Microstructural Characterization of Materials

by Brandon, David; Kaplan, Wayne D.

• ISBN13: 9780470027851
• ISBN10: 0470027851
• Edition: 2nd
• Format: Paperback
• Copyright: 2008-06-03
• Publisher: WILEY

Summary

Microstructural characterization is usually achieved by allowing some form of probe to interact with a carefully prepared specimen. The most commonly used probes are visible light, X-ray radiation, a high-energy electron beam, or a sharp, flexible needle. These four types of probe form the basis for optical microscopy, X-ray diffraction, electron microscopy, and scanning probe microscopy. Microstructural Characterization of Materials, 2nd Edition is an introduction to the expertise involved in assessing the microstructure of engineering materials and to the experimental methods used for this purpose. Similar to the first edition, this 2nd edition explores the methodology of materials characterization under the three headings of crystal structure, microstructural morphology, and microanalysis. The principal methods of characterization, including diffraction analysis, optical microscopy, electron microscopy, and chemical microanalytical techniques are treated both qualitatively and quantitatively. An additional chapter has been added to the new edition to cover surface probe microscopy, and there are new sections on digital image recording and analysis, orientation imaging microscopy, focused ion-beam instruments, atom-probe microscopy, and 3-D image reconstruction. As well as being fully updated, this second edition also includes revised and expanded examples and exercises, with a solutions manual available at http://develop.wiley.co.uk/microstructural2e/ Microstructural Characterization of Materials, 2nd Edition will appeal to senior undergraduate and graduate students of material science, materials engineering, and materials chemistry, as well as to qualified engineers and more advanced researchers, who will find the book a useful and comprehensive general reference source.

Author Biography

David Brandon, Israel Institute of Technology, Haifa, Israel, is the author of Microstructural Characterization of Materials, 2nd Edition, published by Wiley.

Wayne D. Kaplan, Israel Institute of Technology, Haifa, Israel, is the author of Microstructural Characterization of Materials, 2nd Edition, published by Wiley.

Table of Contents

Preface to the Second Edition	p. xi
Preface to the First Edition	p. xiii
The Concept of Microstructure	p. 1
Microstructural Features	p. 7
Struture-Property Relationships	p. 7
Microstructural Scale	p. 10
Microstructural Parameters	p. 19
Crystallography and Crystal Structure	p. 24
Interatomic Bonding in Solids	p. 25
Crystalline and Amorphous Phases	p. 30
The Crystal Lattice	p. 30
Summary	p. 46
Bibliography	p. 46
Worked Examples	p. 46
Problems	p. 51
Diffraction Analysis of Crystal Structure	p. 55
Scattering of Radiation by Crystals	p. 56
The Laue Equations and Bragg's Law	p. 56
Allowed and Forbidden Reflections	p. 59
Reciprocal Space	p. 60
The Limiting Sphere Construction	p. 60
Vector Representation of Bragg's Law	p. 61
The Reciprocal Lattice	p. 61
X-Ray Diffraction Methods	p. 63
The X-Ray Diffractometer	p. 67
Powder Diffraction-Particles and Polycrystals	p. 73
Single Crystal Laue Diffraction	p. 76
Rotating Single Crystal Methods	p. 78
Diffraction Analysis	p. 79
Atomic Scattering Factors	p. 80
Scattering by the Unit Cell	p. 81
The Structure Factor in the Complex Plane	p. 83
Interpretation of Diffracted Intensities	p. 84
Errors and Assumptions	p. 85
Electron Diffraction	p. 90
Wave Properties of Electrons	p. 91
Ring Patterns, Spot Patterns and Laue Zones	p. 94
Kikuchi Patterns and Their Interpretation	p. 96
Summary	p. 98
Bibliography	p. 103
Worked Examples	p. 103
Problems	p. 114
Optical Microscopy	p. 123
Geometrical Optics	p. 125
Optical Image Formation	p. 125
Resolution in the Optical Microscope	p. 130
Depth of Field and Depth of Focus	p. 133
Construction of The Microscope	p. 134
Light Sources and Condenser Systems	p. 134
The Specimen Stage	p. 136
Selection of Objective Lenses	p. 136
Image Observation and Recording	p. 139
Specimen Preparation	p. 143
Sampling and Sectioning	p. 143
Mounting and Grinding	p. 144
Polishing and Etching Methods	p. 145
Image Contrast	p. 148
Reflection and Absorption of Light	p. 149
Bright-Field and Dark-Field Image Contrast	p. 150
Confocal Microscopy	p. 152
Interference Contrast and Interference Microscopy	p. 152
Optical Anisotropy and Polarized Light	p. 157
Phase Contrast Microscopy	p. 163
Working with Digital Images	p. 165
Data Collection and The Optical System	p. 165
Data Processing and Analysis	p. 165
Data Storage and Presentation	p. 166
Dynamic Range and Digital Storage	p. 167
Resolution, Contrast and Image Interpretation	p. 170
Summary	p. 171
Bibliography	p. 173
Worked Examples	p. 173
Problems	p. 176
Transmission Electron Microscopy	p. 179
Basic Principles	p. 185
Wave Properties of Electrons	p. 185
Resolution Limitations and Lens Aberrations	p. 187
Comparative Performance of Transmission and Scanning Electron Microscopy	p. 192
Specimen Preparation	p. 194
Mechanical Thinning	p. 195
Electrochemical Thinning	p. 198
Ion Milling	p. 199
Sputter Coating and Carbon Coating	p. 201
Replica Methods	p. 202
The Origin of Contrast	p. 203
Mass-Thickness Contrast	p. 205
Diffraction Contrast and Crystal Lattice Defects	p. 205
Phase Contrast and Lattice Imaging	p. 207
Kinematic Interpretation of Diffraction Contrast	p. 213
Kinematic Theory of Electron Diffraction	p. 213
The Amplitude-Phase Diagram	p. 213
Contrast From Lattice Defects	p. 215
Stacking Faults and Anti-Phase Boundaries	p. 216
Edge and Screw Dislocations	p. 218
Point Dilatations and Coherency Strains	p. 219
Dynamic Diffraction and Absorption Effects	p. 221
Stacking Faults Revisited	p. 227
Quantitative Analysis of Contrast	p. 230
Lattice Imaging at High Resolution	p. 230
The Lattice Image and the Contrast Transfer Function	p. 230
Computer Simulation of Lattice Images	p. 231
Lattice Image Interpretation	p. 232
Scanning Transmission Electron Microscopy	p. 234
Summary	p. 236
Bibliography	p. 238
Worked Examples	p. 238
Problems	p. 247
Scanning Electron Microscopy	p. 261
Components of The Scanning Electron Microscope	p. 262
Electron Beam-Specimen Interactions	p. 264
Beam-Focusing Conditions	p. 265
Inelastic Scattering and Energy Losses	p. 266
Electron Excitation of X-Rays	p. 269
Characteristic X-Ray Images	p. 271
Backscattered Electrons	p. 277
Image Contrast in Backscattered Electron Images	p. 279
Secondary Electron Emission	p. 280
Factors Affecting Secondary Electron Emission	p. 283
Secondary Electron Image Contrast	p. 286
Alternative Imaging Modes	p. 288
Cathodoluminescence	p. 288
Electron Beam Induced Current	p. 288
Orientation Imaging Microscopy	p. 289
Electron Backscattered Diffraction Patterns	p. 289
OIM Resolution and Sensitivity	p. 291
Localized Preferred Orientation and Residual Stress	p. 292
Specimen Preparation and Topology	p. 294
Sputter Coating and Contrast Enhancement	p. 295
Fractography and Failure Analysis	p. 295
Stereoscopic Imaging	p. 298
Parallax Measurements	p. 298
Focused Ion Beam Microscopy	p. 301
Principles of Operation and Microscope Construction	p. 302
Ion Beam-Specimen Interactions	p. 304
Dual-Beam FIB Systems	p. 306
Machining and Deposition	p. 306
TEM Specimen Preparation	p. 310
Serial Sectioning	p. 314
Summary	p. 315
Bibliography	p. 318
Worked Examples	p. 318
Problems	p. 326
Microanalysis in Electron Microscopy	p. 333
X-Ray Microanalysis	p. 334
Excitation of Characteristic X-Rays	p. 334
Detection of Characteristic X-Rays	p. 338
Quantitative Analysis of Composition	p. 343
Electron Energy Loss Spectroscopy	p. 357
The Electron Energy-Loss Spectrum	p. 360
Limits of Detection and Resolution in EELS	p. 361
Quantitative Electron Energy Loss Analysis	p. 364
Near-Edge Fine Structure Information	p. 365
Far-Edge Fine Structure Information	p. 366
Energy-Filtered Transmission Electron Microscopy	p. 367
Summary	p. 370
Bibliography	p. 375
Worked Examples	p. 375
Problems	p. 386
Scanning Probe Microscopy and Related Techniques	p. 391
Surface Forces and Surface Morphology	p. 392
Surface Forces and Their Origin	p. 392
Surface Force Measurements	p. 396
Surface Morphology: Atomic and Lattice Resolution	p. 397
Scanning Probe Microscopes	p. 400
Atomic Force Microscopy	p. 403
Scanning Tunnelling Microscopy	p. 410
Field-Ion Microscopy and Atom Probe Tomography	p. 413
Identifying Atoms by Field Evaporation	p. 414
The Atom Probe and Atom Probe Tomography	p. 416
Summary	p. 417
Bibliography	p. 420
Problems	p. 420
Chemical Analysis of Surface Composition	p. 423
X-Ray Photoelectron Spectroscopy	p. 424
Depth Discrimination	p. 426
Chemical Binding States	p. 428
Instrumental Requirements	p. 429
Applications	p. 431
Auger Electron Spectroscopy	p. 431
Spatial Resolution and Depth Discrimination	p. 433
Recording and Presentation of Spectra	p. 434
Identification of Chemical Binding States	p. 435
Quantitative Auger Analysis	p. 436
Depth Profiling	p. 437
Auger Imaging	p. 438
Secondary-Ion Mass Spectrometry	p. 440
Sensitivity and Resolution	p. 442
Calibration and Quantitative Analysis	p. 444
SIMS Imaging	p. 445
Summary	p. 446
Bibliography	p. 448
Worked Examples	p. 448
Problems	p. 453
Quantitative and Tomographic Analysis of Microstructure	p. 457
Basic Stereological Concepts	p. 458
Isotropy and Anisotropy	p. 459
Homogeneity and Inhomogeneity	p. 461
Sampling and Sectioning	p. 463
Statistics and Probability	p. 466
Accessible and Inaccessible Parameters	p. 467
Accessible Parameters	p. 468
Inaccessible Parameters	p. 476
Optimizing Accuracy	p. 481
Sample Size and Counting Time	p. 483
Resolution and Detection Errors	p. 485
Sample Thickness Corrections	p. 487
Observer Bias	p. 489
Dislocation Density Revisited	p. 490
Automated Image Analysis	p. 491
Digital Image Recording	p. 494
Statistical Significance and Microstructural Relevance	p. 495
Tomography and Three-Dimensional Reconstruction	p. 495
Presentation of Tomographic Data	p. 496
Methods of Serial Sectioning	p. 498
Three-Dimensional Reconstruction	p. 499
Summary	p. 500
Bibliography	p. 503
Worked Examples	p. 503
Problems	p. 514
Appendices	p. 517
Useful Equations	p. 517
Interplanar Spacings	p. 517
Unit Cell Volumes	p. 518
Interplanar Angles	p. 518
Direction Perpendicular to a Crystal Plane	p. 519
Hexagonal Unit Cells	p. 520
The Zone Axis of Two Planes in the Hexagonal System	p. 521
Wavelengths	p. 521
Relativistic Electron Wavelengths	p. 521
X-Ray Wavelengths for Typical X-Ray Sources	p. 521
Index	p. 523
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