CN-121986071-A - Method for producing molybdenum trioxide with reduced Sb content

CN121986071ACN 121986071 ACN121986071 ACN 121986071ACN-121986071-A

Abstract

The problem of the present disclosure is to provide a method for manufacturing molybdenum trioxide with reduced Sb content. A process for producing molybdenum trioxide, which comprises a step of mixing a raw material comprising a molybdenum compound or a hydrate thereof with chlorine gas, hydrogen chloride or a chloride, and a step of heating the obtained mixture at a temperature of 70 ℃ or higher. The method for producing molybdenum trioxide comprises a step of mixing a raw material comprising molybdenum trioxide, ammonium molybdate or a hydrate thereof with ammonium chloride, and a step of heating the obtained mixture at a temperature of 180 ℃ or higher.

Inventors

KUWAYAMA YASUHIRO
TSUCHITA KATSUYUKI
NAKAMURA TAICHI

Assignees

ＪＸ金属株式会社

Dates

Publication Date: 20260505
Application Date: 20241009
Priority Date: 20240423

Claims (9)

1. A method for producing molybdenum trioxide, comprising: A step of mixing a raw material composed of a molybdenum compound or a hydrate thereof with chlorine gas, hydrogen chloride or a chloride, and And heating the obtained mixture at a temperature of 70 ℃ or higher.
2. A method for producing molybdenum trioxide, comprising: A step of mixing a raw material composed of molybdenum trioxide, ammonium molybdate or a hydrate thereof with ammonium chloride, and And heating the obtained mixture at a temperature of 180 ℃ or higher.
3. A method for producing molybdenum trioxide, comprising: A step of mixing a raw material composed of molybdenum trioxide, ammonium molybdate or a hydrate thereof with an aqueous solution containing ammonium chloride, and And heating the obtained mixture at a temperature of 180 ℃ or higher.
4. A method for producing molybdenum trioxide, comprising: mixing a raw material comprising molybdenum trioxide, ammonium molybdate or a hydrate thereof with ammonia water, then mixing hydrochloric acid, and heating the obtained mixture at a temperature of 180 ℃ or higher.
5. A method for producing molybdenum trioxide, comprising: mixing a raw material comprising molybdenum trioxide, ammonium molybdate or a hydrate thereof with hydrochloric acid, then mixing ammonia water, and heating the obtained mixture at a temperature of 180 ℃ or higher.
6. The method for producing molybdenum trioxide according to any one of claims 1-5, wherein, The Sb content in the produced molybdenum trioxide is 1/3 or less in terms of weight ratio relative to the Sb content contained in the raw material.
7. The method for producing molybdenum trioxide according to any one of claims 1-5, wherein, The S content in the produced molybdenum trioxide is 1/2 or less in terms of weight ratio to the S content contained in the raw material.
8. The method for producing molybdenum trioxide according to any one of claims 1-5, wherein, The Sb content in the produced molybdenum trioxide is 0.2 ppm by weight or less.
9. The method for producing molybdenum trioxide according to any one of claims 1-5, wherein, The S content in the produced molybdenum trioxide is 0.1 ppm by weight or less.

Description

Method for producing molybdenum trioxide with reduced Sb content Technical Field The present invention relates to a method for producing molybdenum trioxide having a reduced Sb content. Background Molybdenum (Mo) is expected to be used as a material for electronic devices such as a contact plug in a large scale integrated circuit (LSI), a wiring, a word line in a semiconductor memory, or a diffusion barrier layer under the wiring, because of its low resistivity and chemical stability. For example, a layer formed of molybdenum or a compound thereof is formed by a Chemical Vapor Deposition (CVD) method in which a molybdenum-containing compound is vaporized as a precursor, decomposed on a substrate surface, and reacted to form a thin film. In recent years, in order to uniformly form a molybdenum layer in a recess of a high aspect ratio (aspect ratio), a technique of forming a thin layer of molybdenum using an Atomic Layer Deposition (ALD) and then forming a thick layer by CVD, plating, or the like has also been used. In the case of forming a layer formed of molybdenum or a compound thereof using CVD or ALD, molybdenum oxychloride, which is a compound of chlorine and molybdenum oxide, is used as a precursor. Molybdenum oxychloride is typically synthesized by chlorinating molybdenum oxide with chlorine gas. The molybdenum oxide used as a raw material is a high purity product. Examples of a method for producing high-purity molybdenum or molybdenum oxide include patent documents 1 to 4. These patent documents disclose that molybdenum trioxide (molybdenum oxide) is produced in high purity by dissolving molybdenum trioxide in aqueous ammonia, separating out and separating out impurity elements, crystallizing and precipitating ammonium molybdate using an acid, and calcining the same. Prior art literature Patent literature Patent document 1 Japanese patent publication No. 6-10090 Patent document 2 Japanese patent laid-open No. 2-141507 Patent document 3 Japanese patent publication No. 5-64683 Patent document 4 Japanese patent publication No. 3-7607 Disclosure of Invention Problems to be solved by the invention Molybdenum oxychloride used as a precursor for CVD and ALD is synthesized by chlorinating molybdenum oxides such as molybdenum trioxide with chlorine gas. In order to improve the purity of molybdenum oxychloride as a precursor, it is necessary to purify molybdenum oxide as a raw material. Conventionally, molybdenum trioxide is produced by dissolving a molybdenum trioxide raw material with ammonia water, filtering the solution to remove solid impurities, adding nitric acid to precipitate ammonium molybdate, and calcining the ammonium molybdate. However, the molybdenum trioxide obtained by this method has problems in that it is difficult to reduce antimony (Sb) as an impurity or the effect of reduction is low, repeated purification is required to reduce the content of Sb, and the purification cost increases. In view of such problems, the present disclosure has an object to provide a method for producing molybdenum trioxide, which can reduce the Sb content. Solution for solving the problem The gist of the present disclosure includes the following. [1] A process for producing molybdenum trioxide, which comprises a step of mixing a raw material comprising a molybdenum compound or a hydrate thereof with chlorine gas, hydrogen chloride or a chloride, and a step of heating the obtained mixture at a temperature of 70 ℃ or higher. [2] A method for producing molybdenum trioxide, comprising a step of mixing a raw material comprising molybdenum trioxide, ammonium molybdate or a hydrate thereof with ammonium chloride, and a step of heating the obtained mixture at a temperature of 180 ℃ or higher. [3] A method for producing molybdenum trioxide, comprising a step of mixing a raw material comprising molybdenum trioxide, ammonium molybdate or a hydrate thereof with an aqueous solution containing ammonium chloride, and a step of heating the obtained mixture at a temperature of 180 ℃ or higher. [4] A process for producing molybdenum trioxide, which comprises mixing ammonia water with a raw material comprising molybdenum trioxide, ammonium molybdate or a hydrate thereof, then mixing hydrochloric acid, and heating the resulting mixture at a temperature of 180 ℃ or higher. [5] A process for producing molybdenum trioxide, which comprises mixing hydrochloric acid with a raw material comprising molybdenum trioxide, ammonium molybdate or a hydrate thereof, and then mixing ammonia water, and heating the resulting mixture at a temperature of 180 ℃ or higher. [6] The method for producing molybdenum trioxide according to any one of the above [1] to [5], wherein the Sb content in the produced molybdenum trioxide is 1/3 or less in terms of weight ratio to the Sb content contained in the raw material. [7] The method for producing molybdenum trioxide according to any one of the above [1] to [6], wherein the S content in the produced molybdenum tr