Preparative Methods in Solid State Chemistry

1st Edition - January 28, 1972
Editor: Paul Hagenmuller
Language: English
eBook ISBN:
9 7 8 - 0 - 3 2 3 - 1 4 4 3 6 - 0

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… Read more

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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.

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