Method of preparing di and poly chalcogenides of group IVb, Vb, molybdenum and tungsten transition metals by low temperature precipitation from non-aqueous solution and the product obtained by said method
AssigneeExxon Research & Engineering Co.
InventorsMartin B. Dines, Russell R. Chianelli
Life of this patent
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Abstract
Finely divided, high surface area, small crystallite (0.1 micron or less) di- and poly-transition metal chalcogenides are prepared by mixing in the absence of an aqueous solvent a transition metal salt with a source of chalcogen yielding a precipitate. The salt and the chalcogen source can be mixed either neat or in the presence of a nonaqueous solvent. The precipitate which results before removal of the anion salt is a finely divided product.
Claims24
A method for the preparation of chalcogenides of the formula MX.sub.y wherein M is a metal selected from the group consisting of IVb, Vb, molybdenum and tungsten transition metals of the Periodic Table of the Elements, X is selected from the group consisting of sulfur, selenium and tellurium, and y is a number ranging from about 2 to about 4, which comprises reacting in the absence of aqueous protic solution a solution of a transition metal salt, the transition metal being selected from the group consisting of Group IVb, Vb, molybdenum, and tungsten with a source of sulfide, selenide or telluride ions which source is selected from the group consisting of Li.sub.2 X, Na.sub.2 X, K.sub.2 X, LiHX, NaHX, KHX, (NH.sub.4).sub.2 X, (NH.sub.4)HX, (RNH.sub.3).sub.2 X, (RR'NH.sub.2).sub.2 X, (RR'R"NH).sub.2 X, wherein R, R' and R" are the same or different and are selected from the group consisting of C.sub.1 to C.sub.20 alkyl and C.sub.6 to C.sub.20 aryl groups and X is the chalcogen selected from the group consisting of sulfur selenium and tellurium at a temperature of from -78.degree. C. to 400.degree. C. for a time sufficient for reaction to occur.
A method for the simultaneous production of a cathode of the formula MX.sub.y wherein M is a transition metal selected from the group consisting of Group IVb, Vb, molybdenum and tungsten, X is selected from the group consisting of sulfur, selenium and tellurium and y is a number from about 2 to about 4 and electrolytes which comprise:
- (1) mixing a transition metal salt wherein the transition metal is selected from the group consisting of Group IVb, Vb, molybdenum and tungsten, with a nonaqueous solvent;
- (2) mixing the solution of step (1) with a strong acid HY wherein Y is selected from the group consisting of Cl.sup.-, Br.sup.-, I.sup.-, ClO.sub.4.sup.-, PF.sub.6.sup.-, BF.sub.4.sup.-, SO.sub.3 CF.sub.3.sup.- ;
- (3) mixing the solution of step (2) with a lithium salt of sulfur, selenium or tellurium at a temperature of from 0.degree. to 400.degree. C. thereby generating the MX.sub.y cathode and the electrolyte LiY.
Dependencies are inferred from the claim text.