Description: 1. Elementary Crystallography. 1-1 The Crystalline State. 1-1.1 Crystalline and Amorphous Solids. 1-1.2 Definition of a Crystal. 1-1.3 Characteristics of the Crystalline and Vitreous States. 1-2 Crystal Geometry. 1-2.1 External Form and Habit of Crystals. 1-2.2 Constancy of Interfacial Angles. 1-2.3 Symmetry Elements of Crystals. 1-2.4 Pseudosymmetry, 13. 1-2.5 Crystallographic Axes. 1-2.6 Axial Ratios. 1-2.7 The Six Crystal Symmetry Systems. 1-2.8 Miller Indices. 1-2.9 The Law of Rational Indices. 1-2.10 Crystal Forms. 1-2.11 Composite Crystals and Twinning. 1-2.12 Equation for the Plane (hkl). 1-2.13 Zones and Zone Relationships. 1-3 Space Lattices. 1-3.1 Historical Introduction. 1-3.2 Definition. 1-3.3 The Unit Ceil. 1-3.4 The 14 Bravais Lattices. 1-3.5 Some Crystallographic Implications of Space Lattices. 1-3.6 Distance between Neighboring Lattice Planes in the Series (hkl). 1-3.7 The Reciprocal Lattice. 1-4 Point Groups and Space Groups. 1-4.1 The Point Group or Crystal Symmetry Class. 1-4.2 The Space Group. General References. Specific References. 2. The Production and Properties of X-rays. 2-1 X-Ray Safety and Protection. 2-2 The Production of X-Rays. 2-2.1 The Origin of X-Rays. 2-2.2 X-Ray Tubes. A. Gas tubes. B. Hot-cathode tubes. C. Modern diffraction tube design. D. Cold-cathode diffraction tubes. E. High-intensity diffraction tubes. F. Microfocus diffraction tubes. 2-2.3 Power Equipment for the Production of X-rays. 2-2.4 Commercial X-ray Generators for Diffraction. 2-2.5 Isotopic X-ray Sources. 2-3 Properties of X-Rays and their Measurement. 2-3.1 The X-ray Spectrum of an Element. A. The continuous x-ray spectrum. B. The characteristic x-ray spectrum. 2-3.2 The Precise Determination of X-ray Wavelengths. 2-3.3 Absorption of X-rays. 2-3.4 Secondary Fluorescent and Scattered X-rays. 2-3.5 Refraction of X-rays. 2-3.6 Monochromatization of X-radiation. A. Single filter technique. B. Balanced-filter technique. C. Crystal monochromator techniques. D. Graphite monochromators. 2-3.7 The Photographic Effects of X-rays. General References. Specific References. 3. Fundamental Principles of X-ray Diffraction. 3-1 Kinematical and Dynamical Diffraction Theory. 3-2 The Geometry of Diffraction. 3-2.1 Scattering of X-rays by Electrons and Atoms. 3-2.2 Scattering by a Regularly Spaced Row of Atoms. 3-2.3 Conditions for Diffraction by a Linear Lattice of Atoms. 3-2.4 Diffraction by a Simple Cubic Lattice. 3-2.5 Proof that the "Diffracting Plane" is a Lattice Plane. 3-2.6 The Bragg Equation. 3-2.7 Derivation of the Bragg Equation from the "Reflection" Analogy. 3-2.8 The Geometrical Picture of Diffraction in Reciprocal Space. 3-3 The Intensity of Diffraction. 3-3.1 Perfect and Imperfect Crystals. 3-3.2 Primary and Secondary Extinction. 3-3.3 Relative and Absolute Intensities. 3-3.4 Factors Affecting the Diffraction Intensities. A. The polarization factor. B. The Lorentz and "velocity" factors. C. The temperature factor. D. The atomic scattering factor. E. The structure factor. F. The multiplicity factor. G. The absorption factor. 3-3.5 Expressions for the Relative Intensity of Diffraction by the Various Techniques. 3-3.6 Lattice-Centering and Space-Group Extinctions. General References. Specific References. 4. Photographic Powder Techniques. 4-1 The Debye-Scherrer Method. 4-1.1 Introduction. 4-1.2 Camera Design. A. General geometry. B. Details of camera construction. C. Camera support and alignment. 4-1.3 Preparation of the Powder. 4-1.4 Mounting the Powder. 4-1.5 Making the Exposure. 4-1.6 Processing the Film. 4-2 Parafocusing Methods. 4-3 Monochromatic-Pinhole Techniques. 4-3.1 Forward-Reflection Method. 4-3.2 Back-Reflection Method. 4-4 Microcameras and Microbeam Techniques. 4-5 High-Temperature Techniques. 4-6 Low-Temperature Techniques. 4-7 High-Pressure Techniques. General References. Specific References. Diffractometric Powder Technique. 5-1 Geometry of the Powder Diffractometer. 5-1.1 General Features. 5-1.2 Details of the Optical Arrangement. 5-1.3 The Seemann-Bohlin Diffractometer. 5-1.4 Alignment and Angular Calibration of the Diffractometer. A. Operations appropriately performed in advance by the manufacturer. B. Further internal alignment of the goniometer. C. Alignment of the goniometer with respect to the x-ray tube. D. Calibration of the O° 2 position. E. Calibration of angular registration between 0 and 180° 2. 5-2 Profiles and positions of diffraction maxima. 5-2.1 Convolution Synthesis of Line Profiles. A. X-ray source, gI. B. Flat specimen surface, gII. C. Axial divergence, gIII. D. Specimen transparency, gIV. E. Receiving slit, gv. F. Comparison of calculated and experimental line profiles. 5-2.2 Displacement and Breadth of Diffraction Maxima. A. Line position. B. Line breadth. C. The practical determination of the centroid and variance. 5-2.3 Accurate Determination of Interplanar (d) Spacings. 5-2.4 "Routine" Determination of Interplanar (d) Spacings. 5-3 Electrical Characteristics of the Diffractometer. 5-3.1 General Arrangement of Components. 5-3.2 Radiation Detectors (Quantum Counters). A. Gas-ionization counters. B. Geiger-Müller counters. C. Proportional counters. D. Scintillation counters. E. Solid-state (energy-dispersive) detectors. 5-3.3 Nonlinearity of Detector Response. 5-3.4 Monochromatizing Techniques. A. Pulse-height discrimination and analysis. B. Ross balanced filters. C. Crystal monochromators. 5-4 Choice of Experimental Conditions and Procedures. 5-4.1 Statistical Accuracy of Counter Measurements. 5-4.2 The Specimen. A. Preparation of powders. B. Rotation of the specimen. C. Preferred orientation and the specimen mount. D. High-temperature techniques. E. Low-temperature techniques. F. Other special specimen techniques. 5-4.3 Transmission Techniques. 5-4.4 Continuous-Scan Techniques. 5-4.5 Step-Scan Techniques and Automation. General References. Specific References. 6. The Interpretation of Powder Diffraction Data. 6-1 The Viewing and Precision Measurement of Powder Photographs. 6-2 Determination of Interplanar (d) Spacings. 6-2.1 Debye-Scherrer Patterns, 424. 6-2.2 Monochromatic-Pinhole (Flat-Film) Patterns, 435. 6-3 Indexing Cubic Powder Patterns. 6-3.1 Reciprocal-Lattice Picture of Diffraction by a Cubic Powder. 6-3.2 Indexing a Cubic Pattern by sin2 Ratios. 6-3.3 Determination of the Unit-Cell Dimension a. 6-3.4 Indexing a Cubic Pattern When a Is Known. 6-4 Determination of Lattice Type. 6-5 Indexing Noncubic Powder Patterns. 6-5.1 Indexing Noncubic Patterns When the Unit-Cell Dimensions are Known. 6-5.2 Graphical Methods of Indexing. 6-5.3 Analytical Methods of Indexing: Tetragonal, Hexagonal, and Orthorhombic Patterns. 6-5.4 Analytical Methods of Indexing: Monoclinic and Triclinic Patterns. 6-6 Automated Computing Procedures for Indexing Powder Patterns. 6-6.1 Programs for Patterns of Orthorhombic and Higher Symmetry. 6-6.2 Programs for Patterns of Low Symmetry. 6-7 The Measurement of Intensities from Photographic Blackening. 6-7.1 Introduction. 6-7.2 Preparation of a Graded Intensity Scale. 6-7.3 Visual Estimation of Intensities. 6-7.4 Photometer Techniques. 6-8 The Measurement of Intensities with the X-Ray Diffractometer. 6-9 Putting Intensities on an Absolute Scale. 6-10 Special Scattering and Diffraction Effects. 6-10.1 Background Effects. A. Background due to lattice imperfections. B. Background due to general radiation. C. Absorption discontinuities. D. Air scatter. E. Secondary fluorescence radiation. 6-10.2 Reflections of Unusual Character. A. Spotty lines. B. Arclike lines. C. Broadened lines. D. Two-dimensional lattice lines. E. Splitting of lines. 6-10.3 Spurions lines. A. Lines due to misalignment of camera elements. B. Diffraction effects from the sample mount. C. Diffraction from radiation contaminants. General References. Specific References. 7. Qualitative and Quantitative Analysis of Crystalline Powders. 7-1 Routine Qualitative Identification of Crystalline Powders. 7-1.1 The JCPDS Powder Diffraction File (PDF). 7-1.2 Experimental Technique of the PDF Method. A. Preparation of the diffraction pattern. B. Measurement of lines on films and diffractometer charts. C. Identification interpretation of the data. 7-1.3 Computer Applications in the PDF Method. 7-1.4 Complications and Limitations of the PDF Method. 7-1.5 Special Identification Techniques. A. Compound identification by isomorphism. B. Procedures for or ganic compounds. C. Identi

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