Thin Film and Depth Profile Analysis

213 Pages·1984·4.823 MB·English

by  H. Oechsner (auth.), Professor Dr. Hans Oechsner (eds.)

37
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20 Inverse ScaHering Problems in Optics 37 Thin Film and Depth Profile Analysis
Editor: H. P. Baltes Editor: H. Oechsner
Thin Film and
Depth Profile Analysis
Edited by H. Oechsner
With Contributions by
H.-W. Etzkorn W. O. Hofer S. Hofmann J. E. Kempf
J. Kirschner U. Littmark H. J. Mathieu
H. Oechsner J. M. Sanz H. H. Wagner
H.W. Werner
With 99 Figures
Springer-Verlag
Berlin Heidelberg New York Tokyo 1984
Professor Dr. Hans Oechsner
Universitat Kaiserslautern, Erwin-Schrodinger-Straf3e, Gebaude 46,
D-6750 Kaiserslautern, Fed. Rep. of Germany
ISBN-13:978-3-642-46501-7 e-ISBN-13:978-3-642-46499-7
DOl: 10.1007/978-3-642-46499-7
Library of Congress cataloging in Publication Data. Main entry under title: Thin film and depth profile
analysis. (Topics in current physics; 37) Includes bibliographical references and index. 1. Thin films
Surfaces. 2. Surface chemistry. 3. Sputtering (Physics) I. Oechsner, H. (Hans), 1934-. II. Etzkorn, H. W. III.
Series. QC176.84.S93T46 1984 530.4'1 84-5394
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Preface
The characterization of thin films and solid interfaces as well as the determina
tion of concentration profiles in thin solid layers is one of the fields which re
quire a rapid transfer of the results from basic research to technological applica
tions and developments. It is the merit of the Dr. Wilhelm Heinrich and Else
Heraeus-Stiftung to promote such a transfer by organizing high standard seminars
mostly held at the "Physikzentrum" in Bad Honnef near Bonn. The present book has
been stimulated by one of these seminars assembling most of the invited speakers as
co-authors. The editor appreciates the cooperation of his colleagues contributing
to this book.
Kaiserslautern, April 1984 H. Oechsner
v
Contents
1. Introduction. ByH. Oechsner ........................................... .
1.1 Requirements for Thin Film and In-Depth Analysis .................. . 1
1. 2 Object and Outl i ne of the Book .................................... . 2
References 4
2. The Application of Beam and Diffraction Techniques to Thin Film and
Surface Micro-Analysis. By H. W. Werner (With 25 Fi gures) ............... . 5
2.1 Methods to Determine Chemical Structures in Material Research 5
2.2 Selected Analytical Features Used to Determine Chemical Structures 9
2.2.1 Depth Profi 1i ng ............................................ . 9
a) Destructive Depth Profiling 9
b) Nondestructive Methods for Depth and Thin Film Analysis 15
2.2.2 Microspot Analysis and Element Imaging 19
2.3 Determining Physical Structures in Material Research ....... ........ 27
2.3.1 X-Ray Diffraction . ............ ...... .... ...... ...... ........ 27
2.3.2 X-Ray Double Crystal Diffraction ...... .... ............ ...... 28
2.3.3 Ultrasonic (Acoustic) Microscopy 29
2.4 Application of Different Microanalytical Techniques to Specific
Ana lyti ca 1 Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
2.4.1 AES and TEM-EDX in Interface Analysis of MnZn Ferrites 29
2.4.2 Interfaces of SrTi03 Boundary Layer Capacitor Material
Studies by TEM and Selected-Area EDX ........................ 31
2.4.3 Analysis of GaA1As with SIMS, X-Ray Diffraction and AES 32
2.5 Future Prospects 36
References 37
3. Depth Profile and Interface Analysis of Thin Films by AES and XPS
By H.J. Mathieu (With 13 Figures) ....................................... 39
3.1 Quantification from First Principles ............................... 39
3.2 Initial Transient Layer ............................................ 43
3.3 Steady-State Region ................................................ 47
3.4 Film-Substrate Interface 51
References 58
VII
4. Secondary Neutral Mass Spectrometry (SNMS) and Its Application to
Depth Profile and Interface Analysis. By H. Oechsner (With 17 Figures) 63
4.1 Background • . . . . . . . . . . . . . . • . . . . . . . . . . . . • . • . • . . . • . . . . . . . . . . . . . . . . . . . . 63
4.2 Experimental Method ....•......... , ...•.....•.. " . . . . . .. . . . .••. .. ... 64
4.2.1 Related Techniques ..........•.....................•.....•... 64
4.2.2 Performance of SNMS ... • . . . . • • . . . . . . . . . . . . . . . . . . . . . . . . . . • . . . . 65
a) The Postionizing Method .....•.....•..................•... 65
b) Opera t i on r~odes of SNMS .. • . . . • • . . . . . . . . . • . . . . . . . • . . . . . . • . 67
4.3 Quantification of SNMS ...........•......•..•..•........•.••........ 69
4.3.1 Quantification for Atomic Sputtering ..•.......•....•........ 70
4.3.2 Quantification Using Molecular SNMS Signals ......... ........ 74
4.3.3 Sensitivity of SNMS ......•............•.........•........... 76
4.4 Applications of SNMS to Depth Profile Analysis 77
4.4.1 General Considerations •.................•...•..•............ 77
4.4.2 Examples of Depth Profiling by SNMS ......................... 80
4.5 Concluding Remarks 84
References 84
5. In-Situ Laser Measurements of Sputter Rates During SIMS/AES In-Depth
Profiling. By J.E. Kempf and H.H. Wagner (With 16 Figures) .............. 87
5.1 Background . . . . . . . . . . . • . . . . . . . . . • . . . . • . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
5.2 Principles of Laser Technique ...........................•.......... 87
5.2.1 Laser Optical Arrangement ....................•.............. 87
5.2.2 Phase and Reflectance Measurement ......................•.... 88
5.2.3 Fundamentals of Sputter-Rate Determination 88
5.3 Experiments 89
5.4 Results and Discussion 90
5.4.1 Signal Artefacts 90
5.4.2 Phase and Reflectance Measurements During Sputtering 91
a) Sputtering of Silicon Surfaces .•......................... 91
b) Doped S i 1 icon ...........................•................ 94
c) Metal Film Material ....................................... 94
d) Transparent Material 96
e) Opaque and Transparent Multilayers 97
5.5 Conclusion 98
5.A. Appendix ....•.......•.............................................. 99
A.1. Opaque Material ..........•..•................................ 99
A.2. Transparent Material 99
References 101
VIII
6. Physical Limitations to Sputter Profiling at Interfaces - Model Experiments with
Ge/Si Using KARMA. By J. Kirschner and H.-W. Etzkorn (With 14 Figures). 103
6.1 Background ... ....... ..... ..... .... ............ ........ ............. 103
6.1.1 General Problems Encountered in Sputter Profiling 103
6.1.2 Requirements for a Model Experiment 107
6.2 Experimenta 1 Approach . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108
6.2.1 KARMA ....................................................... 108
6.2.2 Sample Preparation 111
6.3 Conversion of Raw Sputter Profiles into Depth Profiles .... ......... 112
6.3.1 Establishing the Depth Scale ................................ 112
6.3.2 Escape-Depth Correction 114
6.3.3 Self-Consistent Determination of Effective ~1ean Free Paths 118
6.4 Depth Profiles of the GelSi Interface ..................... , ....... . 120
6.4.1 Asymmetry of Depth Profiles ................................ . 120
6.4.2 Broadening as a Function of Ion Mass and Energy ............ . 125
6.5 Dose Effects and Preferential Sputtering .......................... . 127
6.5.1 Dose Effects ............................................... . 127
6.5.2 Preferential Sputter~ng 129
6.6 Depth Resolution in Sputter Profiling ........ '" .................. . 130
6.6.1 Depth Resolution Limits .................................... . 131
6.7 Summary and Outlook 134
References 137
7. Depth Resolution and Quantitative Evaluation of AES Sputtering Profiles
By S. Hofmann and J.M. Sanz (With 9 Figures) ............................ 141
7.1 Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141
7.2 Calibration of the Depth Scale ... ..... .......... ............. ...... 142
7.3 Calibration of the Concentration Scale 143
7.4 Depth Resolution in Sputter Profiling 145
7.5 Determination of the Resolution Function 146
7.5.1 Definition of Depth Resolution 146
7.5.2 Experimental Determination of Depth Resolution .... .......... 147
7.5.3 Model Descriptions of Depth Resolution ...................... 148
7.6 Deconvolution Procedures 152
7.7 Conclusion 156
References 156
8. The Theory of Recoil Mixing in Solids
By U. Littmark and W.O. Hofer (With 5 Figures) ......................... . 159
8.1 Background ..................................... " ................. . 159
8.1.1 Nomenclature 160
IX
8.2 Review of Recoil Mixing Models ..................................... 161
8.2.1 Primary Recoil Implantation and Mixing ...................... 163
8.2.2 Cascade Mixing .............................................. 165
a) Random-Wa 1k Model s . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
b) Transport Theory Approach 166
c) Miscellaneous Approaches 168
8.3 General Formulation of Atomic Relocation Phenomena 170
8.3.1 Target Description .......................................... 171
a) Unbounded Total Density N(~,x) " ......................... 172
b) Total Density Bounded to N(x) = No ....................... 172
8.3.2 Description of Atomic Relocation ............................ 173
8.3.3 Balance Equation' for Atomic Relocation ...................... 175
a) The Diffusion Approximation ....... '" .................... 178
8.4 Solutions to the Specific Mixing Models ............................ 184
8.4.1 Thermal Mixing and Thermal Diffusion ........................ 184
8.4.2 Recoil Mixing 186
a) Cascade Mixing, Diffusion Approaches 189
b) Cascade Mixing, Forthright Solutions 190
8.5 Summary and Outlook ................................................ 196
8.6 List of Symbols .................................................... 198
References 199
Additional References with Titles 201
Subject Index ................................. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 203
x
List of Contributors
Etzkorn, Heinz-Werner
Institut fUr Grenzflachenforschung und Vakuumphysik der Kernforschungsanlage
JUlich GmbH, 0-5170 JUlich, Fed. Rep. of Germany
Present address: Battelle-Institut e.V., Postfach 90 01 60,
0-6000 Frankfurt 90, Fed. Rep. of Germany
Hofer, Wolfgang O.
Institut fUr Grenzflachenforschung und Vakuumphysik der Kernforschungsanlage
JUlich GmbH, EURATOM Association, 0-5170 JUlich, Fed. Rep. of Germany
Hofmann, Siegfried
Max-Planck-Institut fUr Metallforschung, Institut fUr Werkstoffwissenschaften
SeestraBe 92, 0-7000 Stuttgart 1, Fed. Rep. of Germany
Kempf, Jurgen E.
IBM Germany, 0-7000 Stuttgart 80, Fed. Rep. of Germany
Kirschner, Jurgen
Institut fUr Grenzflachenphysik und Vakuumforschung der Kernforschungsanlage
JUlich GmbH, 0-5170 JUlich, Fed. Rep. of Germany
Littmark, Uffe
Institut fUr Grenzflachenforschung und Vakuumphysik der Kernforschungsanlage
JUlich GmbH, EURATOM Association, 0-5170 JUlich, Fed. Rep. of Germany
Mathieu, Hans J.
Ecole Poly technique Federale de Lausanne (EPFL), O~partement des Mat~riaux,
CH-1007 Lausanne, Switzerland
Oechsner, Hans
Universitat Kaiserslautern, Erwin-Schrodinger-Str., Gebaude 46
0-6750 Kaiserslautern, Fed. Rep. of Germany
Sanz, Jose M.
Max-Planck-Institut fUr Metallforschung, Institut fUr Werkstoffwissenschaften,
SeestraBe 92, 0-7000 Stuttgart 1, Fed. Rep. of Germany
Wagner, Hans H.
IBM Germany, 0-7000 Stuttgart 80, Fed. Rep. of Germany
Werner, Helmut W.
Philips Research Laboratories, NL-5600 JA Eindhoven, The Netherlands
XI