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Thio sol-gel synthesis of titanium disulfide thin films and powders using titanium alkoxide precursors

机译:烷氧基钛前驱体溶胶-凝胶法合成二硫化钛薄膜和粉末

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摘要

Titanium alkoxides react at room temperature with H2S to form an amorphous titanium alkoxy-sulfide precursor which can be converted to TiS2 by heat-treatment in a flowing H2S gas stream. The reaction of titanium isopropoxide (Ti(OPri)(4)) with H2S in n-butylamine solvent has been studied using infrared spectroscopy (FTIR), gas chromatography/mass spectroscopy (GC/MS), XRD and EDAX measurements. Based on these studies, it is shown that a partially sulfidized alkoxide precursor forms through the partial replacement of some alkoxy groups by hydrosulfide moieties. The alkoxy-hydrosulfide is believed to form following a thiolysis-condensation mechanism similar to the hydrolysis-condensation process that occurs during the oxide sol-gel reaction. The alkoxy-hydrosulfide species then undergoes complete sulfidization at 800 degrees C in a stream of H2S to yield pure, hexagonal TiS2 in either film or powder forms. Crown Copyright (C) 2007 Published by Elsevier B.V. All rights reserved.
机译:烷氧基钛在室温下与H2S反应形成无定形的烷氧基硫化钛钛,可通过在流动的H2S气流中进行热处理将其转化为TiS2。使用红外光谱(FTIR),气相色谱/质谱(GC / MS),XRD和EDAX测量研究了异丙醇钛(Ti(OPri)(4))与H2S在正丁胺溶剂中的反应。基于这些研究,表明部分硫化的醇盐前体是通过氢硫化物部分部分取代某些烷氧基而形成的。据信,烷氧基-氢硫化物是通过类似于在氧化物溶胶-凝胶反应期间发生的水解-缩合过程的硫解-缩合机理而形成的。然后,烷氧基氢硫化物物质在H2S气流中在800摄氏度下进行完全硫化,从而以薄膜或粉末形式生成纯净的六角形TiS2。 Crown版权所有(C)2007,Elsevier B.V.保留所有权利。

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