Fourier Transform Spectrometer

(2)

3.2 Vacuum and Gases

101

(11)

R. Payling

3.2.1 Vacuum System

102

(1)

3.2.2 Pumps

103

(2)

3.2.3 Gauges

105

(1)

3.2.4 Residual Vacuum

106

(2)

3.2.5 Gases

108

(4)

3.3 dc and rf Power Supplies

112

(5)

R. Payling

3.3.1 dc Power Supplies

112

(1)

3.3.2 rf Power Supplies

113

(4)

3.4 Signal Acquisition

117

(8)

M. Analytis

S. Rumble

3.4.1 Background

117

(1)

3.4.2 Detectors

117

(3)

3.4.3 Signal Processing

120

(5)

3.5 Computing

125

(6)

M. Analytis

3.5.1 Typical Hardware Requirements

126

(2)

3.5.2 Sample Software Implementation

128

(3)

3.6 Commercial Systems

131

(18)

3.6.1 ISA Jobin-Yvon Division

131

(6)

P. Hunault

3.6.2 LECO Corporation

137

(6)

K. Marshall

3.6.3 Spectruma-Analytik GmbH

143

(6)

M. Analytis

3.7 Sample Preparation

149

(6)

W. Fischer

3.7.1 General

149

(1)

3.7.2 Powdered Samples

150

(2)

3.7.3 Reference Materials

152

(1)

3.7.4 Non-flat Samples

152

(1)

3.7.5 Surfaces

153

(2)

3.8 Non-flat Samples

155

(5)

F. Schwoehrer

3.8.1 Introduction

155

(1)

3.8.2 Description of Device

156

(4)

3.9 Basic Operations

160

(5)

D.G. Jones

3.9.1 Standard Operating Procedures

160

(1)

3.9.2 Importance of the Anode-Sample Gap

161

(1)

3.9.3 Source Window Cleanliness

162

(2)

3.9.4 Anode Condition

164

(1)

4. Direct Current Discharge

165

(42)

4.1 Basic Principles

167

(9)

K. Wagatsuma

4.1.1 General Characteristics of a dc Glow Discharge

167

(3)

4.1.2 Structure of dc Glow Discharges

170

(2)

4.1.3 Behaviour of Electrons

172

(4)

4.2 Plasma Models

176

(16)

A. Bogaerts

R. Gijbels

4.2.1 Introduction

176

(1)

4.2.2 Overview and Description of Models

177

(4)

4.2.3 Results

181

(9)

4.2.4 Summary

190

(2)

4.3 Glow Discharge Characteristics

192

(6)

A. Bengtson

4.3.1 Introduction

192

(1)

4.3.2 Voltage-Current-Pressure Characteristics

193

(3)

4.3.3 Optical Emission Linewidths

196

(1)

4.3.4 Summary

197

(1)

4.4 Emission Characteristics

198

(9)

R. Payling

4.4.1 Introduction

198

(1)

4.4.2 Intensity Changes with Current, Potential, Pressure and Power

199

(1)

4.4.3 Emission Yields

200

(1)

4.4.4 Sensitivity Factors

201

(2)

4.4.5 He/Ar Plasma Gas Mixtures

203

(4)

5. Radio Frequency Discharge

207

(36)

5.1 Basic Principles

209

(17)

M. R. Winchester

5.1.1 Nature of the Radio Frequency Glow Discharge

209

(1)

5.1.2 Sputtering in the Radio Frequency Glow Discharge

210

(4)

5.1.3 Radio Frequency Plasma Sheaths

214

(2)

5.1.4 Excitation and Ionisation in the Radio Frequency Glow Discharge

216

(2)

5.1.5 Radio Frequency Source Design

218

(8)

5.2 Emission Characteristics

226

(9)

M.R. Winchester

5.2.1 Dependencies of Emission Intensities on Discharge Parameters

226

(4)

5.2.2 Self-absorption in the rf Glow Discharge

230

(2)

5.2.3 Effect of Insulating Samples

232

(3)

5.3 Analytical Characteristics and Figures of Merit

235

(8)

M.R. Winchester

5.3.1 Plasma Stabilisation Times

235

(3)

5.3.2 Signal Precision

238

(1)

5.3.3 Sample-to-Sample Reproducibility

239

(1)

5.3.4 Detection Limits

239

(1)

5.3.5 Matrix Effects and Spectral and Chemical Interferences

240

(1)

5.3.6 Analytical Accuracy

241

(2)

6. Sputtering

243

(50)

6.1 Basic Principles

245

(9)

B.V. King

6.1.1 Introduction

245

(2)

6.1.2 Sputter Yield

247

(2)

6.1.3 Sputtered Species and Energies

249

(1)

6.1.4 Preferential Sputtering

250

(1)

6.1.5 Ion Implantation and Reflection

251

(1)

6.1.6 Surface Topography

251

(3)

6.2 Sputtering in the Glow Discharge Source

254

(19)

R. Payling

6.2.1 Introduction

254

(1)

6.2.2 Ion Beam Sputtering

254

(2)

6.2.3 Non-linear Theory

256

(3)

6.2.4 Sputtering Equations

259

(2)

6.2.5 Experimental Data

261

(9)

6.2.6 Conclusion

270

(3)

6.3 Near Surface

273

(14)

B. V. King

R. Payling

6.3.1 Introduction

273

(1)

6.3.2 Plasma Formation

273

(7)

6.3.3 Non-equilibrium Sputtering

280

(4)

6.3.4 GD-OES of the Near Surface

284

(3)

6.4 Mass Loss Versus Depth Dilemma

287

(6)

R. Payling

6.4.1 Introduction

287

(1)

6.4.2 Factors Determining Density

287

(2)

6.4.3 Calculations of Density

289

(2)

6.4.4 Consequences for GD-OES

291

(2)

7. Crater Effects and Depth Resolution

293

(46)

7.1 Crater Depth Measurement

295

(5)

A. Quentmeier

7.1.1 Measurement of Sputtered Mass

295

(1)

7.1.2 Profiling Techniques

296

(4)

7.2 Evolution of Crater Shape

300

(9)

A. Quentmeier

7.2.1 General Considerations

300

(2)

7.2.2 Definitions of Parameters

302

(1)

7.2.3 Influence of Working Conditions

303

(1)

7.2.4 Changes of Crater Shape and Roughness with Sputtered Depth

304

(5)

7.3 Depth Resolution

309

(10)

A. Quentmeier

7.3.1 Definitions

309

(2)

7.3.2 Measurement of Depth Resolution

311

(4)

7.3.3 Ultimate Limits

315

(4)

7.4 Experimental Results for Iron and Zinc Matrices

319

(10)

J. Angeli

7.4.1 Working Field of dc GD-OES

319

(2)

7.4.2 Shape of the Erosion Crater

321

(4)

7.4.3 Sputtering-induced Microstructures

325

(4)

7.5 Crater Effect, Depth Resolution and Thickness Determination

329

(10)

Z. Weiss

7.5.1 Introduction

329

(1)

7.5.2 Model of Crater Effect

330

(2)

7.5.3 Results

332

(7)

8. Optical Emission

339

(72)

8.1 Basic Physical Principles

341

(6)

K. Wagatsuma

8.1.1 Nature of Optical Emission

341

(2)

8.1.2 Intensity of Emission Line

343

(1)

8.1.3 Temperature of Excitation Source

343

(1)

8.1.4 Local Thermodynamic Equilibrium (LTE)

344

(1)

8.1.5 Measurement of Excitation Temperatures

345

(2)

8.2 Optical Emission in the Glow Discharge Source

347

(8)

K. Wagatsuma

8.2.1 Energy Distribution of Particles

347

(1)

8.2.2 Non-LTE

348

(1)

8.2.3 Excitation and De-excitation Processes in GD Plasma

349

(6)

8.3 Interpreting Spectra

355

(5)

T.R. Harville

8.3.1 Introduction

355

(2)

8.3.2 Examples

357

(3)

8.4 Line Selection

360

(5)

T.R. Harville

8.4.1 Selection Criteria

360

(1)

8.4.2 Line Selection Methodology

361

(4)

8.5 Lineshape

365

(11)

R. Payling

P.L. Larkins

8.5.1 Physical Lineshapes

365

(2)

8.5.2 Voigt Profile

367

(3)

8.5.3 Measured Profiles

370

(6)

8.6 Self-absorption

376

(16)

R. Payling

M. S. Marychurch

A. Dixon

8.6.1 Introduction

376

(5)

8.6.2 Self-absorption Model

381

(2)

8.6.3 Calculated Line Profiles

383

(1)

8.6.4 Calculated Signal

384

(2)

8.6.5 Experimental

386

(3)

8.6.6 Results

389

(1)

8.6.7 Summary

390

(2)

8.7 Background Effects

392

(11)

R. Payling

8.7.1 Introduction

392

(2)

8.7.2 Background Correction

394

(5)

8.7.3 Inter-element Line Interferences

399

(4)

8.8 Poisoning Effects

403

(8)

W. Fischer

8.8.1 Introduction

403

(1)

8.8.2 Compacted Powders

404

(1)

8.8.3 Gaseous Contamination

404

(7)

9. Bulk Analysis

411

(42)

9.1 Calibration

413

(5)

T. Nelis

9.1.1 Choice of Certified Reference Materials

413

(1)

9.1.2 Linear Approach

413

(1)

9.1.3 Weighted Regression

414

(1)

9.1.4 Internal Standards

414

(1)

9.1.5 The Relative (Virtual) Method

415

(1)

9.1.6 Recalibration

416

(2)

9.2 Multi-element Calibration

418

(10)

Z. Weiss

9.2.1 Method

418

(3)

9.2.2 Examples

421

(7)

9.3 Analytical Figures of Merit

428

(12)

R. Payling

9.3.1 Quality of the Signal

428

(3)

9.3.2 Precision

431

(3)

9.3.3 Calibration

434

(3)

9.3.4 Accuracy

437

(1)

9.3.5 Depth Profiling

438

(1)

9.3.6 Other Quality Factors

438

(2)

9.4 Detection Limits

440

(13)

P.W.J.M. Boumans

9.4.1 Detection Limit and SBR-RSDB Approach

440

(5)

9.4.2 Detection Limit and Precision

445

(1)

9.4.3 'True' Detection Limit and Line Interference

446

(7)

10. Quantitative Depth Profiling

453

(44)

10.1 General Principles

455

(5)

A. Bengtson

10.1.1 Bulk Analytical Methods for Elemental Concentrations

455

(2)

10.1.2 Sputtering Depth Determination

457

(1)

10.1.3 The Emission Yield Concept as a Basis for Quantification

458

(2)

10.2 Quantitative Models Based on Emission Yields

460

(12)

R. Payling

D.G. Jones

10.2.1 Introduction

460

(1)

10.2.2 Simplest Model

460

(3)

10.2.3 General Equation

463

(1)

10.2.4 Sputtering Rate and Depth

463

(1)

10.2.5 Relative Sensitivity Factors

464

(1)

10.2.6 Emission Yield

464

(3)

10.2.7 Binary Alloys: a Special Case

467

(2)

10.2.8 Integrated Intensities: another Special Case

469

(3)

10.3 Intensity Normalisation

472

(11)

A. Bengtson

10.3.1 Calibration by Normalisation to a Standard Sputtering Rate

473

(2)

10.3.2 Determination of Elemental Concentrations and Sputtered Mass

475

(1)

10.3.3 Calculation of Sputtered Depth

475

(1)

10.3.4 The Empirical Intensity Expression

476

(2)

10.3.5 Normalisation of Intensities to the Reference Excitation Condition

478

(1)

10.3.6 Determination of the Sputtering Rate

479

(1)

10.3.7 Use of the Intensity Normalisation Technique in Practice

479

(2)

10.3.8 Use of an Ar Emission Line as an Internal Standard

481

(1)

10.3.9 Summary

482

(1)

10.4 Influence of Source Parameters

483

(14)

R. Payling

10.4.1 Introduction

483

(1)

10.4.2 Theory

484

(2)

10.4.3 Tests of Emission Yield Dependence

486

(9)

10.4.4 Conclusions

495

(2)

11. Applications of GD-OES to Bulk Analysis

497

(66)

11.1 Steel

499

(12)

R. Payling

11.1.1 Introduction

499

(2)

11.1.2 Experimental

501

(3)

11.1.3 Calibration

504

(4)

11.1.4 Analysis

508

(1)

11.1.5 Further Refinements

508

(3)

11.2 Cast Iron

511

(7)

Z. Weiss

11.3 Brasses

518

(6)

Z. Weiss

11.4 Zinc-Aluminium Alloys

524

(7)

M. S. Marychurch

R. Payling

11.4.1 Method 1 (Empirical)

527

(1)

11.4.2 Method 2 (Theoretical)

528

(2)

11.4.3 Summary

530

(1)

11.5 Aluminium-Silicon Alloys

531

(5)

Z. Weiss

11.6 Precious Metals

536

(5)

T. R. Harville

11.7 Polymers

541

(6)

D.G. Jones

11.7.1 Introduction

541

(1)

11.7.2 Experimental

541

(2)

11.7.3 Results

543

(3)

11.7.4 Discussion

546

(1)

11.8 Glasses and Ceramics

547

(4)

T.R. Harville

11.9 Compacted Powders

551

(12)

V. Hoffmann

H. Mai

11.9.1 Introduction

551

(2)

11.9.2 Peculiarities in the Analysis of Compacted Powders

553

(3)

11.9.3 Preparation

556

(13)

11.9.4 Analysis

569

12. Applications of GD-OES to the Depth Profiling of Metallic Coatings

563

(34)

12.1 Basic Applications

565

(10)

J. Angeli

12.1.1 General Aspects

565

(1)

12.1.2 Experimental

566

(1)

12.1.3 Examples

567

(8)

12.2 Zinc-Iron Coatings

575

(7)

S. Suzuki

K. -I. Suzuki

12.2.1 Sputtering Rate and Optical Emission

576

(1)

12.2.2 Evaluation of Depth Profiling

577

(2)

12.2.3 Quantification of Zinc-Iron Coatings

579

(3)

12.3 Other Alloy Coatings

582

(7)

K. Hirokawa

12.3.1 Iron-Nickel

582

(3)

12.3.2 Copper-Zinc

585

(4)

12.4 Metal Interfaces

589

(8)

R. Payling

12.4.1 Introduction

589

(1)

12.4.2 Theory

589

(1)

12.4.3 Hot-dipped Interfacial Alloy Layers

590

(1)

12.4.4 Results

591

(4)

12.4.5 Conclusion

595

(2)

13. Applications of GD-OES to Reactive Diffusion

597

(62)

13.1 Depth Profiling and Reactive Diffusion

599

(6)

Z.Weiss

13.1.1 Theory of Reactive Diffusion

599

(4)

13.1.2 Examples

603

(2)

13.2 High-temperature Corrosion and Oxide Scales on Steels

605

(8)

Z. Weiss

13.2.1 General Overview and Analytical Requirements

605

(4)

13.2.2 A High-temperature Oxidation Study Based on GD-OES Depth Profiles

609

(4)

13.3 Oxidised Alloy Surfaces

613

(14)

K. Hirokawa

13.3.1 Oxidised Layer on Copper-Nickel Binary Alloys

613

(4)

13.3.2 Oxide Sputtering Rates and Thicknesses

617

(10)

13.4 Oxide Scales on Steel

627

(7)

S. Suzuki

S. Yamazaki

13.4.1 Emission and Sputtering Characteristics

627

(3)

13.4.2 Quantitative Depth Profiling of Oxide Scales

630

(1)

13.4.3 Examples

630

(4)

13.5 Oxide Scales on High-temperature Alloys

634

(7)

W. Fischer

13.5.1 Introduction

634

(1)

13.5.2 Optimum Mode of Operation

635

(1)

13.5.3 Simplified Quantitative Method for Oxides

636

(1)

13.5.4 Results

637

(4)

13.6 Surface Hardened Steels

641

(11)

Z. Weiss

13.6.1 Terminology and Analytical Requirements

641

(1)

13.6.2 Nitrogen Depth Profiling by GD-OES

642

(6)

13.6.3 Examples

648

(4)

13.7 Other Applications Involving Diffusion

652

(7)

Z. Weiss

14. Other Applications of GD-OES to Depth Profiling

659

(54)

14.1 Polymers

661

(7)

D.G. Jones

R. Payling

14.1.1 Introduction

661

(1)

14.1.2 Pigmented Polyester Coatings

662

(2)

14.1.3 Weathered Polyester Coatings

664

(4)

14.2 Semiconductors

668

(8)

I. M. Dharmadasa

M. Ives

J. S. Brooks

C. Breen

14.2.1 Introduction

668

(1)

14.2.2 Experimental Results

669

(6)

14.2.3 Discussion and Concluding Remarks

675

(1)

14.3 Hard Coatings

676

(12)

H. Bohm

14.3.1 Materials and Production Processes

676

(2)

14.3.2 Analysis and Quantification of Time-related Depth Profiles

678

(5)

14.3.3 Quantification of Time-related Depth Profiles of Hard Coatings

683

(5)

14.4 Characterisation of Steel Sheet Surfaces

688

(10)

J. Angeli

14.4.1 Measurement Settings

688

(3)

14.4.2 Precision of the Analysis Results

691

(3)

14.4.3 Some Applications

694

(4)

14.5 Non-flat Samples

698

(15)

F. Schwoehrer

14.5.1 Materials Studied

698

(1)

14.5.2 Determination of the Optimum Conditions of Analysis

698

(3)

14.5.3 Results and Discussion

701

(9)

14.5.4 Conclusion

710

(3)

15. Comparison with Other Techniques

713

(44)

15.1 Surface Analysis

715

(7)

R. Payling

15.1.1 Introduction

715

(1)

15.1.2 Comparisons from Multi-technique Analysis of Surfaces

716

(5)

15.1.3 Conclusion

721

(1)

15.2 Coating Analysis

722

(7)

S. Suzuki

15.2.1 AES and GD-OES

722

(3)

15.2.2 XPS and GD-OES

725

(1)

15.2.3 SIMS and GD-OES

726

(3)

15.3 Bulk Analysis: Glow Discharge Versus Spark

729

(6)

Z. Weiss

15.3.1 Fundamental Differences

729

(2)

15.3.2 Experimental Comparisons

731

(4)

15.4 Glow Discharge Mass Spectrometry

735

(22)

A. Raith

15.4.1 Instrumentation

735

(1)

15.4.2 Bulk Analysis

736

(9)

15.4.3 Depth Profiling

745

(9)

15.4.4 Conclusion

754

(3)

Appendix 1. Spectral Data

757

(12)

R. Payling

Appendix 2. Calibration Data

769

(2)

A. Bengtson

Appendix 3. Operating Procedures

771

(10)

D. G. Jones

Bibliography

781

(47)

R. Payling

Units, Conversions and Constants

828

(1)

Index

829

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Glow Discharge Optical Emission Spectrometry

Summary

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Glow Discharge Optical Emission Spectrometry

Summary

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