Preface ....................................................... ix
List of Contributors .......................................... xi
1 An Overview of Powder Diffraction ........................... 1
Lachlan M.D. Cranswick
1.1 Introduction ........................................... 1
1.2 Range of fields using powder diffraction ............... 6
1.3 Advantages of powder diffraction ....................... 6
1.4 Limitations of powder diffraction ..................... 17
1.5 Pitfalls, misconceptions and requirements ............. 28
1.6 Comparison to single-crystal diffraction .............. 32
1.7 Applications using powder diffraction ................. 37
1.8 Conclusion ............................................ 58
Acknowledgments ............................................ 58
References ................................................. 58
Appendix A. 1 List of available software relevant to
powder diffraction ......................................... 62
2 Introduction to Diffraction ................................ 73
Abraham Clearfield
2.1 Introduction to X-ray diffraction ..................... 73
2.2 Solving the geometric problem ......................... 77
2.3 Scattering theory and treatment of X-ray
diffraction data ...................................... 88
2.4 The intensity formula (Nuffield, 1966) ................ 95
2.5 The reciprocal lattice (Buerger, 1942; Ladd and
Palmer, 2003) ......................................... 97
2.6 Crystal symmetry and space groups (Buerger, 1971;
Hammond, 2004) ....................................... 102
References ................................................ 121
3 Practical Aspects ......................................... 123
Joseph H. Reibenspies and Nattamai Bhuvanesh
3.1 Generation of X-rays: general concepts and
terminology .......................................... 123
3.2 Typical laboratory experimental setups ............... 126
3.3 X-ray optics: monochromators and Gobel mirrors ....... 132
3.4 Detection of X-rays: general concepts and
terminology .......................................... 132
3.5 Specimen mounting methods: general concepts and
terminology .......................................... 143
3.6 Data collection: general concepts .................... 150
3.7 Pitfalls and errors .................................. 154
References ................................................ 155
4 Profile Analysis .......................................... 158
Arnt Kern
4.1 Introduction ......................................... 158
4.2 Origin of line profile shapes ........................ 158
4.3 Convolution-based profile fitting .................... 178
References ................................................ 196
5 Introduction to Non-Laboratory Radiation Sources .......... 199
Peter J. Chupas and Karena W. Chapman
5.1 Introduction to non-laboratory radiation sources ..... 199
5.2 Synchrotron radiation instrumentation ................ 209
5.3 Neutron diffraction instrumentation .................. 217
5.4 Resources ............................................ 223
References ................................................ 223
6 Phase Identification and Quantitative Methods ............. 226
Pamela Whitfield and Lyndon Mitchell
6.1 Introduction ......................................... 226
6.2 Sample preparation for phase ID and quantitative
analysis ............................................. 227
6.3 Data collection ...................................... 234
6.4 Powder diffraction as a fingerprint method ........... 236
6.5 Phase matching using the powder diffraction file -
search-match routines ................................ 242
6.6 Profile fitting ...................................... 246
6.7 Assigning hkls and cell parameter refinement ......... 248
6.8 Quantitative phase determination in the absence of
structural information ............................... 251
6.9 Conclusions .......................................... 258
Acknowledgment ............................................ 258
References ................................................ 259
7 Structure Solution ........................................ 261
Armel Le Bail
7.1 An overview of structure solution by powder
methods .............................................. 261
7.2 Indexing a powder diffraction pattern:
a bottleneck ......................................... 264
7.3 Space group determination, intensities extraction .... 274
7.4 Classical (Patterson and direct) methods of
structure solution ................................... 280
7.5 Direct space methods of structure solution ........... 289
7.6 Structure prediction and powder diffraction .......... 297
7.7 Structure solution from multiple powder patterns
and multiple techniques ............................. 299
7.8 Conclusion ........................................... 301
References ................................................ 302
8 Structure Refinement ...................................... 310
James A. Kaduk
8.1 An introduction to Rietveld refinement ............... 310
8.2 Statistical and graphical measures of a refinement ... 311
8.3 Functions for describing peak shapes, backgrounds,
and diffuse scattering ............................... 317
8.4 Refinement strategies ................................ 323
8.5 Use of chemical knowledge in Rietveld refinement -
organic examples ..................................... 326
8.6 Use of chemical knowledge in Rietveld refinement -
inorganic examples ................................... 332
8.7 X-ray/neutron combined refinement - inorganic
examples ............................................. 346
8.8 Quantitative analysis by Rietveld refinement ......... 352
8.9 Limitations of Rietveld refinement ................... 360
Acknowledgments ........................................... 361
References ................................................ 361
9 Other Topics .............................................. 365
E. Andrew Payzant
9.1 Size/strain determination ............................ 365
9.2 Non-ambient diffraction methods (temperature,
pressure, humidity) .................................. 369
9.3 In situ diffraction experiments ...................... 372
9.4 An introduction to PDF analysis ...................... 376
9.5 Summary .............................................. 378
References ................................................ 378
Index ........................................................ 381
|
