Microstructural Characterization of Materials » (2nd Edition)

Microstructural Characterization of Materials- 2nd Edition

David Brandon and Wayne D. Kaplan.

Israel Institute of Technology, Haifa, Israel

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.

The book 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 of Microstructural Characterization of Materials 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.

The book should appeal to senior undergraduate and graduate students of material science, materials engineering, and materials chemistry, as well as toqualified engineers and more advanced researchers, who should find the book a useful and comprehensive general reference source.

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