Ayache / Beaunier / Boumendil Sample Preparation Handbook for Transmission Electron Microscopy

Methodology
1. Auflage 2010
ISBN: 978-0-387-98182-6
Verlag: Springer
Format: PDF
Kopierschutz: 1 - PDF Watermark

E-Book, Englisch, 250 Seiten

Successful transmission electron microscopy in all of its manifestations depends on the quality of the specimens examined. Biological specimen preparation protocols have usually been more rigorous and time consuming than those in the physical sciences. For this reason, there has been a wealth of scienti?c literature detailing speci?c preparation steps and numerous excellent books on the preparation of b- logical thin specimens. This does not mean to imply that physical science specimen preparation is trivial. For the most part, most physical science thin specimen pre- ration protocols can be executed in a matter of a few hours using straightforward steps. Over the years, there has been a steady stream of papers written on various aspects of preparing thin specimens from bulk materials. However, aside from s- eral seminal textbooks and a series of book compilations produced by the Material Research Society in the 1990s, no recent comprehensive books on thin spe- men preparation have appeared until this present work, ?rst in French and now in English. Everyone knows that the data needed to solve a problem quickly are more imp- tant than ever. A modern TEM laboratory with supporting SEMs, light microscopes, analytical spectrometers, computers, and specimen preparation equipment is an investment of several million US dollars. Fifty years ago, electropolishing, chemical polishing, and replication methods were the principal specimen preparation me- ods.

Autoren/Hrsg.

Ayache, Jeanne

Beaunier, Luc

Boumendil, Jacqueline

Ehret, Gabrielle

Laub, Danièle

Inhaltsverzeichnis

1;Foreword;6
2;Preface to the English Edition;10
3;About the Authors;13
4;Contents;15
5;Abbreviations;21
6;1 Methodology: General Introduction;22
7;2 Introduction to Materials;24
7.1; Introduction;24
7.1.1;1.1 Origin of Materials;24
7.1.2;1.2 Evolution of Materials;24
7.1.3;1.3 General Problems Presented by Microstructure Investigations;25
7.2; Classification of Materials and Properties;27
7.2.1;2.1 Types of Chemical Bonds: Atomic and Molecular;27
7.2.2;2.2 Type of Materials and Chemical Bonds;29
7.2.3;2.3 Chemical Bonds and Mechanical Properties;29
7.2.3.1;2.3.1 Mechanical Properties and Crystallinity;30
7.2.3.2;2.3.2 Rigidity: From Hard to Soft;31
7.2.3.3;2.3.3 Tensile Strength: Ductility--Brittleness;31
7.2.3.4;2.3.4 Mechanical Properties of Organic Materials and Glass Transition (Tg);33
7.3; Microstructures in Materials Science;34
7.3.1;3.1 Problems to Be Solved in Materials Science;34
7.3.2;3.2 Materials Microstructures;35
7.3.3;3.3 Polymer Microstructures;39
7.3.4;3.4 Crystalline Defects and Properties of Materials;40
7.3.5;3.5 Solid-State Polymer Properties;44
7.4; Microstructures in Biological Materials;45
7.4.1;4.1 Problems to Be Solved in Biology;45
7.4.2;4.2 Singularity of Biological Materials: Importance of the Liquid Phase;47
7.4.3;4.3 Microstructure in Biology;48
7.4.4;4.4 Role of Structures on Functional Properties;51
7.5; Bibliography;51
8;3 The Different Observation Modes in Electron Microscopy (SEM, TEM, STEM);53
8.1; Introduction;53
8.2; Signals Used for Electron Microscopy;53
8.2.1;2.1 Electron--Matter Interaction;53
8.2.2;2.2 Signals Used for Imaging;55
8.2.3;2.3 Signals Used for Chemical Analysis;56
8.2.4;2.4 Signals Used for Structure;57
8.2.4.1;2.4.1 Transmitted Electrons: Thin Samples with Thickness 100 nm;57
8.3; Microscopes and Observation Modes;57
8.3.1;3.1 Illumination Sources;57
8.3.1.1;3.1.1 Thermionic Sources;58
8.3.1.2;3.1.2 Field Emission Guns (FEGs);58
8.3.2;3.2 Illumination Modes and Detection Limits;59
8.3.3;3.3 Microscope Resolutions and Analysis;59
8.3.3.1;3.3.1 Resolution Limit of the TEM;59
8.3.3.2;3.3.2 Spatial Resolution;60
8.4; The Different Types of Microscopes: SEM, TEM, and STEM;61
8.4.1;4.1 Scanning Electron Microscope (SEM);61
8.4.2;4.2 Conventional Transmission Electron Microscope (CTEM);61
8.4.3;4.3 Analytical TEM/STEM Microscope and ''Dedicated STEM'';64
8.5; Different TEM Observation Modes;66
8.5.1;5.1 Origin of Contrast;66
8.5.1.1;5.1.1 Amplitude Contrast and Phase Contrast;67
8.5.2;5.2 Diffraction Contrast Imaging Modes in TEM and TEM/STEM;68
8.5.3;5.3 Chemical Contrast Imaging Modes in TEM and TEM/STEM;69
8.5.4;5.4 Spectroscopic Contrast Imaging Modes in TEM and TEM/STEM;70
8.5.5;5.5 EDS Chemical Analysis Methods in TEM and TEM/STEM;71
8.5.6;5.6 EELS Spectroscopic Analysis Modes in TEM and TEM/STEM;72
8.6; Conclusion and Information Assessment;72
8.7; Bibliography;74
9;4 Materials Problems and Approaches for TEM and TEM/STEM Analyses;76
9.1; Introduction;76
9.2; Analyses Conducted Prior to TEM Analyses;76
9.2.1;2.1 Macroscopic Characterization;78
9.2.2;2.2 Microscopic Characterization;78
9.2.3;2.3 Microscopic and Nanoscopic Characterization;79
9.3; Approach for Beginning the Investigation of a Material;80
9.4; Selection of the Type of TEM Analysis;82
9.5; Analysis of Topography;82
9.6; Structural Analysis in TEM;83
9.6.1;6.1 Morphology and Structure of Materials;83
9.6.2;6.2 Atomic Structure;87
9.7; Crystallographic Analysis;89
9.8; Analysis of Crystal Defects: 1D (Dislocations), 2D (Grain Boundaries and Interfaces), and 3D (Precipitates);91
9.9; EDS Chemical Analysis and EELS Spectroscopic Analysis;92
9.9.1;9.1 Phase Identification and Distribution;92
9.9.2;9.2 Concentration Profiles and Interface Analysis;93
9.10; Structural Analyses Under Special Conditions;94
9.10.1;10.1 In Situ Analyses;94
9.10.1.1;10.1.1 At Room Temperature;94
9.10.1.2;10.1.2 At High Temperatures;94
9.10.1.3;10.1.3 At Low Temperatures;95
9.10.2;10.2 Cryomicroscopy;95
9.10.2.1;10.2.1 Structure of Isolated Particles from Biological Materials or Polymers;95
9.10.2.2;10.2.2 Structure of Bulk Frozen Samples;96
9.11; Study of Properties;96
9.11.1;11.1 Optical Properties;96
9.11.2;11.2 Electrical Properties;96
9.11.3;11.3 Electronic Properties;96
9.11.4;11.4 Magnetic Properties;97
9.11.5;11.5 Mechanical Properties;97
9.11.6;11.6 Chemical Properties;97
9.11.7;11.7 Functional Properties;97
9.12; Relationship Between Sample Thickness and Analysis Type in TEM and TEM/STEM;100
9.13; Assessment of TEM Analyses;100
10;5 Physical and Chemical Mechanisms of Preparation Techniques;101
10.1; Introduction;101
10.2; Mechanical Action;102
10.2.1;2.1 Principles of a Material's Mechanical Behavior;102
10.2.2;2.2 Abrasion Principle;103
10.2.2.1;2.2.1 Techniques Involving Cutting by Means of Mechanical Abrasion: Sawing and Grinding;104
10.2.2.2;2.2.2 Abrasive Techniques: Mechanical Polishing, Dimpling, and Tripod Polishing;104
10.2.3;2.3 Rupture Principles;105
10.2.3.1;2.3.1 Techniques Involving Fracture: Crushing, Wedge Cleavage, Ultramicrotomy, and Freeze Fracture;105
10.3; Chemical Action;108
10.3.1;3.1 Principle of Chemical and Electrochemical Dissolution;108
10.3.1.1;3.1.1 Techniques Involving Chemical and Electrochemical Dissolution;110
10.4; Ionic Action;111
10.4.1;4.1 Ionic Abrasion Principles;111
10.4.2;4.2 Techniques Involving Ion Abrasion;112
10.4.2.1;4.2.1 Ion Beam Thinning and Focused Ion Beam Thinning (FIB);112
10.5; Actions Resulting in a State Change of Materials Containing an Aqueous Phase;116
10.5.1;5.1 Elimination of the Aqueous Phase;116
10.5.2;5.2 Freezing Principles;118
10.5.3;5.3 Principle of Substitution, Infiltration, and Embedding in Cryogenic Mode;120
10.5.4;5.4 Cryo-sublimation (or Freeze-Drying) Principle;121
10.6; Actions Resulting in a Change in Material Properties;121
10.6.1;6.1 Chemical Fixation Principles;122
10.6.1.1;6.1.1 Constancy of pH;123
10.6.1.2;6.1.2 Molar Concentration;124
10.6.1.3;6.1.3 Ionic Concentration;124
10.6.2;6.2 Dehydration Principles;126
10.6.3;6.3 Infiltration Principles;126
10.6.4;6.4 Embedding or Inclusion Principles;128
10.6.5;6.5 ''Positive-Staining'' Contrast Principles;129
10.7; Physical Actions Resulting in Deposition;130
10.7.1;7.1 Physical Deposition;130
10.7.2;7.2 Physics of the Coating Process;131
10.7.2.1;7.2.1 Nature of Chemical Elements Used as Sources;132
10.7.2.2;7.2.2 Different Methods of Particle Production;133
10.7.2.3;7.2.3 Vacuum;137
10.7.2.4;7.2.4 Substrate;137
10.7.3;7.3 Techniques Involving a Physical Deposition: Continuous or Holey Thin Film, Contrast Enhancement by Shadowing or Decoration, Replicas, and Freeze Fracture;137
10.7.3.1;7.3.1 Replica Techniques;138
10.7.3.2;7.3.2 Contrast Enhancement by Physical Coating: ''Negative-Staining'' Contrast;138
10.8; Bibliography;140
10.8.1;Mechanical Action;140
10.8.2;Chemical Action;140
10.8.3;Ionic Action;140
10.8.4;Actions Resulting in a State Change of Materials Containing an Aqueous Phase ;140
10.8.5;Actions Resulting in a Change in Material Properties;141
10.8.6;Physical Actions Resulting in a Deposit;141
11;6 Artifacts in Transmission Electron Microscopy;142
11.1; Introduction;142
11.2; Preparation-Induced Artifacts;142
11.2.1;2.1 Mechanical Preparation-Induced Artifacts;144
11.2.1.1;2.1.1 Secondary Thermal Damage Induced During Mechanical Preparation;146
11.2.2;2.2 Ionic Preparation-Induced Artifacts;147
11.2.2.1;2.2.1 Secondary Thermal Damage Induced During Ionic Preparation;148
11.2.3;2.3 Chemical Preparation-Induced Artifacts;148
11.2.3.1;2.3.1 Changes Specific to Biological Materials;149
11.2.3.2;2.3.2 Secondary Thermal Damage Induced During Chemical Preparation;150
11.2.4;2.4 Physical Preparation-Induced Artifacts;151
11.2.4.1;2.4.1 Secondary Thermal Damage Induced During Physical Preparation;151
11.3; Artifacts Induced During TEM Observation;152
11.3.1;3.1 Artifacts Not Linked to Thermal Damages;152
11.3.2;3.2 Secondary Thermal Damage;154
11.4; Examples of Artifacts;154
11.4.1;4.1 Artifacts Induced by the Tripod Polishing Technique;154
11.4.2;4.2 Artifacts Induced by the Ultramicrotomy Technique;157
11.4.3;4.3 Artifacts Induced by the Freeze-Fracture Technique;164
11.4.4;4.4 Artifacts Induced by Ion Milling or FIB;165
11.4.5;4.5 Artifacts Induced by the Substitution--Infiltration--Embedding Technique;171
11.4.6;4.6 Artifacts Induced by Chemical Fixation;171
11.4.7;4.7 Artifacts Induced by the Extractive-Replica Technique;172
11.4.8;4.8 Artifacts Induced by the Shadowing Technique;173
11.4.9;4.9 Artifacts Induced by the ''Positive-Staining'' Contrast Technique;174
11.4.10;4.10 Artifacts Induced by the Cryofixation Technique;175
11.4.11;4.11 Artifacts Induced by the Fine Particle Dispersion Technique;176
11.4.12;4.12 Artifacts Induced by the Frozen-Hydrated-Film Technique;178
11.4.13;4.13 Artifacts Induced by the ''Negative-Staining'' Contrast Technique;180
11.4.14;4.14 Artifacts Induced by the Electron Beam;181
11.5; Summary Tables;185
11.6; Bibliography;186
12;7 Selection of Preparation Techniques Based on Material Problems and TEM Analyses;188
12.1; Introduction;188
12.2; Classification of Preparation Techniques;188
12.3; Characteristics of Preparation Techniques;189
12.4; Criteria Used to Select a Preparation Technique;190
12.5; Selection Criteria Based on Material Type;190
12.6; Selection Criteria Based on Material Organization;193
12.6.1;6.1 Bulk Materials;193
12.6.2;6.2 Single-Layer or Multilayer Materials;193
12.6.3;6.3 Fine Particles;194
12.7; Selection Criteria Based on Material Properties;194
12.7.1;7.1 Based on the Physical State of the Material;194
12.7.2;7.2 Based on the Chemical Phases in the Material;194
12.7.3;7.3 Based on the Electrical Properties of the Material;195
12.7.4;7.4 Based on the Mechanical Properties of the Material;195
12.7.4.1;7.4.1 Materials in Solid-State Physics;195
12.7.4.2;7.4.2 Soft-Ductile Materials;196
12.7.4.3;7.4.3 Hard-Resistant Materials;196
12.7.4.4;7.4.4 Materials of Intermediate Hardness and Ductility;196
12.7.4.5;7.4.5 Biological Materials;197
12.8; Selection Criteria Related to the Type of TEM Analysis;198
12.8.1;8.1 Preparation Techniques;199
12.9; Selection of the Orientation of the Sample Section;200
12.9.1;9.1 Microstructure Geometry;204
12.9.2;9.2 Defect Geometry;206
12.10; Selection Criteria Related to Artifacts Induced by the Preparation Technique;206
12.11; Adaptation of the Technique Based on Problems Related to Observation;208
12.11.1;11.1 Reducing Sample Thickness;208
12.11.2;11.2 Increasing Contrast;209
12.11.3;11.3 Reducing Charge Effects;209
12.11.4;11.4 Limitation of Strain Hardening;209
12.11.5;11.5 Removal of Surface Amorphization;209
12.11.6;11.6 Removal of Surface Contamination;209
12.11.7;11.7 Final Cleaning of the Thin Slice;210
12.12; Conclusion;210
12.13; Bibliography;214
13;8 Comparisons of Techniques;215
13.1; Introduction;215
13.2; Examples Using Fine Particle Materials;215
13.2.1;2.1 Comparison of Mechanical Preparations and Replicas;215
13.2.2;2.2 Comparison of ''Negative-Staining'' Contrast and Freeze-Fracture Techniques;218
13.2.3;2.3 Comparison of ''Negative-Staining'' and Decoration-Shadowing Contrast Techniques;219
13.2.4;2.4 Comparison of ''Positive-Staining'' and Decoration-Shadowing Contrast Techniques;222
13.3; Examples Using Bulk or Multilayer Materials;223
13.3.1;3.1 Comparison Between Different Mechanical Preparations;223
13.3.2;3.2 Comparison Between Mechanical Preparations and Ionic Preparations;225
13.3.3;3.3 Comparison Between Mechanical Preparations and Electrolytic Preparations;236
13.3.4;3.4 Comparison Between Techniques Specific to Biology;238
13.3.5;3.5 Comparison Between All Techniques That Can Be Used in Biology on One Example: Collagen;245
13.4; Bibliography;249
14;9 Conclusion: What Is a Good Sample?;251
15;Photo Credits;253
16;Index;255