Metallographic Etching

2nd Edition

By Günter Petzow

In collaboration with Veronika Carle

Translated by Uta Harnisch

Techniques for Metallography Ceramography Plastography Contents

Preface to the German Edition ...... VIII Preface ...... IX Introduction ...... 1 1 Metallography ...... 7 1.1 Preparation of Metallographic Specimens ...... 7 1.2 Specimen Sectioning ...... 8 1.3 Mounting...... 11 1.3.1 Clamping ...... 12 1.3.2 Embedding ...... 13 1.3.3 Special Mounting Techniques ...... 15 1.4 Identification (Marking)...... 18 1.5 Grinding and Polishing ...... 18 1.5.1 Mechanical Grinding and Polishing ...... 19 1.5.2 Microtome Cutting and Ultramilling ...... 29 1.5.3 Electrolytic Grinding and Polishing ...... 30 1.5.4 Chemical Polishing ...... 34 1.5.5 Combined Polishing Methods ...... 34 1.5.6 Evaluation of Polishing Methods ...... 36 1.6 Cleaning ...... 37 1.7 Metallographic Etching ...... 38 1.7.1 Optical Etching ...... 39 1.7.2 Electrochemical (Chemical) Etching ...... 40 1.7.3 Physical Etching ...... 44 1.7.4 Etching Reproducibility ...... 45 1.7.5 Etching Terminology ...... 47 1.7.6 Definitions of Etching Terms ...... 47 1.8 Field Metallography/Nondestructive Metallography...... 50 1.9 Preparation and Etching Recipes for Metallic Materials ...... 51 1.9.1 Silver ...... 53 1.9.2 Aluminum ...... 57 1.9.3 Gold ...... 64

v 1.9.4 Beryllium...... 67 1.9.5 Bismuth and Antimony ...... 70 1.9.6 Cadmium, Indium, and Thallium ...... 72 1.9.7 Cobalt ...... 75 1.9.8 Refractory Metals (Chromium, Molybdenum, Niobium, Rhenium, Tantalum, Vanadium, and Tungsten) . . . . 80 1.9.9 Copper...... 88 1.9.10 Iron, Steel, and Cast Iron ...... 94 1.9.11 Semiconductors (Germanium, Silicon,

Selenium, Tellurium, AIIIBVI, and AIIBVI Compounds)...... 102 1.9.12 Hafnium and Zirconium ...... 109 1.9.13 Mercury (Amalgams)...... 112 1.9.14 Magnesium ...... 114 1.9.15 Manganese...... 117 1.9.16 Nickel ...... 118 1.9.17 Lead...... 125 1.9.18 Platinum Metals (Platinum, Palladium, Rhodium, Iridium, Ruthenium, and Osmium) ...... 130 1.9.19 Plutonium, Thorium, and Uranium, Americium, and Neptunium ...... 133 1.9.20 Tin ...... 135 1.9.21 Titanium ...... 139 1.9.22 Yttrium, Lanthanum, and Rare Earth Metals...... 144 1.9.23 Zinc ...... 148

2 Ceramography ...... 153 2.1 Sample Preparation for Ceramic Materials ...... 153 2.2 Sampling ...... 154 2.3 Mounting...... 154 2.4 Identification ...... 155 2.5 Grinding and Polishing ...... 155 2.5.1 Mechanical Grinding and Polishing ...... 155 2.5.2 Other Grinding and Polishing Methods ...... 158 2.6 Cleaning ...... 158 2.7 Ceramographic Etching ...... 159 2.7.1 Optical Etching ...... 159 2.7.2 Electrochemical (Chemical) Etching ...... 160 2.7.3 Physical Etching ...... 162 2.8 Preparation and Etch Recipes of Ceramic Materials ...... 163 2.8.1 Oxide Ceramics ...... 164 2.8.2 Nitride Ceramics ...... 168 2.8.3 Boride Ceramics ...... 169

vi 2.8.4 Carbide Ceramics...... 169 2.8.5 Phosphide and Sulfide Ceramics ...... 172 2.8.6 Hardmetals (Cemented Carbides)...... 172

3 Plastography...... 175 3.1 Plastographic Sample Preparation ...... 177 3.2 Plastographic Etching ...... 179 3.3 Etchants for Polymers ...... 180 3.4 Plastographic Thin Sectioning ...... 181 3.5 Plastographic Microtome Sectioning ...... 182 3.6 Light Microscopic Studies of Thin Sections or Microtomed Sections . . . 183

4 Appendix ...... 185 4.1 Designation of Etchants ...... 185 4.2 List of Chemicals...... 190 4.3 Hazardous Chemical Symbols and Their Interpretation ...... 196 4.4 Handling Tips for Hazardous Materials ...... 198 4.4.1 Rules, Tips, and Precautions...... 198 4.4.2 Important Special Precautions ...... 199 4.4.3 Dangerous Reactions of Chemicals ...... 202 4.4.4 Disposal of Hazardous Materials...... 203

5 Literature References...... 205 Journals ...... 205 General Textbooks and Reviews...... 205 Handbooks, Compilations, and Tables ...... 208 Metallographic Preparation...... 209 Metallic Materials...... 210 Ceramic Materials ...... 211 Polymer Materials ...... 212

vii ASM International is the society for materials engineers and scientists, a worldwide network dedicated to advancing industry, technology, and applications of metals and materials.

ASM International, Materials Park, Ohio, USA www.asminternational.org

Publication title Product code Metallographic Etching, 2nd Edition 06670G

To order products from ASM International:

Online Visit www.asminternational.org/bookstore

Telephone 1-800-336-5152 (US) or 1-440-338-5151 (Outside US)

Fax 1-440-338-4634

Customer Service, ASM International Mail 9639 Kinsman Rd, Materials Park, Ohio 44073, USA

Email [email protected]

American Technical Publishers Ltd. 27-29 Knowl Piece, Wilbury Way, Hitchin Hertfordshire SG4 0SX, United Kingdom In Europe Telephone: 01462 437933 (account holders), 01462 431525 (credit card) www.ameritech.co.uk

Neutrino Inc. In Japan Takahashi Bldg., 44-3 Fuda 1-chome, Chofu-Shi, Tokyo 182 Japan Telephone: 81 (0) 424 84 5550

Terms of Use. This publication is being made available in PDF format as a benefit to members and customers of ASM International. You may download and print a copy of this publication for your personal use only. Other use and distribution is prohibited without the express written permission of ASM International.

No warranties, express or implied, including, without limitation, warranties of merchantability or fitness for a particular purpose, are given in connection with this publication. Although this information is believed to be accurate by ASM, ASM cannot guarantee that favorable results will be obtained from the use of this publication alone. This publication is intended for use by persons having technical skill, at their sole discretion and risk. Since the conditions of product or material use are outside of ASM's control, ASM assumes no liability or obligation in connection with any use of this information. As with any material, evaluation of the material under end-use conditions prior to specification is essential. Therefore, specific testing under actual conditions is recommended.

Nothing contained in this publication shall be construed as a grant of any right of manufacture, sale, use, or reproduction, in connection with any method, process, apparatus, product, composition, or system, whether or not covered by letters patent, copyright, or trademark, and nothing contained in this publication shall be construed as a defense against any alleged infringement of letters patent, copyright, or trademark, or as a defense against liability for such infringement.