Progress in Materials Analysis: Vol. 1

347 Pages·1983·9.61 MB·English

by  Wolfgang O. Hofer (auth.), Prof. Dr. M. Grasserbauer, M. K. Zacherl (eds.)

~-
Supplementum 10
Proceedings of the 11th Colloquium on
Metallurgical Analysis, Institute for Analytical Chemistry,
Technical University in Vienna, November 3-5, 1982
Springer Science+ Business Media, LLC
Vol.1
Edited by M. Grasserbauer
and M. K. Zacherl
Springer-Verlag Wien GmbH
Scientific and Organisation Committee
Prof. Dr. M. Grasserbauer, Technical University of Vienna; Chairman
Dr. S. Baumgartl, Thyssen AG, Duisburg
Prof. Dr. Th. Hehenkamp, University of GDttingen
Dr. K. H. Koch, Hoesch AG, Dortmund
Prof. Dr. H. Malissa, Technical University of Vienna
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With 201 Figures
ISBN 978-3-211-81759-9 ISBN 978-3-7091-3943-1 (eBook)
DOI 10.1007/978-3-7091-3943-1
Preface
The 11th Colloquium on Metallurgical Analysis - a joint venture of the
Institute of Analytical Chemistry of the Technical University in Vienna, the
Austrian Society for Analytical Chemistry and Microchemistry, the German
Metals Society (DGM), and the Society of German Iron and Steel Engineers
(VDEh) - was attended by 120 scientists from 12 nations.
The major topics covered were surface, micro and trace analysis of materials
with a heavy emphasis on metals. According to the strategy of the meeting
attention was focussed on an interdisciplinary approach to materials
science - combining analytical chemistry, solid state physics and tech
nology.
Therefore progress reports on analytical techniques (like SIMS, SNMS,
Positron Annihilation Spectroscopy, AES, XPS) were given as well as pre
sentations on the development of materials (like for the fusion reactor). The
majority of the discussion papers centered on the treatment of important
technical problems in materials science and technology by a (mostly sophis
ticated) combination of physical and chemical analytical techniques.
The intensive exchange of ideas and results between the scientists oriented
towards basic research and the industrial materials technologists was very
fruitful and resulted in the establishment of several scientific cooperations.
Major trends in materials analysis were also dealt with in a plenary discussion
of which a short summary is contained in this volume.
In order to facilitate international communication in the field of materials
analysis and in view of the important questions treated in the various contri
butions this proceedings volume was edited in English.
On behalf of the scientific committee I would like to express my gratitude to
all authors for their contributions and support in publishing the proceedings.
Special thanks go to Doz. Dr. W. Wegscheider, Technical University Graz, for
linguistic editorial work.
M. Grasserbauer
Technical University Vienna
Chairman of Scientific Committee
Contents
Page
Grasserbauer, M. Summary of Plenary Discussion on "Materials
Development - a Challenge to Analytical Chemistry . . . . . . . . . . . . . XI
Hofer, W. 0. Materials for the First Wall of Fusion Reactors and Their
Analytical Characterization ............................... .
Hehenkamp, Th., W. Liihr-Tanck, and A. Sager. Application of Positron
Annihilation to Metallic Alloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Lodding, A., and H. Odelius. Applications of SIMS in Interdisciplinary
Materials Characterization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Miiller, K. H., and H. Oechsner. Quantitative Secondary Neutral Mass
Spectrometry Analysis of Alloys and Oxide-Metal-Interfaces . . . . . . . 51
Pimminger, M., and M. Grasserbauer. Surface Analysis of Metals with
. SIMS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
Mai, H. Characterization of Metallic Glasses by Ion and Electron
Microprobes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
Stingeder, G., M. Grasserbauer, H. M. Ortner, W. Schintlmeister, and
W. Wallgram. Quantitative Surface Analysis of CVD-Hard Material
Coatings with SIMS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
Puderbach, H. ISS-and SIMS-Analysis of Thin Organic Layers on
Metal Surfaces . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Steiger, W., F. Riidenauer, H. Gnaser, P. Pollinger, and H. Studnicka.
New Developments in Spatially Multidimensional Ion Microprobe
Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Ill
Grabke, H. J., H. Erhart, and R.Moller. Investigation of Grain Boundary
Segregation in Iron-Base Alloys by Auger Electron Spectroscopy ... 119
VIII Contents
Hofmann, S., and J. M. Sanz. Characterization of Anodic Oxide Layers
by Sputter Proftling with AES and XPS ....................... 135
Bubert, H., R. Garten, R. Klockenkamper, and H. Puderbach. Investiga
tions of Phosphate Coatings of Galvanized Steel Sheets by a Surface-
Analytical Multi-Method Approach .......................... 145
Dudek, H. J., W. Braue, and G. Ziegler. Surface-and Microanalytical
Investigations of the Chemical Constitution of the Grain Boundary
Phase in Dense Silicon Nitride . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159
Laimer, S., P. Braun, H. Stori, F. ViehbOck, P. Rodhammer, and
K. Kailer. Analysis of Reactively Ion Plated Titanium-Nitride Films . 177
Ebel, M. F., H. Ebel, U. Paschke, G. Zuba, and J. Wernisch. Quantita-
tive Surface Analysis Without Reference Samples . . . . . . . . . . . . . . . 189
von Rosenstiel, A. P., P. Schwaab, and J.D. Brown. Improved Methods
of Quantitative Electron Probe Microanalysis of Carbon-1P(pz)
Compared to Other Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 199
Willich, P., A. P. von Rosenstiel, and N. Drost. Quantitative Electron
Probe Microanalysis of Sputtered FeC Dry Lubrication Films ...... 211
Kleykamp, H. Experimental and ZAF Correction Aspects of Carbon
Analysis in Steels: Application to the Carburization of Irradiated
Uranium-Plutonium Carbide Fuel Pin Claddings ................. 217
Karduck, P., H. J. Schiirhoff, and W.-G. Burchard. Quantitative
Electron Probe Microanalysis of Borides in Aluminium ........... 231
Rudolph, G. Microprobe Measurements to Determine Phase Boundaries
and Diffusion Paths in Ternary Phase Diagrams Taking a Cu-Ni-Al
System as an Example .................................... 241
Ullrich, H.-J., S. Rolle, A. Uhlig, P. Ettmayer, and B. Lux. Investiga
tion of (Mo,W)C Mixed Carbides by Electron Probe Microanalysis
and Kassel Technique ..................................... 251
Falch, S., and S. Steeb. X-Ray Emission Spectroscopy by Means of
Electron-Microprobe for the Determination of the Density of
States with Binary Amorphous Alloys . . . . . . . . . . . . . . . . . . . . . . . . 261
Eckert, R., and S. Steeb. X-Ray Excited Fluorescence Spectroscopy
Within SEM for Trace Analysis ............................. 271
Contents IX
Pohl, M., H. Oppolzer, and S. Schild. STEM-EDX Measurements on
Grain Boundary Phenomena of Sensitized Chrome-Nickel Steels .... 281
Thien, V., J. Ewald, and W. Voss. Metallurgical Investigations of
Microstructure and Behaviour of High-Alloyed Manganese-
Chromium Austenitic Steels for Generator-Rotor Retaining Rings . . . 297
Hoke, E., G. Eder, and M. Grasserbauer. Analytical Electron Micro-
scopy for Interface Characterization - Corrosion of Concrete . . . . . . 307
Fidler, J., and P. Skalicky. Electron Microscope Characterization of
Highest-Coercivity Magnetic Materials ........................ 315
Jackwerth, E., and H. Mittelstadt. Multi-Element Preconcentration
from Technical Alloys .................................... 325
Foryst, J ., and W. Przybylo. Application of the Levitation Melting
Technique in the Investigations of Iron and Steel Making ......... 337
Summary of Plenary Discussion on "Materials Development
a Challenge to Analytical Chemistry"
The 11th Colloquium on Metallurgical Analysis was concluded by a plenary
discussion on "Materials Development - a Challenge to Analytical
Chemistry" in which experts from industry and research institutions treated
important areas of materials research and the resulting demands for materials
characterization. The discussion did not cover all important areas of materials
development but rather a selection of topics which seemed important to the
participants. The summary reported here is based mainly on contributions
from K. H. Koch, Hoesch Hiittenwerke, Dortmund, G. Kraft, Deutsche
Metallgesellschaft, Frankfurt, K. H. Schmitz, Mannesmann-Rohren-Werke,
Duisburg, V. Thien, Kraftwerks-Union, Miilheim, H. Beske, Kernforschungs
anlage Jiilich, W. Wintsch, Sulzer, Winterthur, E. Kny, Metallwerk Plansee,
A. P. von Rosenstiel, TNO Apeldoorn, L. Rinderer, Technical University,
Lausanne, G. Tolg, Institute for Applied Spectroscopy and Spectrochemistry,
Dortmund, H. Straube, H. Malissa, and M. Grasserbauer, Technical University,
Vienna.
Development of the following analytical areas and techniques were found to
be particularly important:
1. Development of High Speed Routine Methods - especially for iron and
steel production in order to cope with the increasing speed of the process.
2. Automated Routine Measurements for Gases -- especially oxygen - in
metal melts. Although substantial progress has been achieved the accuracy of
the results is still usually unsatisfactory.
3. Surface Analysis by combination of all major techniques for characteriza
tion of surface treated materials - e.g. wear resistant coatings on hard metals
or steel. High accuracy, high lateral and depth resolution are usually required.
For routine applications large area techniques (like GDOES) seem useful.
The transfer of surface analysis from research institutions to industrial
laboratories is just under way but - despite exceptions -usually not suffi
cient to cope with industrial needs. Main hindrance are the high costs of
establishing surface analytical laboratories.
XII Summary
In-situ-analysis of liquid-solid interfaces for study of reaction phenomena
(electrochemical processes in corrosion) by FTIR-spectrometry seems very
promising.
4. Multi-Element Trace Analysis especially by contamination free techniques
(like SIMS, SNMS, NAA) for low impurity levels (ng/g ··· p.gjg range). The
rapid increase in purity requirements in the course of refinement of materials
demands not only the development of more sensitive methods but also
higher accuracy of trace analytical results. Combination of chemical enrich
ment steps with physical detection methods seems particularly promising.
Due to the development of new materials (e.g. for nuclear power plants)
extreme trace analysis has to be developed even for rare elements (e.g. Gd
in Zr).
Reference materials and recommended methods are still missing for many
problems in multielement trace analysis.
Recycling of materials may introduce a variety of impurities into the pro
cess. The influence of many of these impurities is not well understood. On
the other hand controlled doping of materials with trace elements can be
used to generate specific microstructures and properties. Systematic study
of the behaviour of such trace elements for sinter materials, cast alloys etc.
is necessary - starting with accurate multielement characterization, includ
ing the use of mathematical procedures to correlate properties and trace ele
ments (e.g. by clustering techniques).
5. Distribution Analysis of Trace Elements. Since not only the type and bulk
concentration of trace elements but also their distribution influence material
properties techniques which allow distribution characterization with maxi
mum spatial resolution have to be applied or developed. Scanning AES and
SIMS (Ion Probes, Ion Microprobes) seem to be particularly useful. Major
progress has already been achieved in semiconductor analysis and grain
boundary segregation studies of some elements (e.g. P in iron). Major limita
tions however are still the limited sensitivity of AES and the often unsuffi
cient lateral resolution of SIMS. Major developments in this direction, e.g. by
use of metal ion sources (In, Ga) may open up the area of sub-micrometer
surface distribution analysis of trace elements.
This is particularly useful for characterization of semiconductor devices
(VLSI-circuits), grain boundaries in metals, and compound structures.
Development 'of quantification methods is necessary - especially production
of trace element standards for distribution analysis in metals. Ion implanta
tion may offer large possibilities.
6. Ultra-Microanalysis. Microstructures of dimensions well below 1 p.m are
important for the properties of many materials- e.g. precipitations at grain
boundaries in metals, interface domains in semiconductors. Means to charac-