Preparative Methods in Solid State Chemistry

Preparative Methods in Solid State Chemistry deals with the preparative methods used in solid state chemistry and highlights the importance of the chemist's role in preparing materials of desired quality as well as obtaining materials according to the requirements of the user such as the physicist. Topics covered range from high-pressure techniques in preparative chemistry to methods of growing single crystals of high-melting-point oxides.
This book is comprised of 14 chapters and begins with an overview of possibilities for high-pressure synthesis, as well as the methods used to obtain high pressures, including transmission by gaseous or liquid fluids or in the solid state. The method of shock waves is then considered both from the point of view of thermodynamics and thermoelasticity, along with the possibility of using superpressures for evidently revolutionary applications. Subsequent chapters focus on the synthesis of single crystals of refractory oxides either at high temperatures (essentially liquid-solid transformations) or at lower temperatures in the presence of a solvent or a chemical reagent. The production of single crystals by electrolytic reduction in molten salts is also described. Numerous examples of vapor transport reactions in a temperature gradient are presented.
This monograph should be of interest to chemists and students of solid state chemistry.

Contenu

List of Contributors
Preface
Introduction
High-Pressure Synthesis
I. Introduction
II. General Techniques
III. Structural Considerations
IV. High-Pressure Transformations
V. Syntheses Requiring High Pressure
VI. Syntheses Aided by High Pressure
References
High-Pressure Techniques in Preparative Chemistry
I. Introduction
II. Systems under High-Pressure Gas Conditions
III. Systems under High-Pressure Liquid Conditions
IV. Solid State Systems under High-Pressure Conditions
V. Shock Waves
VI. Safety
Bibliography
References
Syntheses under Shock-Wave Pressures
I. Introduction
II. Thermodynamics of Shock Compression
III. Transmission of Shock Waves in Single Crystals
IV. Transmission of Shock Waves in Polycrystalline Materials
V. Inorganic Syntheses in Shock Waves
References
Modern Methods of Growing Single Crystals of High-Melting-Point Oxides
Introduction
I. High-Temperature Crystal Growth
II. Low-Temperature Crystal Growth (in Solution)
III. Comparison between Crystals Obtained with the Two Methods
References
Chemical Transport as a Preparative Procedure
Introduction
I. Fundamentals of Chemical Transport
II. Criteria for the Choice of Transport Reactions
III. Specifications of the Technique
IV. Transported Materials and Transporting Agents
V. Simultaneous Use of Several Transporting Gases
VI. The Amount of Transporting Agent
VII. Impurities in the Transported Solid Phase
VIII. Complex Solid Phases
IX. Solid Solutions; Hägg-Magnéli Phases
X. Promotion of Solid State Reactions by a Transporting Gas Phase
XI. Purification and Separation of Materials
XII. Illustrations of Crystals
References
Preparation of Transition Metal Compounds by Electrolytic Reduction of Fused Salts
I. Introduction
II. Preparation of Transition Metal Oxides
III. Preparation of Transition Metal Sulfides
IV. Transition Metal Phosphides
V. Transition Metal Arsenides and Antimonides
VI. Preparation of Transition Metal Carbides, Silicides, and Germanides
VII. Transition Metal Borides
VIII. Summary
References
Preparation of Single Crystals of III-V Compounds
I. Physical Properties and Applications
II. Preparation of Large Single Crystals
III. Growth of Thin Layers
IV. III-V Ternary Compounds
References
Preparation of CdS Single Crystals by Epitaxial Growth on Germanium Substrates
I. Introduction
II. Experimental
III. Properties of the CdS Crystals
IV. Epitaxial Relations
References
Oriented Eutectic Crystallization
I. Introduction
II. Unidirectional Eutectic Solidification
III. Off-Eutectic Lamellar Growth
IV. Composite Growth Other Than Eutectic
V. Growth of Complex Regular Structures
VI. Final Remarks
References
Preparative Methods for Solid Fluorine Compounds
I. Introduction
II. General Fluorine Technology
III. Reactions in Solution
IV. Gas-Solid Reactions
V. Solid-Phase Reactions
VI. Gas-Phase Reactions
VII. Other Methods
References
Boron Syntheses
Introduction
I. The Various Forms of Boron in the Solid State
II. Reduction of Boron Compounds by Metals
III. Reduction of Boron Compounds by Electrolysis
IV. Reduction of Boron Halides by Hydrogen
V. Purification of Boron by Zone Melting
Summary
References
Preparation Conditions of the Ferrites
I. Introduction
II. Thermodynamic Equilibria
III. Solid State Formation
IV. Preparation of Ferrites
V. Forming of Compacts
VI. Sintering
VII. Crystal Growth
References
Preparation of Transition-Metal Carbides and Related Compounds
I. Introduction
II. Methodology
III. Special Operations
IV. Binary Carbides
V. Intercarbide Systems
VI. Metal-Nonmetal Carbides
References
Preparation of Chalcogenides and Pnyctides at Low Temperature
I. Introduction
II. Preparation from the Elements Using Halides
III. Removal of the Halide
IV. Purity of the Products
V. Characteristics and Applicability of the Method
VI. Experimental
References
Author Index
Subject Index