Chapter 1 Analytical Electron Microscope(AEM) 1
1.1 Brief introduction of AEM history 2
1.2 Interaction between electrons and specimen and signals used by AEM 3
1.3 Electron wavelength and electromagnetic lens 4
1.3.1 Electron wavelength 4
1.3.2 Electromagnetic lens 5
1.4 Structure and function of AEM 11
1.4.1 Illumination system 12
1.4.2 Specimen holders 18
1.4.3 Imaging system 19
1.4.4 Image recording 20
1.4.5 Power supply system and vacuum system 23
1.4.6 Computer control 25
1.5 The principle of imaging,magnifying and diffracting 26
1.6 Theoretical resolution limit 29
1.7 Depth of focus and depth of field 31
1.8 Spherical aberration-corrected TEMs 33
References 35
Chapter 2 Specimen Preparation 37
2.1 Traditional techniques 38
2.1.1 Replica 38
2.1.2 Preparation of powders 42
2.1.3 Film preparation for plan view 43
2.1.4 Film preparation from a bulk metallic sample 44
2.1.5 Film preparation from a bulk nonmetallic sample 52
2.2 Special techniques 56
2.2.1 Cross-sectional specimen preparation 56
2.2.2 Cleaving and small angle cleavage technique 60
2.2.3 Ultramicrotomy 62
2.2.4 Focused ion beam technique 63
References 66
Chapter 3 Electron Diffraction 67
3.1 Comparison of electron diffraction with X-ray diffraction 68
3.2 Conditions of diffraction 69
3.2.1 Geometric condition 69
3.2.2 Physical condition 72
3.2.3 Diffraction deviating from exact Bragg condition 74
3.3 Basic equation used for analysis of electron diffraction pattern 76
3.3.1 Diffraction in an electron diffractometer 76
3.3.2 Diffraction in a TEM 78
3.4 Principle and operation of selected area electron diffraction 81
3.5 Rotation of image relative to diffraction pattern 83
3.6 Diffraction patterns of polycrystal and their applications 84
3.6.1 Formation and geometric features of diffraction patterns for polycrystal 85
3.6.2 Applications of ring patterns 87
3.7 Geometric features of diffraction patterns of single crystals 88
3.7.1 Geometric features and diffraction intensity of a single crystal pattern 89
3.7.2 Indexing methods of single crystal diffraction patterns 93
3.8 Main applications of single crystal pattern 97
3.8.1 Identification of phases 97
3.8.2 Determination of orientation relationship 101
3.9 Diffraction spot shift by stacking faults and determination of stacking fault probability 103
3.9.1 Diffraction from planar defect 103
3.9.2 Determination of stacking fault probability in HCP crystal 104
3.9.3 Determination of stacking fault probability in FCC crystal 108
3.10 Systematic tilting technique and its applications 114
3.10.1 Systematic tilting technique by double tilt holder 115
3 10.2 Determination of electron beam direction 117
3.10.3 Determination of misorientation axis/angle pair 119
3.10.4 Determining phase using reconstruction of reciprocal lattice 122
3.10.5 Trace analysis 125
3.10.6 Unambiguity of orientation determination 130
3.11 Characteristics and indexing of complex electron diffraction patterns 134
3.11.1 Diffraction patterns with the orientation relationship between two phases 134
3.11.2 Twin diffraction pattern 135
3.11.3 High order Laue diffraction pattern 138
3.11.4 Superlattice diffraction pattern 146
3.11.5 Double diffraction pattern 147
3.11.6 Moiré patterns 151
3.11.7 Diffraction pattern of modulated structure 153
3.11.8 Long-period stacking order structures and their diffraction patterns 154
3.11.9 Kikuchi line pattern 161
References 169
Chapter 4 Mathematics Analysis in Electron Diffraction and Crystallography 171
4.1 Transformation matrices of orientation relationships 171
4.1.1 Introduction to matrix analysis 171
4.1.2 Prediction of an arbitrary zone of diffraction pattern based on orientation relationship 173
4.1.3 Transformation matrices for indices of direction and plane in different coordinate systems 188
4.1.4 Mathematics description of characteristics parameters of coincidence site lattice 192
4.1.5 Transformation matrix of twinning orientation relationship 196
4.2 Prediction of orientation relationships 204
4.2.1 Introduction 204
4.2.2 Edge-to-edge matching 205
4.2.3 Invariant line strain model 228
4.2.4 O-line model 236
4.3 Systematic extinction caused by crystallographic symmetry 254
4.3.1 Symmetry elements and their corresponding operation matrices 254
4.3.2 Combination laws of macro-symmetry elements 258
4.3.3 Derivations of the point groups and their transition matrices 261
4.3.4 Relationships between point groups,crystal systems and Bravais lattices 268
4.3.5 Translational symmetry elements in space groups 271
4.3.6 Equivalent positions 273
4.3.7 Two dimensional lattice,plane point groups and plane groups 275
4.3.8 Symmetry of electron diffraction patterns 280
4.3.9 Systematic extinction 281
4.3.10 Example of determining crystal structures by crystal symmetry analysis 285
References 291
Chapter 5 Diffraction Contrast 295
5.1 Classification of electron image contrasts and imaging modes 295
5.1.1 Imaging principles of mass-thickness contrast 296
5.1.2 Principle of diffraction contrast imaging 300
5.1.3 Imaging principle of phase contrast 304
5.2 Kinematical theory of diffraction contrast 304
5.2.1 Basic assumption and approximate treatment 305
5.2.2 Kinematical equation of diffraction contrast for perfect crystals 309
5.2.3 Thickness fringes and bend contours 311
5.2.4 Kinematical equation of diffraction contrast for imperfect crystals 314
5.2.5 Determination of natures of stacking fault and dislocation by diffraction contrast 316
5.3 Dynamical theory of diffraction contrast(wave-optical formulation) 348
5.3.1 Scattering of electrons from atoms 348
5.3.2 Dynamical equation and diffraction contrast for perfect crystals 351
5.3.3 Solution of the equations of the dynamical theory in perfect crystals 355
5.3.4 Bend contours and thickness fringes 359
5.3.5 Anomalous absorption effect 364
5.3.6 Dynamical equations of diffracted contrast for an imperfect crystal 368
5.3.7 Example of computer simulation of dislocations based on two-beam dynamical theory 373
References 377
Chapter 6 High Resolution and High Spatial Resolution of Analytical Electron Microscopy 379
6.1 HRTEM and its applications 380
6.1.1 Electron scattering 380
6.1.2 Fourier transform and convolution 382
6.1.3 Two important functions describing the formation of high resolution images 388
6.1.4 Direct explanation of high resolution image for WPOA 394
6.1.5 High resolution images of thick crystal specimens 400
6.1.6 Application examples of high resolution images 408
6.2 CBED and its applications 424
6.2.1 Formation and features of CBED patterns 424
6.2.2 Identification of crystal symmetry 432
6.2.3 Determination of carbon content by CBED 444
6.2.4 CBED for strain determination at the nanoscale 447
6.3 EDS and its quantitative microanalysis 449
6.3.1 Characteristic X-rays and their detection 449
6.3.2 Quantitative analysis 454
6.3.3 Spatial resolution and detection limits 456
6.4 EELS and its quantitative microanalysis 457
6.4.1 Electron energy loss spectrometer 458
6.4.2 EELS spectrum 459
6.5 Brief introduction to advanced AEMs 467
6.5.1 Negative Cs imaging(NCSI)technique 467
6.5.2 Atomic resolution Z-contrast imaging technique 473
6.5.3 Electron holography 481
References 488
Appendix 491
A.1 Physical constants and conversion factors 491
A.2 Geometrical relationships of crystals 492
A.3 Table of angles between planes(or directions)of cubic crystal 494
A.4 Electron diffraction patterns(EDPs)of FCC,BCC and HCP 503
A.5 Standard high order Laue diffraction patterns of FCC,BCC and HCP 509
A.6 Eight kinds of typical crystal structures 515
A.7 Stereographic projections of cubic and hexagonal systems(c/a=1.633) 516
A.8 Relationship of parameters of coincidence site lattice(CSL)in cubic crystal 526
A.9 Table of atomic scattering factors 532
A.10 Table of characteristic X-ray's wavelength(A)and energy(keV) 539
A.11 Table of electron binding energy for electron energy loss spectroscopy(EELS) 542
References 544
Index 545