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9783540437642

Transmission Electron Microscopy and Diffractometry of Materials

by ;
  • ISBN13:

    9783540437642

  • ISBN10:

    3540437649

  • Edition: 2nd
  • Format: Hardcover
  • Copyright: 2002-11-01
  • Publisher: Springer Verlag
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Summary

This textbook develops the concepts of transmission electron microscopy (TEM) and x-ray diffractometry (XRD) that are important for the characterization of materials. It emphasizes themes common to both techniques, such as scattering from atoms, wave interference, and the formation and analysis of diffraction patterns. It explains the uniqueness of each technique, especially imaging and spectroscopy in the TEM. Simple citations of rules are avoided as much as possible, and both practical and theoretical issues are explained in detail. The book can be used as both an introductory and advanced-level graduate text since sections/chapters are sorted according to difficulty and grouped for use in quarter and semester courses on TEM and XRD. Numerous problems are provided at the end of each chapter to reinforce key concepts, and solutions are available to instructors. Appendices provide procedures for introductory laboratory exercises, and up-to-date tabulations of physical data useful for TEM and XRD.

Table of Contents

Diffraction and the X-ray Powder Diffractometer
1(62)
Diffraction
1(12)
Introduction to Diffraction
1(2)
Bragg's Law
3(3)
Strain Effects
6(1)
Size Effects
7(1)
A Symmetry Consideration
8(1)
Experimental Methods
9(4)
The Creation of X-Rays
13(10)
Bremsstrahlung
13(3)
Characteristic Radiation
16(4)
Synchrotron Radiation
20(3)
The X-Ray Powder Diffractometer
23(6)
Practice of X-Ray Generation
23(2)
Goniometer for Powder Diffraction
25(3)
Monochromators and Filters
28(1)
X-Ray Detectors for XRD and TEM
29(8)
Detector Principles
29(5)
Position-Sensitive Detectors
34(1)
Charge Sensitive Preamplifier
35(1)
Other Electronics
35(2)
Experimental X-Ray Powder Diffraction Data
37(26)
Intensities of Powder Diffraction Peaks
37(8)
Phase Fraction Measurement
45(5)
Lattice Parameter Measurement
50(2)
Refinement Methods for Powder Diffraction Data
52(3)
Pair Distribution Function Analysis
55(1)
Further Reading
56(1)
Problems
57(6)
The TEM and its Optics
63(60)
Introduction to the Transmission Electron Microscope
63(4)
Working with Lenses and Ray Diagrams
67(5)
Single Lenses
67(3)
Multi-Lens Systems
70(2)
Modes of Operation of a TEM
72(17)
Conventional Modes
72(11)
Convergent-Beam Electron Diffraction
83(1)
High-Resolution Imaging
84(5)
Real Lens Systems
89(4)
Illumination Lens Systems
89(4)
Imaging Lens Systems
93(1)
Glass Lenses
93(7)
Interfaces
93(2)
Lenses and Rays
95(3)
Lenses and Phase Shifts
98(2)
Magnetic Lenses
100(4)
Lens Aberrations and Other Defects
104(9)
Spherical Aberration
105(1)
Chromatic Aberration
106(1)
Diffraction
107(1)
Astigmatism
107(4)
Gun Brightness
111(2)
Resolution
113(10)
Further Reading
115(1)
Problems
116(7)
Scattering
123(44)
Coherence and Incoherence
123(7)
Phase and Energy
123(3)
Wave Amplitudes and Cross-Sections
126(4)
X-Ray Scattering
130(8)
Electrodynamics of X-Ray Scattering
130(4)
Inelastic Compton Scattering
134(2)
X-Ray Mass Attenuation Coefficients
136(2)
Coherent Elastic Scattering
138(17)
Born Approximation for Electrons
138(5)
Atomic Form Factors--Physical Picture
143(3)
Scattering of Electrons by Model Potentials
146(4)
Atomic Form Factors--General Formulation
150(5)
Nuclear Scattering
155(12)
Properties of Neutrons
156(2)
Inelastic Neutron Scattering
158(4)
Mossbauer Scattering
162(2)
Further Reading
164(1)
Problems
164(3)
Inelastic Electron Scattering and Spectroscopy
167(58)
Inelastic Electron Scattering
167(2)
Electron Energy-Loss Spectrometry (EELS)
169(8)
Instrumentation
169(1)
General Features of EELS Spectra
170(2)
Fine Structure
172(5)
Plasmon Excitations
177(4)
Plasmon Principles
177(2)
Plasmons and Specimen Thickness
179(2)
Core Excitations
181(17)
Scattering Angles and Energies--Qualitative
182(2)
Inelastic Form Factor
184(4)
Double-Differential Cross-Section, d2σin/dφdE
188(2)
Scattering Angles and Energies--Quantitative
190(2)
Differential Cross-Section, dσin/dE
192(1)
Partial and Total Cross-Sections σin
193(3)
Quantification of EELS Core Edges
196(2)
Energy-Filtered TEM Imaging (EFTEM)
198(5)
Energy Filters
199(1)
Chemical Mapping with Energy-Filtered Images
200(2)
Chemical Analysis with High Spatial Resolution
202(1)
Energy Dispersive X-Ray Spectrometry (EDS)
203(22)
Electron Trajectories Through Materials
203(4)
Fluorescence Yield
207(3)
EDS Instrumentation Considerations
210(3)
Thin-Film Approximation
213(3)
ZAF Correction
216(2)
Limits of Microanalysis
218(2)
Further Reading
220(1)
Problems
221(4)
Diffraction from Crystals
225(50)
Sums of Wavelets from Atoms
225(7)
Electron Diffraction from a Material
226(2)
Wave Diffraction from a Material
228(4)
The Reciprocal Lattice and the Laue Condition
232(5)
Diffraction from a Simple Lattice
232(1)
Reciprocal Lattice
233(2)
Laue Condition
235(1)
Equivalence of the Laue Condition and Bragg's Law
235(1)
Reciprocal Lattices of Cubic Crystals
236(1)
Diffraction from a Lattice with a Basis
237(12)
Structure Factor and Shape Factor
237(2)
Structure Factor Rules
239(5)
Symmetry Operations and Forbidden Diffractions
244(1)
Superlattice Diffractions
245(4)
Crystal Shape Factor
249(9)
Shape Factor of Rectangular Prism
249(4)
Other Shape Factors
253(1)
Small Particles in a Large Matrix
254(4)
Deviation Vector (Deviation Parameter)
258(1)
Ewald Sphere
259(4)
Ewald Sphere Construction
259(2)
Ewald Sphere and Bragg's Law
261(1)
Tilting Specimens and Tilting Electron Beams
261(2)
Laue Zones
263(3)
Effects of Curvature of the Ewald Sphere
266(9)
Further Reading
267(1)
Problems
268(7)
Electron Diffraction and Crystallography
275(64)
Indexing Diffraction Patterns
275(9)
Issues in Indexing
276(2)
Method 1--Start with Zone Axis
278(4)
Method 2--Start with Diffraction Spots
282(2)
Stereographic Projections and Their Manipulation
284(9)
Construction of a Stereographic Projection
284(1)
Relationship Between Stereographic Projections and Electron Diffraction Patterns
285(1)
Manipulations of Stereographic Projections
286(7)
Kikuchi Lines and Specimen Orientation
293(11)
Origin of Kikuchi Lines
293(4)
Indexing Kikuchi Lines
297(1)
Specimen Orientation and Deviation Parameter
298(3)
The Sign of s
301(1)
Kikuchi Maps
301(3)
Double Diffraction
304(2)
Occurrence of Forbidden Diffractions
304(1)
Interactions Between Crystallites
305(1)
Convergent-Beam Electron Diffraction
306(26)
Convergence Angle of Incident Electron Beam
308(1)
Determination of Sample Thickness
309(2)
Measurements of Unit Cell Parameters
311(5)
Determination of Point Groups
316(11)
Determination of Space Groups
327(5)
Further Reading
332(7)
Problems
332(7)
Diffraction Contrast in TEM Images
339(84)
Contrast in TEM Images
339(2)
A Review of Structure and Shape Factors
341(2)
Extinction Distance
343(3)
The Phase-Amplitude Diagram
346(2)
Fringes from Sample Thickness Variations
348(5)
Thickness and Phase-Amplitude Diagrams
348(1)
Thickness Contours in TEM Images
349(4)
Bend Contours in TEM Images
353(4)
Diffraction Contrast from Strain Fields
357(4)
Dislocations and Burgers Vector Determination
361(9)
Diffraction Contrast from Dislocation Strain Fields
361(2)
The g.b Rule for Null Contrast
363(4)
Image Position and Dislocation Pairs or Loops
367(3)
Semi-Quantitative Diffraction Contrast from Dislocations
370(8)
Weak-Beam Dark-Field (WBDF) Imaging of Dislocations
378(7)
Procedure to Make a WBDF Image
379(1)
Diffraction Condition for a WBDF Image
380(2)
Analysis of WBDF Images
382(3)
Fringes at Interfaces
385(7)
Phase Shifts of Electron Wavelets Across Interfaces
385(4)
Moire Fringes
389(3)
Diffraction Contrast from Stacking Faults
392(13)
Kinematical Treatment
393(4)
Results from Dynamical Theory
397(3)
Determination of the Intrinsic or Extrinsic Nature of Stacking Faults
400(1)
Partial Dislocations Bounding the Fault
400(1)
An Example of a Stacking Fault Analysis
401(2)
Sets of Stacking Faults in TEM Images
403(1)
Related Fringe Contrast
404(1)
Antiphase (π) Boundaries and δ Boundaries
405(3)
Antiphase Boundaries
405(1)
δBoundaries
406(2)
Contrast from Precipitates and Other Defects
408(15)
Vacancies
408(1)
Coherent Precipitates
409(5)
Semicoherent and Incoherent Particles
414(1)
Further Reading
414(1)
Problems
415(8)
Diffraction Lineshapes
423(42)
Diffraction Line Broadening and Convolution
423(11)
Crystallite Size Broadening
424(3)
Strain Broadening
427(3)
Instrumental Broadening--Convolution
430(4)
Fourier Transform Deconvolutions
434(7)
Mathematical Features
434(3)
Effects of Noise on Fourier Transform Deconvolutions
437(4)
Simultaneous Strain and Size Broadening
441(6)
Fourier Methods with Multiple Orders
447(12)
Formulation
447(5)
Strain Heterogeneity and Peak Asymmetry
452(3)
Column Lengths
455(1)
Size Coefficients
456(2)
Practical Issues in Warren-Averbach Analysis
458(1)
Comments on Diffraction Lineshapes
459(6)
Further Reading
462(1)
Problems
462(3)
Patterson Functions and Diffuse Scattering
465(56)
The Patterson Function
465(9)
Overview
465(1)
Atom Centers at Points in Space
466(1)
Definition of the Patterson Function
467(2)
Properties of Patterson Functions
469(2)
Perfect Crystals
471(3)
Patterson Functions for Homogeneous Disorder and Atomic Displacement Diffuse Scattering
474(11)
Deviations from Periodicity
474(1)
Uncorrelated Displacements
475(3)
Correlated Displacements: Atomic Size Effects
478(2)
Temperature
480(5)
Diffuse Scattering from Chemical Disorder
485(10)
Randomness--Uncorrelated Chemical Disorder
485(4)
SRO Parameters
489(2)
Patterson Function for Chemical SRO
491(1)
Short-Range Order Diffuse Intensity
492(1)
Isotropic Materials
493(1)
Polycrystalline Average and Single Crystal SRO
494(1)
Amorphous Materials
495(11)
One-Dimensional Model
495(5)
Radial Distribution Function
500(4)
Partial Pair Correlation Functions
504(2)
Small Angle Scattering
506(15)
Concept of Small Angle Scattering
506(3)
Guinier Approximation (small Δκ)
509(2)
Porod Law (large Δκ)
511(3)
Density-Density Correlations (all Δκ)
514(2)
Further Reading
516(1)
Problems
517(4)
High-Resolution TEM Imaging
521(76)
Huygens Principle
522(14)
Wavelets from Points in a Continuum
522(5)
Huygens Principle for a Spherical Wavefront-Fresnel Zones
527(4)
Fresnel Diffraction Near an Edge
531(5)
Physical Optics of High-Resolution Imaging
536(6)
Wavefronts and Fresnel Propagator
536(2)
Lenses
538(2)
Materials
540(2)
Experimental High-Resolution Imaging
542(17)
Defocus and Spherical Aberration
542(5)
Lenses and Specimens
547(3)
Lens Characteristics
550(9)
Simulations of High-Resolution TEM Images
559(7)
Principles of Simulations
559(6)
Practice of Simulations
565(1)
Issues and Examples in High-Resolution TEM Imaging
566(20)
Images of Nanostructures
566(3)
Examples of Interfaces
569(3)
Effects of Solute Misfit and Scattering Factor Differences on Spot Intensities
572(4)
Specimen and Microscope Parameters
576(7)
Hints and Tricks for HRTEM
583(3)
Z-Contrast Imaging
586(11)
Characteristics of Z-Contrast Imaging
586(4)
Comparison of Z-Contrast Imaging with HRTEM Imaging
590(2)
Z-Contrast Imaging with Atomic Resolution
592(2)
Developments in Atomic-Resolution Imaging
594(1)
Further Reading
594(1)
Problems
595(2)
Dynamical Theory
597(66)
Chapter Overview
597(2)
Mathematical Features of High-Energy Electrons in a Periodic Potential
599(10)
The Schrodinger Equation
599(6)
Kinematical and Dynamical Theory
605(2)
The Crystal as a Phase Grating
607(2)
First Approach to Dynamical Theory--Beam Propagation
609(4)
Second Approach to Dynamical Theory--Bloch Waves and Dispersion Surfaces
613(19)
Diffracted Beams, {φg}, are Beats of Bloch Waves, {ψ(j)}
613(6)
Crystal Periodicity and Dispersion Surfaces
619(4)
Energies of Bloch Waves in a Periodic Potential
623(3)
General Two-Beam Dynamical Theory
626(6)
Essential Difference Between Kinematical and Dynamical Theories
632(5)
Diffraction Error, sg, in Two-Beam Dynamical Theory
637(4)
Bloch Wave Amplitudes and Diffraction Error
637(2)
Dispersion Surface Construction
639(2)
Dynamical Diffraction Contrast from Crystal Defects
641(14)
Dynamical Diffraction Contrast Without Absorption
641(5)
Two-Beam Dynamical Theory of Stacking Fault Contrast
646(4)
Dynamical Diffraction Contrast with Absorption
650(5)
Multi-Beam Dynamical Theories of Electron Diffraction
655(8)
Further Reading
658(1)
Problems
658(5)
Bibliography 663(14)
Further Reading
663(4)
References and Figures
667(10)
A. Appendix 677(58)
A.1 Indexed Powder Diffraction Patterns
677(1)
A.2 Mass Attenuation Coefficients for Characteristic α X-Rays
678(1)
A.3 Atomic Form Factors for X-Rays
679(4)
A.4 X-Ray Dispersion Corrections for Anomalous Scattering
683(1)
A.5 Atomic Form Factors for 200 keV Electrons and Procedure for Conversion to Other Voltages
684(5)
A.6 Indexed Single Crystal Diffraction Patterns: fcc, bcc, dc, hcp
689(10)
A.7 Stereographic Projections
699(4)
A.8 Examples of Fourier Transforms
703(3)
A.9 α1, α2 Splitting and the Rachinger Correction
706(1)
A.10 Numerical Approximation for the Voigt Function
707(1)
A.11 Debye--Waller Factor from Wave Amplitude
708(1)
A.12 Review of Dislocations
709(7)
A.13 TEM Laboratory Exercises
716(16)
A.13.1 Preliminary--JEOL 2000FX Daily Operation
716(4)
A.13.2 Preliminary--Philips 400T Daily Operation
720(2)
A.13.3 Laboratory 1 -- Microscope Procedures and Calibration with Au and MoO3
722(4)
A.13.4 Laboratory 2 -- Diffraction Analysis of θ' Precipitates
726(3)
A.13.5 Laboratory 3 -- Chemical Analysis of θ' Precipitates
729(1)
A.13.6 Laboratory 4 -- Contrast Analysis of Defects
730(2)
A.14 Fundamental and Derived Constants
732(3)
Index 735

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