Microstructural Characterization of Materials

Transcription

1 Microstructural Characterization of Materials 2nd Edition DAVID BRANDON AND WAYNE D. KAPLAN Technion, Israel Institute of Technology, Israel John Wiley & Sons, Ltd

2 Contents Preface to the Second Edition Preface to the First Edition 1 The Concept of Microstructure Microstructural Features Structure-Property Relationships Microstructural Scale Microstructural Parameters Crystallography and Crystal Structure Interatomic Bonding in Solids Crystalline and Amorphous Phases The Crystal Lattice 30 Summary 42 Bibliography 46 Worked Examples 46 Problems 51 2 Diffraction Analysis of Crystal Structure Scattering of Radiation by Crystals The Laue Equations and Bragg's Law Allowed and Forbidden Reflections Reciprocal Space The Limiting Sphere Construction Vector Representation of Bragg's Law The Reciprocal Lattice X-Ray Diffraction Methods The X-Ray Diffractometer Powder Diffraction-Particles and Polycrystals Single Crystal Laue Diffraction Rotating Single Crystal Methods Diffraction Analysis Atomic Scattering Factors Scattering by the Unit Cell The Structure Factor in the Complex Plane Interpretation of Diffracted Intensities Errors and Assumptions Electron Diffraction Wave Properties of Electrons 91 xi xiii

3 Contents Ring Patterns, Spot Patterns and Laue Zones Kikuchi Patterns and Their Interpretation Summary Bibliography Worked Examples Problems Optical Microscopy 3.1 Geometrical Optics Optical Image Formation Resolution in the Optical Microscope Depth of Field and Depth of Focus 3.2 Construction of The Microscope Light Sources and Condenser Systems The Specimen Stage Selection of Objective Lenses Image Observation and Recording 3.3 Specimen Preparation Sampling and Sectioning Mounting and Grinding Polishing and Etching Methods 3.4 Image Contrast Reflection and Absorption of Light Bright-Field and Dark-Field Image Contrast Confocal Microscopy Interference Contrast and Interference Microscopy Optical Anisotropy and Polarized Light Phase Contrast Microscopy 3.5 Working with Digital Images Data Collection and The Optical System Data Processing and Analysis Data Storage and Presentation Dynamic Range and Digital Storage 3.6 Resolution, Contrast and Image Interpretation Summary Bibliography Worked Examples Problems Transmission Electron Microscopy 4.1 Basic Principles Wave Properties of Electrons Resolution Limitations and Lens Aberrations Comparative Performance of Transmission and Scannin Electron Microscopy

4 Contents vii 4.2 Specimen Preparation Mechanical Thinning Electrochemical Thinning Ion Milling Sputter Coating and Carbon Coating Replica Methods The Origin of Contrast Mass-Thickness Contrast Diffraction Contrast and Crystal Lattice Defects Phase Contrast and Lattice Imaging Kinematic Interpretation of Diffraction Contrast Kinematic Theory of Electron Diffraction The Amplitude-Phase Diagram Contrast From Lattice Defects Stacking Faults and Anti-Phase Boundaries Edge and Screw Dislocations Point Dilatations and Coherency Strains Dynamic Diffraction and Absorption Effects Stacking Faults Revisited Quantitative Analysis of Contrast Lattice Imaging at High Resolution The Lattice Image and the Contrast Transfer Function Computer Simulation of Lattice Images Lattice Image Interpretation Scanning Transmission Electron Microscopy 234 Summary 236 Bibliography 238 Worked Examples 238 Problems 247 Scanning Electron Microscopy Components of The Scanning Electron Microscope Electron Beam-Specimen Interactions Beam-Focusing Conditions Inelastic Scattering and Energy Losses Electron Excitation of X-Rays Characteristic X-Ray Images Backscattered Electrons Image Contrast in Backscattered Electron Images Secondary Electron Emission Factors Affecting Secondary Electron Emission Secondary Electron Image Contrast Alternative Imaging Modes Cathodoluminescence Electron Beam Induced Current Orientation Imaging Microscopy 289

5 viii Contents Electron Backscattered Diffraction Patterns OIM Resolution and Sensitivity Localized Preferred Orientation and Residual Stress Specimen Preparation and Topology Sputter Coating and Contrast Enhancement Fractography and Failure Analysis Stereoscopic Imaging Parallax Measurements Focused Ion Beam Microscopy Principles of Operation and Microscope Construction Ion Beam-Specimen Interactions Dual-Beam FIB Systems Machining and Deposition TEM Specimen Preparation Serial Sectioning 314 Summary 315 Bibliography 318 Worked Examples 318 Problems Microanalysis in Electron Microscopy X-Ray Microanalysis Excitation of Characteristic X-Rays Detection of Characteristic X-Rays Quantitative Analysis of Composition Electron Energy Loss Spectroscopy The Electron Energy-Loss Spectrum Limits of Detection and Resolution in EELS Quantitative Electron Energy Loss Analysis Near-Edge Fine Structure Information Far-Edge Fine Structure Information Energy-Filtered Transmission Electron Microscopy 367 Summary 370 Bibliography 375 Worked Examples 375 Problems Scanning Probe Microscopy and Related Techniques Surface Forces and Surface Morphology Surface Forces and Their Origin Surface Force Measurements Surface Morphology: Atomic and Lattice Resolution Scanning Probe Microscopes Atomic Force Microscopy Scanning Tunnelling Microscopy Field-Ion Microscopy and Atom Probe Tomography 413

6 Contents ix Identifying Atoms by Field Evaporation The Atom Probe and Atom Probe Tomography 416 Summary 417 Bibliography 420 Problems Chemical Analysis of Surface Composition X-Ray Photoelectron Spectroscopy Depth Discrimination Chemical Binding States Instrumental Requirements Applications Auger Electron Spectroscopy Spatial Resolution and Depth Discrimination Recording and Presentation of Spectra Identification of Chemical Binding States Quantitative Auger Analysis Depth Profiling Auger Imaging Secondary-Ion Mass Spectrometry Sensitivity and Resolution Calibration and Quantitative Analysis SIMS Imaging 445 Summary 446 Bibliography 448 Worked Examples 448 Problems Quantitative and Tomographie Analysis of Microstrueture Basic Stereological Concepts Isotropy and Anisotropy Homogeneity and Inhomogeneity Sampling and Sectioning Statistics and Probability Accessible and Inaccessible Parameters Accessible Parameters Inaccessible Parameters Optimizing Accuracy Sample Size and Counting Time Resolution and Detection Errors Sample Thickness Corrections Observer Bias Dislocation Density Revisited Automated Image Analysis Digital Image Recording Statistical Significance and Microstructural Relevance 495

7 x Contents 9.5 Tomography and Three-Dimensional Reconstruction Presentation of Tomographie Data Methods of Serial Sectioning Three-Dimensional Reconstruction 499 Summary 500 Bibliography 503 Worked Examples 503 Problems 514 Appendices 517 Appendix 1: Useful Equations 517 Interplanar Spacings 517 Unit Cell Volumes 518 Interplanar Angles 518 Direction Perpendicular to a Crystal Plane 519 Hexagonal Unit Cells 520. The Zone Axis of Two Planes in the Hexagonal System 521 Appendix 2: Wavelengths 521 Relativistic Electron Wavelengths 521 X-Ray Wavelengths for Typical X-Ray Sources 521 Index 523