Ultratrace and microdistribution analysis in material sciences |
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Authors: | Hugo M Ortner and Peter Wilhartitz |
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Institution: | (1) Metallwerk Plansee GmbH, A-6600 Reutte, Austria |
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Abstract: | Summary All-rounders and experts are two basic types of scientists. A harmonic cooperation between these two groups is essential for today's large study groups engaged in materials development. Materials development programmes in many high-tech countries are major fields of research supported by special financial arrangements (e.g. COST, EURAM or BRITE-programmes in Europe). Modern materials development is not possible without analytical guidance. This is not always realized by all engaged partners and it is a main obligation of analytical chemists to make aware of the role of a potent materials characterization in relevant development programmes. This should be demonstrated in two essential relevant areas:
a) Bulk trace and ultra trace analysis of metals. Many important metal properties are directly or indirectly influenced by trace elements. In complex systems like fusion reactors or microelectronic components, trace contents of even minor metal parts might decisively influence system properties. As refractory metals and their silicides gain rising importance in VLSI microelectronic applications, their ultratrace characterization becomes a major challenge. Essential progress was possible by the complementary application of mass-spectrometric methods. Latest results and a critical survey will be given, including GDMS, SIMS, SSMS, IDMS and ICP-MS.Surprisingly, however, highest sensitivities and best detection limits were recently achieved by a combination of trace-matrix separation procedures and final end determination with ICP-MS. This combination also proved to be the most economic and safest approach from the view point of accuracy and precision.
b) The analytical characterization of discontinuities and heterogeneities in solid matter. Practical examples are again taken from the study of refractory and hard metals and ceramics. A survey is given as to the manifold effects, heterogeneities and discontinuities exert on modern high-tech materials: as a function of their average diameter, they can either strengthen the material (dispersion strengthening), or they can cause deterioration of material properties e.g. as points of crack initiation, by grain boundary embrittlement etc. Together with most important methods for detection and characterization of heterogeneities and discontinuities, their evaluation and possible prevention during materials fabrication are discussed and pertinent examples are given. The phenomena of heterogeneous particles and pores are elucidated in more detail. Acronyms used 1 Abbreviations for European research programmes AGATA
Advanced Gas Turbines for Automobiles
- BRITE
Basic Research for Industrial Technologies for Europe
- COST
Cooperation in Science and Technology
- EURAM
European Research Activities Programme on Materials
2 Abbreviations in the field of refractory metals technology ADM
Ammonium-Di-Molybdate
- APT
Ammonium-Para-Tungstate
- HP
High Purity
- MHC
Molybdenum-based alloy containing 1.2% Hf and 0.1% C
- NS
Non-sag (tungsten, used for lamp filaments and evaporative metallization techniques)
- ODS
Oxide Dispersion Strengthened
- RM
Refractory Metal
- TZM
Molybdenum-base alloy containing 0.5% Ti, 0.08% Zr and 0.025% C
- UHP
Ultra High Purity
- VLSI
Very large scale integration
- ZHM
Molybdenum-base alloy containing 0.40% Zr, 1.2% Hf and 0.15% C
3 Analytical technique names AA
Activation Analysis
- AAS
Atomic Absorption Spectrophotometry
- AES
Auger Electron Spectrometry or Atomic Emission Spectrometry (only used in this work where it is clear that Auger Electron Spectrometry is not meant)
- EDX(RS)
Energy Dispersive X-Ray Spectrometry
- EELS
Electron Energy Loss Spectrometry
- EP(X)MA
Electron Probe X-Ray Microanalysis
- GDMS
Glow Discharge Mass Spectrometry
- GFAAS
Graphite Furnace Atomic Absorption Spectrometry
- ICP-OES, MS
Inductively Coupled Plasma — Optical Emission Spectrometry, Mass Spectrometry
- ID-MS
Isotope Dilution — Mass Spectrometry
- LAS
Classical photometry (Liquid Absorption — Spectrophotometry)
- LEED
Low Energy Electron Diffraction
- MS
Mass Spectrometry
- NAA
Neutron Activation Analysis
- OES
Optical Emission Spectrometry
- SEM
Scanning Electron Microscopy
- SIMS
Secondary Ion Mass Spectrometry
- SSMS
Spark Source Mass Spectrometry
- TEM
Transmission Electron Microscopy
- TMS
Trace-Matrix Separation (procedure)
- WLD(-XRS)
Wave Length Dispersive — XRS
- XR(F)S
X-Ray (Fluorescence) Spectrometry |
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