Abstract

Low temperature methods have been applied to the synthesis of many advanced materials. Non-hydrolytic sol-gel (NHSG) processes offer an elegant route to stable and metastable phases at low temperatures. Excellent atomic level homogeneity gives access to polymorphs that are difficult or impossible to obtain by other methods. The NHSG approach is most commonly applied to the preparation of metal oxides, but can be easily extended to metal sulfides. Exploration of experimental variables allows control over product stoichiometry and crystal structure. This paper reviews the application of NHSG chemistry to the synthesis of negative thermal expansion oxides and selected metal sulfides.

Highlights

  • Advanced materials play an important role in everyday life of modern society

  • Sol-gel methods to metal sulfides can be divided into thio-sol-gel routes, which are the equivalent of conventional sol-gel reactions to metal oxides, and a process similar to Non-hydrolytic sol-gel (NHSG) approaches to metal oxides (Figure 2)

  • In the late 1980’s, Schleich et al investigated the reaction of metal halides with organic sulfur sources [64,65,66,67,68]. This procedure is comparable to NHSG routes developed for metal oxides [24,25,69], and will be referred to as “non-hydrolytic” sol-gel approach to metal sulfides

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Summary

Introduction

Advanced materials play an important role in everyday life of modern society. Solid-state inorganic materials transcend all aspects of our lives, from structural materials to specialized compounds used in electronics, optics, and energy applications. Traditional sol-gel routes rely on hydrolysis and condensation reactions between metal alkoxides and small amounts of water in organic solvents In this process, the breakage of a metal-oxygen bond is the rate limiting step, resulting in significantly different kinetics for different metals. Sol-gel methods to metal sulfides can be divided into thio-sol-gel routes, which are the equivalent of conventional sol-gel reactions to metal oxides, and a process similar to NHSG approaches to metal oxides (Figure 2). In the late 1980’s, Schleich et al investigated the reaction of metal halides with organic sulfur sources [64,65,66,67,68] This procedure is comparable to NHSG routes developed for metal oxides [24,25,69], and will be referred to as “non-hydrolytic” sol-gel approach to metal sulfides

Non-Hydrolytic Sol-Gel Synthesis of Metal Oxides
NHSG Routes to A2M3O12 Materials
Gallium Molybdate Ga2Mo3O12
Low-Temperature Phase of Yttrium Molybdate Y2Mo3O12
Non-Hydrolytic Sol-Gel Synthesis of Metal Sulfides
Synthesis of Troilite with Unusual Stoichiometry
High Pressure Phase of Copper Sulfide
New Phase in the Tungsten Sulfide System
Findings
Conclusions
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