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    • 92. 发明授权
    • Method for the preparation of high surface area amorphous transition
metal chalcogenides
    • 高表面积无定形过渡金属硫族化合物的制备方法
    • US4801441A
    • 1989-01-31
    • US878069
    • 1986-06-24
    • Donald Schleich
    • Donald Schleich
    • C01B19/04C01B17/20C01B19/00C01G39/06H01M4/58C01B17/00
    • C01B17/20C01B19/007C01G39/06C01P2002/02C01P2002/70C01P2006/12C01P2006/42C01P2006/80
    • A process for the direct synthesis of high surface area amorphous chalcogenides of transition metals of Group IV, V, VI and VII elements, comprising the steps of:(1) forming a mixture of:(a) a halide of a said transition metal having the formula MY.sub.n where Y is chlorine, bromine, flurorine, or iodine, and n is 3, 4, 5 or 6, and(b) a source of chalcogen selected from compounds having the formula (R).sub.3 Si--X--Si(R).sub.3 wherein R is alkyl having from 1-4 carbon atoms and X is sulfur, selenium or tellurium,(2) reacting said mixture at a temperature of -77.degree. C. to +160.degree. C.;(3) separating the transition metal chalcogenide from the reaction mixture; and(4) washing said chalcogenide with an inert solvent to remove unreacted materials and the byproducts of the reaction.The high surface area amorphous chalcogenides prepared according to the covalent exchange process of the invention are advantageously used in primary or secondary batteries, particularly lithium cells. They are of amorphous chemical structure as shown by X-ray, Raman and infrared analysis. Their small crystal size, high surface area, and freedom from oxygen and water contamination, make them high activity, rechargeable cathodes in lithium cells.
    • 一种用于直接合成IV,V,VI和VII族元素的过渡金属的高表面积无定形硫族化物的方法,包括以下步骤:(1)形成以下混合物:(a)所述过渡金属的卤化物,其具有 其中Y是氯,溴,氟里昂或碘的式MYn,n是3,4,5或6,和(b)选自具有式(R)3 Si-X-Si(R )3其中R是具有1-4个碳原子的烷基,X是硫,硒或碲,(2)使所述混合物在-77℃至+ 160℃的温度下反应; (3)从反应混合物中分离过渡金属硫族化物; 和(4)用惰性溶剂洗涤所述硫族化物以除去未反应的物质和反应的副产物。 根据本发明的共价交换方法制备的高表面积无定形硫族化物有利地用于一次或二次电池,特别是锂电池中。 它们是非晶化学结构,如X射线,拉曼和红外分析所示。 它们的小晶体尺寸,高表面积,免受氧和水污染,使其具有高活性,锂电池中的可充电阴极。