1、MANUAL ON ELECTRON METALLOGRAPHY TECHNIQUES Sponsored by Subcommittee E04.1 1 on Electron Microscopy and Diffraction of Committee E-4 on Metallography AMERICAN SOCIETY FOR TESTING AND MATERIALS ASTM SPECIAL TECHNICAL PUBLICATION 547 G.N.Maniar and Albert Szirmae,coordinators List price$5.25 04-54700
2、0-28 l AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race Street,Philadelphia,Pa.19103 Copyright by ASTM Intl(all rights reserved);Fri Nov 27 12:21:57 EST 2015Downloaded/printed byUniversity of Washington(University of Washington)pursuant to License Agreement.No further reproductions authorized.?9
3、 by American Society for Testing and Materials 1973 Library of Congress Catalog Card Number:73-84362 NOTE The Society is not responsible,as a body,for the statements and opinions advanced in this publication.Printed in Baltimore,Md.October 1973 Copyright by ASTM Intl(all rights reserved);Fri Nov 27
4、12:21:57 EST 2015Downloaded/printed byUniversity of Washington(University of Washington)pursuant to License Agreement.No further reproductions authorized.Foreword The Manual on Electron Metallography Techniques was sponsored and compiled by Subcommittee E04.11 on Electron Microscopy and Diffraction
5、of Committee E4 on Metallography,American Society for Testing and Materials.Subcommittee E04.11 officers are G.N.Maniar,chairman,and Albert Szirmae,secretary.Copyright by ASTM Intl(all rights reserved);Fri Nov 27 12:21:57 EST 2015Downloaded/printed byUniversity of Washington(University of Washington
6、)pursuant to License Agreement.No further reproductions authorized.Related ASTM Publications Applications of Modern Metallographic Techniques,STP 480(1970),$17.00(04-480000-28)Application of Electron M icrofractography to Materials Research,STP 493(1971),$8.25(04-493000-30)Stereology and Quantitativ
7、e Metallography,STP 504(1972),$9.75(04-504000-28)Copyright by ASTM Intl(all rights reserved);Fri Nov 27 12:21:57 EST 2015Downloaded/printed byUniversity of Washington(University of Washington)pursuant to License Agreement.No further reproductions authorized.Contents Introduction Chapter 1-Procedures
8、 for Standard Replication Techniques for Elec-tron Microscopy 1.1 Introduction 1.2 Specimen Preparation for Replication 1.2.1 Mounting 1.2.2 Polishing 1.2.3 Etching 1.3 Replication 1.3.1 Direct Methods 1.3.2 Indirect Methods 1.3.3 Fracture Replication 1.4 Summary References Chapter 2-Extraction Repl
9、ica Techniques 2.1 Introduction 2.2 General Methods 2.2.1 Direct Stripped Plastic Extraction Replicas 2.2.2 Indirect Stripped Plastic Extraction Replicas 2.2.3 Positive Carbon Extraction Replica 2.2.4 Direct Carbon Extraction Replica 2.2.5 Extraction Replicas Removed by Two Stage Etching 2.2.6 Repli
10、cation of Thin Surface Films 2.2.7 Aluminum Oxide Extraction Replica 2.3 Tables of Extraction Replica Techniques 2.4 Bibliography References Chapter 3-Thin Foil Preparation for Transmission Electron Microscopy 3.1 Introduction 3.2 Bulk Thinning to 500 tam(0.5 mm)3.2.1 Cutoff Wheel 3.2.2 Spark Machin
11、ing 3.2.3 Electrolytic Acid Saw and Acid Planing Wheel 3.3 Prethinning to 50 tam(0.05 mm)3.3.1 Surface Grinding and Hand Grinding 3.3.2 Cold Rolling 3.3.3 Chemical Prethinning 3.3.4 Electrolytic and Jet Prethinning 1 3 3 3 3 4 5 6 6 13 15 17 18 19 19 19 20 20 21 22 22 22 23 24 24 24 29 29 29 29 30 3
12、0 30 30 31 31 31 Copyright by ASTM Intl(all rights reserved);Fri Nov 27 12:21:57 EST 2015Downloaded/printed byUniversity of Washington(University of Washington)pursuant to License Agreement.No further reproductions authorized.3.4 Final Thinning to Less Than 0.5/m 3.4.1 Bollmann Method 3.4.2 Window M
13、ethod 3.4.3 Disa Electropol Polishing 3.4.4 Chemical Polishing 3.4.5 Electrolytic and Automatic Jet Polishing 3.5 Unique Thinning Techniques 3.5.1 Small Diameter Wires 3.5.2 Microtomy 3.5.3 Ion Micro Milling 3.6 General Precautions 3.6.1 Mixing Electrolytes 3.6.2 Polishing Film and Staining 3.6.3 El
14、ectrolyte and Specimen Temperature 3.6.4 Cutting and Mounting 3.7 Summary 3.8 Acknowledgments Appendix 3.1 Appendix 3.2 References Chapter 4-Selected Area Electron Diffraction Analysis of Extraction Replica and Thin Foil Specimens in the Transmission Electron Microscope 4.1 Introduction Part I-Parti
15、cle or Second Phase Identification Using Extraction Replica and Selected Area Electron Diffraction 4.2 Introduction 4.3 Technique for Preparing Extraction Replicas 4.4 Indexing Selected Area Electron Diffraction Patterns 4.4.1 Calibration of the Microscope Constant 4.4.2 Identification of Unknown Di
16、ffraction Patterns 4.4.3 Indexing Simple Single Particle Spot Patterns 4.5 Summary Part II-Analysis of Crystallographic Features and Defects in Thin Foil Specimens 4.6 Introduction 4.7 Steps in the Solution of a Selected Area Spot Electron Dif-fraction Pattern of a Thin Foil Specimen Appendix 4.1 Appendix 4.2 Appendix 4.3 Appendix 4.4 References 31 31 32 33 33 33 34 34 34 34 35 35 35 35 36 36 37 37 37 39 41 41 42 42 42 43 43 45 45 50 51 51 52 60 61 62 68 72 vi Copyright by ASTM Intl(all rights r
