Cover
Sample Preparation Handbook for Transmission Electron Microscopy
Foreword
Preface to the English Edition
About the Authors
Contents
Abbreviations
Chapter 1 Methodology: General Introduction
Chapter 2 Introduction to Materials
Introduction
1.1 Origin of Materials
1.2 Evolution of Materials
1.3 General Problems Presented by Microstructure Investigations
Classification of Materials and Properties
2.1 Types of Chemical Bonds: Atomic and Molecular
2.2 Type of Materials and Chemical Bonds
2.3 Chemical Bonds and Mechanical Properties
2.3.1 Mechanical Properties and Crystallinity
2.3.2 Rigidity: From Hard to Soft
2.3.3 Tensile Strength: Ductility--Brittleness
2.3.4 Mechanical Properties of Organic Materials and Glass Transition ( T g )
Microstructures in Materials Science
3.1 Problems to Be Solved in Materials Science
3.2 Materials Microstructures
3.3 Polymer Microstructures
3.4 Crystalline Defects and Properties of Materials
3.5 Solid-State Polymer Properties
Microstructures in Biological Materials
4.1 Problems to Be Solved in Biology
4.2 Singularity of Biological Materials: Importance of the Liquid Phase
4.3 Microstructure in Biology
4.4 Role of Structures on Functional Properties
Bibliography
Chapter 3 The Different Observation Modes in Electron Microscopy (SEM, TEM, STEM)
Introduction
Signals Used for Electron Microscopy
2.1 Electron--Matter Interaction
2.2 Signals Used for Imaging
2.3 Signals Used for Chemical Analysis
2.4 Signals Used for Structure
2.4.1 Transmitted Electrons: Thin Samples with Thickness 100 nm
Microscopes and Observation Modes
3.1 Illumination Sources
3.1.1 Thermionic Sources
3.1.2 Field Emission Guns (FEGs)
3.2 Illumination Modes and Detection Limits
3.3 Microscope Resolutions and Analysis
3.3.1 Resolution Limit of the TEM
3.3.2 Spatial Resolution
The Different Types of Microscopes: SEM, TEM, and STEM
4.1 Scanning Electron Microscope (SEM)
4.2 Conventional Transmission Electron Microscope (CTEM)
4.3 Analytical TEM/STEM Microscope and ''Dedicated STEM''
Different TEM Observation Modes
5.1 Origin of Contrast
5.1.1 Amplitude Contrast and Phase Contrast
5.2 Diffraction Contrast Imaging Modes in TEM and TEM/STEM
5.3 Chemical Contrast Imaging Modes in TEM and TEM/STEM
5.4 Spectroscopic Contrast Imaging Modes in TEM and TEM/STEM
5.5 EDS Chemical Analysis Methods in TEM and TEM/STEM
5.6 EELS Spectroscopic Analysis Modes in TEM and TEM/STEM
Conclusion and Information Assessment
Bibliography
Chapter 4 Materials Problems and Approaches for TEMand TEM/STEM Analyses
Introduction
Analyses Conducted Prior to TEM Analyses
2.1 Macroscopic Characterization
2.2 Microscopic Characterization
2.3 Microscopic and Nanoscopic Characterization
Approach for Beginning the Investigation of a Material
Selection of the Type of TEM Analysis
Analysis of Topography
Structural Analysis in TEM
6.1 Morphology and Structure of Materials
6.2 Atomic Structure
Crystallographic Analysis
Analysis of Crystal Defects: 1D (Dislocations), 2D (Grain Boundaries and Interfaces), and 3D (Precipitates)
EDS Chemical Analysis and EELS Spectroscopic Analysis
9.1 Phase Identification and Distribution
9.2 Concentration Profiles and Interface Analysis
Structural Analyses Under Special Conditions
10.1 In Situ Analyses
10.1.1 At Room Temperature
10.1.2 At High Temperatures
10.1.3 At Low Temperatures
10.2 Cryomicroscopy
10.2.1 Structure of Isolated Particles from Biological Materials or Polymers
10.2.2 Structure of Bulk Frozen Samples
Study of Properties
11.1 Optical Properties
11.2 Electrical Properties
11.3 Electronic Properties
11.4 Magnetic Properties
11.5 Mechanical Properties
11.6 Chemical Properties
11.7 Functional Properties
Relationship Between Sample Thickness and Analysis Type in TEM and TEM/STEM
Assessment of TEM Analyses
Chapter 5 Physical and Chemical Mechanisms of Preparation Techniques
Introduction
Mechanical Action
2.1 Principles of a Material's Mechanical Behavior
2.2 Abrasion Principle
2.2.1 Techniques Involving Cutting by Means of Mechanical Abrasion: Sawing and Grinding
2.2.2 Abrasive Techniques: Mechanical Polishing, Dimpling, and Tripod Polishing
2.3 Rupture Principles
2.3.1 Techniques Involving Fracture: Crushing, Wedge Cleavage, Ultramicrotomy, and Freeze Fracture
Chemical Action
3.1 Principle of Chemical and Electrochemical Dissolution
3.1.1 Techniques Involving Chemical and Electrochemical Dissolution
Ionic Action
4.1 Ionic Abrasion Principles
4.2 Techniques Involving Ion Abrasion
4.2.1 Ion Beam Thinning and Focused Ion Beam Thinning (FIB)
Actions Resulting in a State Change of Materials Containing an Aqueous Phase
5.1 Elimination of the Aqueous Phase
5.2 Freezing Principles
5.3 Principle of Substitution, Infiltration, and Embedding in Cryogenic Mode
5.4 Cryo-sublimation (or Freeze-Drying) Principle
Actions Resulting in a Change in Material Properties
6.1 Chemical Fixation Principles
6.1.1 Constancy of pH
6.1.2 Molar Concentration
6.1.3 Ionic Concentration
6.2 Dehydration Principles
6.3 Infiltration Principles
6.4 Embedding or Inclusion Principles
6.5 ''Positive-Staining'' Contrast Principles
Physical Actions Resulting in Deposition
7.1 Physical Deposition
7.2 Physics of the Coating Process
7.2.1 Nature of Chemical Elements Used as Sources
7.2.2 Different Methods of Particle Production
7.2.3 Vacuum
7.2.4 Substrate
7.3 Techniques Involving a Physical Deposition: Continuous or Holey Thin Film, Contrast Enhancement by Shadowing or Decoration, Replicas, and Freeze Fracture
7.3.1 Replica Techniques
7.3.2 Contrast Enhancement by Physical Coating: ''Negative-Staining'' Contrast
Bibliography
Mechanical Action
Chemical Action
Ionic Action
Actions Resulting in a State Change of Materials Containing an Aqueous Phase
Actions Resulting in a Change in Material Properties
Physical Actions Resulting in a Deposit
Chapter 6 Artifacts in Transmission Electron Microscopy
Introduction
Preparation-Induced Artifacts
2.1 Mechanical Preparation-Induced Artifacts
2.1.1 Secondary Thermal Damage Induced During Mechanical Preparation
2.2 Ionic Preparation-Induced Artifacts
2.2.1 Secondary Thermal Damage Induced During Ionic Preparation
2.3 Chemical Preparation-Induced Artifacts
2.3.1 Changes Specific to Biological Materials
2.3.2 Secondary Thermal Damage Induced During Chemical Preparation
2.4 Physical Preparation-Induced Artifacts
2.4.1 Secondary Thermal Damage Induced During Physical Preparation
Artifacts Induced During TEM Observation
3.1 Artifacts Not Linked to Thermal Damages
3.2 Secondary Thermal Damage
Examples of Artifacts
4.1 Artifacts Induced by the Tripod Polishing Technique
4.2 Artifacts Induced by the Ultramicrotomy Technique
4.3 Artifacts Induced by the Freeze-Fracture Technique
4.4 Artifacts Induced by Ion Milling or FIB
4.5 Artifacts Induced by the Substitution--Infiltration--Embedding Technique
4.6 Artifacts Induced by Chemical Fixation
4.7 Artifacts Induced by the Extractive-Replica Technique
4.8 Artifacts Induced by the Shadowing Technique
4.9 Artifacts Induced by the ''Positive-Staining'' Contrast Technique
4.10 Artifacts Induced by the Cryofixation Technique
4.11 Artifacts Induced by the Fine Particle Dispersion Technique
4.12 Artifacts Induced by the Frozen-Hydrated-Film Technique
4.13 Artifacts Induced by the ''Negative-Staining'' Contrast Technique
4.14 Artifacts Induced by the Electron Beam
Summary Tables
Bibliography
Chapter 7 Selection of Preparation Techniques Based on Material Problems and TEM Analyses
Introduction
Classification of Preparation Techniques
Characteristics of Preparation Techniques
Criteria Used to Select a Preparation Technique
Selection Criteria Based on Material Type
Selection Criteria Based on Material Organization
6.1 Bulk Materials
6.2 Single-Layer or Multilayer Materials
6.3 Fine Particles
Selection Criteria Based on Material Properties
7.1 Based on the Physical State of the Material
7.2 Based on the Chemical Phases in the Material
7.3 Based on the Electrical Properties of the Material
7.4 Based on the Mechanical Properties of the Material
7.4.1 Materials in Solid-State Physics
7.4.2 Soft-Ductile Materials
7.4.3 Hard-Resistant Materials
7.4.4 Materials of Intermediate Hardness and Ductility
7.4.5 Biological Materials
Selection Criteria Related to the Type of TEM Analysis
8.1 Preparation Techniques
Selection of the Orientation of the Sample Section
9.1 Microstructure Geometry
9.2 Defect Geometry
Selection Criteria Related to Artifacts Induced by the Preparation Technique
Adaptation of the Technique Based on Problems Related to Observation
11.1 Reducing Sample Thickness
11.2 Increasing Contrast
11.3 Reducing Charge Effects
11.4 Limitation of Strain Hardening
11.5 Removal of Surface Amorphization
11.6 Removal of Surface Contamination
11.7 Final Cleaning of the Thin Slice
Conclusion
Bibliography
Chapter 8 Comparisons of Techniques
Introduction
Examples Using Fine Particle Materials
2.1 Comparison of Mechanical Preparations and Replicas
2.1.1 Crushing Technique (0Techniques0 Chapter 4 , Section 1 ) and Extractive Replica Technique (0Techniques0 Chapter 5 , Section 3 )
2.1.2 Crushing Technique (0Techniques0 Chapter 4 , Section 1 ) and Extractive Replica Technique (0Techniques0 Chapter 5 , Section 3 )
2.2 Comparison of ''Negative-Staining'' Contrast and Freeze-Fracture Techniques
2.2.1 Negative-Staining (0Techniques0 Chapter 7 , Section 2 ) and Freeze-Fracture Techniques (0Techniques0 Chapter 5 , Section 4)
2.3 Comparison of ''Negative-Staining'' and Decoration-Shadowing Contrast Techniques
2.3.1 Negative-Staining Contrast (0Techniques0 Chapter 7 , Section 2 ) and Decoration-Shadowing (0Techniques0 Chapter 7 , Section 1 ) Techniques
2.3.2 Negative-Staining (0Techniques0 Chapter 7 , Section 2 ) and Decoration-Shadowing (0Techniques0 Chapter 7 , Section 1 ) Contrast Techniques
2.4 Comparison of ''Positive-Staining'' and Decoration-Shadowing Contrast Techniques
2.4.1 Positive-Staining (0Techniques0 Chapter 7 , Section 2 ) and Decoration-Shadowing (0Techniques0 Chapter 7 , Section 1 ) Contrast Techniques
Examples Using Bulk or Multilayer Materials
3.1 Comparison Between Different Mechanical Preparations
3.1.0 Wedge Cleavage Technique (0Techniques0 Chapter 4 , Section 2 ) and Tripod Polishing Technique (0Techniques0 Chapter 5 , Section 3 )
3.2 Comparison Between Mechanical Preparations and Ionic Preparations
3.2.1 Comparison of ''Cleaved Wedge'' and ''Ionic Thinning'' Techniques
3.2.2 Comparison of ''Tripod Polishing + Ions'' and ''FIB Thinning''
3.2.3 Comparison of ''Ultramicrotomy'' and ''Ion Milling'' Techniques
3.2.4 Comparison of ''Tripod Polishing,'' ''Ion Milling,'' and ''FIB Thinning'' Techniques
3.2.5 Comparison of ''Tripod Polishing'' and ''Tripod Polishing + Ion Milling'' Techniques
3.2.6 Comparison of ''Tripod Polishing'' and ''Ion Milling'' Techniques
3.3 Comparison Between Mechanical Preparations and Electrolytic Preparations
3.3.0 Electrolytic Thinning Techniques (0Techniques0 Chapter 3 , Section 1 ), Tripod Polishing Technique + Ion Milling Technique (0Techniques0 Chapter 4 , Section 3 ; 0Techniques0 Chapter 3 , Section 5), and Ultramicrotomy Technique (0Techniques0 Chapter 4 , Section 4)
3.4 Comparison Between Techniques Specific to Biology
3.4.1 Comparison of ''Chemical Methods,'' ''Physical Methods,'' and ''Freeze-Fracture'' Techniques
3.4.2 Comparison of ''Chemical Methods,'' ''Physical Methods,'' and ''Freeze-Fracture'' Techniques
3.4.3 Comparison of ''Chemical Fixation,'' ''Cryo-embedding,'' and ''Immunolabeling'' Techniques
3.4.4 Comparison of ''Immunolabeling,'' ''Ultramicrotomy,'' and ''Cryo-ultramicrotomy'' Techniques
3.5 Comparison Between All Techniques That Can Be Used in Biology on One Example: Collagen
3.5.1 Comparison of ''Negative-Staining Contrast'' and ''Immunolabeling techiques''
3.5.2 Comparison of ''Negative-Staining'' and ''Decoration-Shadowing'' Contrast, and ''Freeze-Fracture'' Techniques
3.5.3 Comparison of ''Chemical Fixation,'' ''Physical Fixation,'' and ''Cryo-embedding'' Techniques
Bibliography
Chapter 9 Conclusion: What Is a Good Sample?
Photo Credits
Index