# US 4,397,682 A · Process for preparing metals from their fluorine-containing compounds

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- Number: US 4,397,682 A
- Document ID: US4397682A
- Status: Granted
- Kind: A
- Application number: 06/319,956
- Filed: 1981-11-10
- Granted: 1983-08-09
- Earliest claimed: 1980-11-18
- Assignees: Solex Research Corporation
- Inventors: Morio Watanabe; Sanji Nishimura; Nobuatsu Watanabe
- Web page: https://patentgrep.com/patent/US4397682A

## CPC

- B22F 9/22: using gaseous reductors
- C01B 9/08: Fluorides
- C22B 5/12: by gases
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS

## Abstract

A process for preparing high purity superfine powders of less than 0.5.mu. diameter of Mo, W, Nb, Zr, Cu, Zn, Co, Ni and In by first producing their fluoride or a double fluoride with ammonium and then decomposing them under heat in a hydrogen-containing stream. Features of the present process are that the double fluoride of the metals with ammonium is faster in crystal growth than their fluoride, recrystallization of these salts can be repeated as desired when a high purity of the metals is required, and particles of a uniform size can be obtained easier.

## Claims

### Claim 1

A process for preparing high purity metals of Mo, W, Zr, Nb, Cu, Zn, Co, Ni and In from fluorine-containing compounds comprising,
heating an ammonium fluoride of said metal in a hydrogen-containing stream.

### Claim 2

A process for preparing high purity metals of Mo, W, Zr, Nb, Cu, Zn, Co, Ni and In from fluorine-containing compounds comprising,
heating an ammonium fluoride of said metal in a hydrogen-containing stream wherein the metal fluoride and the metal ammonium fluoride are prepared from an organic solvent solution of an extracted simple or complex ion of a metal selected from the group consisting of Mo, W, Zr, Nb, Cu, Zn, Co, Ni and In, where the organic solvent is one or more extracting agents selected from the group consisting of alkyl phosphoric acids, dialkyldithiophosphoric acids, diaryldithiophosphoric acids, hydroxyoximes, ketones, neutral phosphoric acid esters, carboxylic acids, and primary to quarternary amines, and diluted with a petroleum hydrocarbon, by bringing into contact with an aqueous solution containing one or more compounds selected from the group consisting of HF, NH.sub.4 HF.sub.2 and NH.sub.4 F.