Modern powder diffraction:
Saved in:
| Format: | Book |
|---|---|
| Language: | English |
| Published: |
Washington, DC
Mineralogical Soc. of America
1989
|
| Series: | Reviews in mineralogy
20 |
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Item Description: | Literaturverz. |
| Physical Description: | XI, 369 S. graph. Darst. |
| ISBN: | 0939950243 |
Staff View
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| 245 | 1 | 0 | |a Modern powder diffraction |c David L. Bish ..., eds. |
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Record in the Search Index
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| adam_text | Table of Contents
Page
ii Copyright; Additional Copies
iii Foreword
iii Preface and Acknowledgments
Chapter 1 R. C. Reynolds, Jr.
Principles of powder Diffraction
1 Introduction
1 Scattering by points
3 Summation of Amplitudes
4 the Intensity of reflection from an Infinite Plane
6 the Intensity of reflection from a finite plane
8 the Bragg law
9 Diffraction from a Set of Reflecting Planes
9 The Unit Cell and the Interference Function
9 The unit cell
11 The interference function
13 Calculation of the Three-Dimensional Diffraction pattern
17 references
Chapter 2 R. Jenkins
INSTRUMENTATION
19 measurement of x-ray powder diffraction patterns—camera
Methods
19 The Debye-Scherrer camera
21 The Gandolfi camera
21 The Guinier camera
23 MEASUREMENT OF X-RAY POWDER PATTERNS—POWDER DlFFRACTOMETERS
23 The Seemann-Bohlin powder diffractometer
24 The Bragg-Brentano parafocusing powder diffractometer
25 Systematic aberrations
25 Axial divergence
26 Flat specimen
26 Absorption
26 Displacement errors
27 EFFECT OF INSTRUMENT PARAMETERS
27 Focal spot dimensions of the tube
27 Effect of take-off angle
27 Effect of receiving slit width
29 Effect of axial divergence
29 Effect of divergence slit
31 Choice of fixed divergence slit
31 Use of the variable divergence slit
31 X-RAY DETECTORS
31 Quantum counting efficiency
32 Linearity
32 Proportionality
32 The gas proportional counter
33 The scintillation detector
34 Solid-state detectors
34 The Si(Li) detector
35 The Ge(Li) detector
35 Cadmium telluride
35 Mercuric iodide
35 Position-sensitive detectors
36 TECHNIQUES FOR THE SELECTION OF MONOCHROMATIC RADIATION
38 Useoftheß-filter
39 Use of pulse-height selection
40 Use of monochromators
41 Use of solid-state detectors
43 resolution versus Intensity
43 References
Chapter 3 R. Jenkins
EXPERIMENTAL PROCEDURES
47 INTRODUCTION
49 FACTORS INFLUENCING d-SPACING ACCURACY
50 Influence of diffractometer misalignment
50 The zero error
50 Errors in the 2:1 rotation of the goniometer
50 Experimental 2e errors
50 Counting statistical limitations
52 Rate-meter errors
54 Step-scanning errors
55 Software-induced errors
56 Problems in specimen placement
57 Problems in establishing the true peak position
57 Problems with manual methods
57 Use of software peak-hunting programs
60 Treatment of the background
60 Treatment of the oq.
60 Errors in conversion of 28 to d
62 FACTORS INFLUENCING INTENSITY ACCURACY
63 Relative and absolute intensities
63 Structure-dependent factors
63 Instrument- and software-dependent factors
63 Effect of the divergence slit
65 Influence of detector dead time
65 Influence of smoothing
65 Specimen-dependent factors
66 Measurement-dependent factors
67 AUTOMATION OF QUALITATIVE PHASE ANALYSIS
67 Computer data-bases
67 Role of the personal computer
68 USE OF STANDARDS
68 Use of standards to establish quality of alignment
69 Use of external 2e-alignment standards
69 Use of internal 29-alignment standards
69 Use of standards to model systematic relative intensity errors
69 REFERENCES
Chapter 4 D. L. Bish and R. C. Reynolds, Jr.
Sample Preparation for x-ray Diffraction
73 introduction
73 Common Problems in Sample Preparation
73 Grinding problems
74 Sample mounting
74 Sample area
75 Sample thickness
76 Sample packing
76 Sample surface
76 Sample-height displacement
77 METHODS OF GRINDING AND DlSAGGREGATION
78 PARTICLE-SEE REQUIREMENTS
78 Extinction
80 Particle statistics
82 Microabsorption
84 RANDOMLY ORIENTED POWDER PREPARATION
84 Side- and back-packed mounts
85 Solid filler materials
85 Use of a viscous mounting material or dispersion in a binder
87 Special methods for minimizing preferred orientation
87 Tubular aerosol suspension
87 liquid-phase spherical agglomeration
88 Spray drying
89 Preparing Oriented Clay Mineral aggregates
91 Reconnaissance
91 Quantitative analysis
92 Crystal structure analysis
93 Special Sample preparation techniques
93 Mounting small samples
97 REFERENCES
Chapter S R. L. Snyder and D. L. Bish
Quantitative analysis
101 Introduction
102 The internal-standard Method of Quantitative Analysis
102 Background
104 The generalized Reference Intensity Ratio
106 corundum
106 Measurement of I/Ic
107 Quantitative analysis with IIIC - the RIR or Chung method
107 Analysis when a known amount of corundum is added to an
unknown
107 Analysis when a known amount of an internal standard is added to a
sample
108 Analysis of a mixture of identified phases without the addition of an
internal standard—the RIR or Chung method
109 Constrained XRD phase analysis—generalized internal-standard method
111 THE INTERNAL-STANDARD METHOD—AN EXAMPLE
112 Internal standard selection
112 Diffraction line selection
115 Calibration of the AI2Q3 standard
115 Calibration of the SiO2 standard
115 Data collection and analysis
116 Running an unknown
120 EXAMPLE USE OF THE REFERENCE INTENSITY RATIO OR CHUNG METHOD
122 The Chung method using direct input of RIR and Irel values
122 Absorption-diffraction Method
122 Analysis of a mixture of known chemical composition
124 Analysis of a mixture of unknown chemical composition by measuring
124 Analysis of a sample whose mass absorption coefficient is the same as that
of the pure phase
124 Analysis of thin films or lightly loaded filters
124 Analysis of a binary mixture of two known phases
125 METHOD OF STANDARD ADDITIONS OR SPIKING METHOD
126 Amorphous phase analysis
126 error propagation in Quantitative Analysis
128 full-pattern Fitting
129 Quantitative phase analysis using the Rietveld method
129 Theory
132 Applications
138 Quantitative phase analysis using observed patterns
142 REFERENCES
Chapter 6 R. C. Reynolds, Jr.
DIFFRACTION BY SMALL AND DISORDERED CRYSTALS
145 INTRODUCTION
145 DIFFRACTION BY SMALL CRYSTALS
145 Equi-dimensional parallelepiped crystals
147 Two-dimensional diffraction from turbostratic structures
150 Two-dimensional diffraction with some third-dimensional influence
155 ONE-DIMENSIONAL DIFFRACTION FROM SIMPLE CLAY MINERALS
155 Mathematical formulation
158 The 00/ series and particle size effects
158 The 00/ series and defect broadening
159 The 00/ series and strain broadening
163 The effect of the continuous function F(8)2 on peak shape and displacement
164 The pure diffraction Une profile
165 The Lorentz factor for oriented clay mineral aggregates
170 MIXED-LAYERED MICAS AND CLAY MINERALS
170 Mathematical formulation
172 Interpretation of basal series diffraction patterns of mixed-layered clay
minerals
175 Examples of mixed-layered clay minerals
178 DIFFRACTION FROM GLASS
178 Mathematical formulation
179 Examples of diffraction patterns from glass
181 REFERENCES
Chapter 7 D. K. Smith
COMPUTER ANALYSIS OF DIFFRACTION DATA
183 INTRODUCTION
184 TYPES OF NUMERICAL DIFFRACTION DATA
185 REFERENCE NUMERIC DATABASES FOR POWDER DIFFRACTION ANALYSIS
185 The Powder Diffraction File
185 PDF-I
186 PDF-2
186 PDF-3
187 NIST Crystal Data File
187 NIST/Sandia/ICDD Electron Diffraction Database
187 FIZ-4 Inorganic Crystal Structure Database
187 NRCC Metals Structure Database
188 Mineral Data databases
188 Analysis of d-i data
188 Processing of d-I data sets
189 Identification of mineral phases
190 Mini- and main-frame routines
190 PC-based search routines
190 Indexing of d-spacing data for an unknown
192 Cell reduction and lattice evaluation
193 Unit-cell refinements
194 Unit-cell identification
195 Quantitative analysis
195 Tests for preferred orientation
196 Structure analysis using integrated intensities
196 Analysis of digitized Diffraction traces
196 Processing of raw digitized data
197 Location of peak positions and intensities
199 Crystal structure analysis
199 Structure modeling
200 Structure refinement
202 Quantification of crystallite parameters
202 Quantitative phase analysis
203 Crystallinity
203 Crystallite size and strain
204 File building and transfer
205 Structure display programs
206 Analytical Packages
206 Miscellaneous routines
207 General Comments and disclaimer
207 Sources of programs
213 references
Chapter 8 S. A. Howard and K. D. Preston
Profile fitting of Powder diffraction patterns
217 INTRODUCTION
220 Advantages of using refined line parameters
220 Qualitative phase analysis
221 Indexing
221 Accurate lattice parameter determination
221 Quantitative phase analysis
222 Development of the profile-shape-functions used in profile and pattern
fitting
224 The Rietveld method of pattern-fitting sructwe-refinement
226 The PSF in Rietveld structure refinement algorithms
228 Profile-shape-functions in profile refinement of X-ray data
231 The use of direct convolution functions
232 Direct convolution products
234 The Voigt and pseudo-Voigt function
240 Particle-size and strain analysis via direct- or approximated-convolution
relations
241 Analysis using the Voigt function
243 Profile fitting of synchrotron diffraction data
243 Two-step structure refinement using a whole-pattem-fitting algorithm
244 Considerations in profile fitting
244 General considerations in profile refinement
245 Minimizing parameter correlation
247 The least-squares error criteria for refinement
248 The choice of optimization algorithm
249 The convergence criterion for the optimization algorithms
250 Goodness of fit
250 Choice of profile-shape-function
251 Single-line PSF s
253 Accommodating satellite tines
253 Compound profile-shape-functions
255 Additional constraints on the profile shapes
257 Alpha-2 stripping
257 Digitalfiltering
259 Accommodating an amorphous profile in the pattern
261 Convolution-based profiles
261 W—the factor determining the number of lines in the instrument
PSF
262 Development of the instrument profile calibration curves
262 The method of profile generation
263 Generation of the specimen profile
264 Numerical convolution of (W*G) and S
264 Maintaining the definition of the convolute profile
266 Specimen broadening as a function of angle: particle size and
strain constraints
268 Miscellaneous considerations
268 Background
269 Adding lines after the initial refinement
210 Discrepancies indicated by the difference patterns
271 SUMMARY
272 REFERENCES
Chapter 9 J. E. Post and D. L. Bish
RIETVELD REFINEMENT OF CRYSTAL STRUCTURES USING
POWDER X-RAY DIFFRACTION DATA
277 INTRODUCTION
279 RIETVELD METHOD IN PRACTICE
279 Data collection
281 Starting model
281 Computer programs
282 The diffraction profile
286 Unit-cell parameter refinement
288 A sample Rietveld refinement
290 Estimated standard deviations
293 EXAMPLES OF RIETVELD REFINEMENTS
294 Zeolites
294 Kaolinite
296 Hollandite
300 Structure solution using Rietveld Methods
301 Todorokite
304 Summary
305 References
Chapter 10 L w Finger
SYNCHROTRON POWDER DIFFRACTION
309 Introduction
309 Source Characteristics
312 Beam divergence/tesolution
314 Photon output
316 Spectral distribution
317 Time structure of ring
318 HIGH-RESOLUTION EXPERIMENTS
318 Peak shape
320 Determination of lattice geometry
321 Extraction of intensities for structure solution
323 Non-isotropic broadening
324 LOW- TO MEDIUM-RESOLUTION EXPERIMENTS
324 Rapid measurement
324 Time-dependent studies
324 UTILIZATION OF SPECTRAL DISTRIBUTION
324 Experiments near absorption edges
326 White beam experiments
327 sample preparation
329 present and Future Opportunities
329 Operating beam-line locations and characteristics
329 New techniques
329 REFERENCES
Chapter 11 R. B. Von Dreele
Neutron powder diffraction
333 introduction
333 the neutron—basic properties
335 neutron powder diffraction theory
338 reactor neutron sources
341 constant-wavelength powder diffractometer design
343 spallation Neutron sources
345 time-of-flight powder diffractometer design
347 Neutron detection
350 Special Sample Environments in Neutron Diffraction
351 rietveld Refinement
352 Background intensity contribution
353 Bragg intensity contribution
354 Profile functions for CW and TOF
354 Reflection positions in powder patterns
354 TOF profile functions
355 Interpretation of TOF profile coefficients
357 CW profile functions
358 Interpretation of CW profile coefficients
359 Reflection peak widths
359 Systematic effects on the intensity
360 Extinction in powders
360 Powder absorption factor
361 Preferred orientation of powders
361 Other angle-dependent corrections
361 APPLICATIONS OF NEUTRON POWDER DIFFRACTION
362 Hydrogen atom location
363 Cation distribution
366 Combined X-ray/neutron Rietveld refinement
367 CONCLUSION
367 REFERENCES
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| indexdate | 2024-07-09T15:45:42Z |
| institution | BVB |
| isbn | 0939950243 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-001600785 |
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| physical | XI, 369 S. graph. Darst. |
| publishDate | 1989 |
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| publisher | Mineralogical Soc. of America |
| record_format | marc |
| series | Reviews in mineralogy |
| series2 | Reviews in mineralogy |
| spelling | Modern powder diffraction David L. Bish ..., eds. Washington, DC Mineralogical Soc. of America 1989 XI, 369 S. graph. Darst. txt rdacontent n rdamedia nc rdacarrier Reviews in mineralogy 20 Literaturverz. Röntgenstrukturanalyse (DE-588)4137203-7 gnd rswk-swf Pulvermethode (DE-588)4176353-1 gnd rswk-swf Debye-Scherrer-Methode (DE-588)4148957-3 gnd rswk-swf (DE-588)4143413-4 Aufsatzsammlung gnd-content Debye-Scherrer-Methode (DE-588)4148957-3 s DE-604 Pulvermethode (DE-588)4176353-1 s Röntgenstrukturanalyse (DE-588)4137203-7 s Bish, David L. Sonstige oth Reviews in mineralogy 20 (DE-604)BV000002349 20 HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=001600785&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Modern powder diffraction Reviews in mineralogy Röntgenstrukturanalyse (DE-588)4137203-7 gnd Pulvermethode (DE-588)4176353-1 gnd Debye-Scherrer-Methode (DE-588)4148957-3 gnd |
| subject_GND | (DE-588)4137203-7 (DE-588)4176353-1 (DE-588)4148957-3 (DE-588)4143413-4 |
| title | Modern powder diffraction |
| title_auth | Modern powder diffraction |
| title_exact_search | Modern powder diffraction |
| title_full | Modern powder diffraction David L. Bish ..., eds. |
| title_fullStr | Modern powder diffraction David L. Bish ..., eds. |
| title_full_unstemmed | Modern powder diffraction David L. Bish ..., eds. |
| title_short | Modern powder diffraction |
| title_sort | modern powder diffraction |
| topic | Röntgenstrukturanalyse (DE-588)4137203-7 gnd Pulvermethode (DE-588)4176353-1 gnd Debye-Scherrer-Methode (DE-588)4148957-3 gnd |
| topic_facet | Röntgenstrukturanalyse Pulvermethode Debye-Scherrer-Methode Aufsatzsammlung |
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