# US 2016/0254100 A1 · Niobium granulated powder production method

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- Number: US 2016/0254100 A1
- Document ID: US20160254100A1
- Status: Published application
- Kind: A1
- Application number: 15/027,794
- Filed: 2014-10-07
- Published: 2016-09-01
- Earliest claimed: 2013-10-08
- Assignees: Showa Denko K.K.
- Applicants: Showa Denko K.K.
- Inventors: Yoshinori SHIBUYA; Yasuo TSUMITA; Toshiya KAWASAKI
- Web page: https://patentgrep.com/patent/US20160254100A1

## CPC

- H01G 9/0525: {Powder therefor}
- B22F 1/142: Thermal or thermo-mechanical treatment
- B22F 1/148: Agglomerating
- B22F 9/04: starting from solid material, e.g. by crushing, grinding or milling ({C22C1/1084 takes precedence}; crushing, grinding or milling, in general, see the relevant subclasses, e.g. B02C)
- B22F 9/20: starting from solid metal compounds
- C22C 27/02: Alloys based on vanadium, niobium, or tantalum
- H01G 9/052: Sintered electrodes
- B22F 2009/041: {by mechanical alloying, e.g. blending, milling}
- B22F 2009/043: {by ball milling}
- B22F 2302/25: Oxide
- B22F 2304/058: Particle size above 300 nm up to 1 micrometer
- H01G: CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE (selection of specified materials as dielectric H01B3/00; capacitors having potential barriers H10D1/62, H10K10/10)
- 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
- C22C: ALLOYS (treatment of alloys C21D, C22F)

## Abstract

A method of producing a niobium granulated powder, including the steps of: mixing niobium hydride and a metal oxide by a mechanical alloying method to produce a mechanical alloy; pulverizing the mechanical alloy; subjecting the pulverized mechanical alloy to heat treatment to allow the pulverized mechanical alloy to aggregate, to thereby form a granulated product. Also disclosed is a sintered body of the niobium granulated powder, an anode body produced from the sintered body and a capacitor including the sintered body.

## Claims

### Claim 1

A method of producing a niobium granulated powder, comprising the steps of:
mixing niobium hydride and a metal oxide by a mechanical alloying method to produce a mechanical alloy;
pulverizing the mechanical alloy;
subjecting the pulverized mechanical alloy to heat treatment to allow the pulverized mechanical alloy to aggregate, to thereby form a granulated product.

### Claim 2 (depends on 1)

The method of producing a niobium granulated powder according to claim 1, in which the metal oxide to be used includes a metal oxide represented by a composition formula M2O3, where M represents a metal element which can be a trivalent cation.

### Claim 3 (depends on 2)

The method of producing a niobium granulated powder according to claim 2, in which M represents one or more kinds selected from scandium, yttrium, lanthanoids, and actinoids.

### Claim 4 (depends on 3)

The method of producing a niobium granulated powder according to claim 3, in which M represents yttrium.

### Claim 5 (depends on 1)

The method of producing a niobium granulated powder according to claim 1, in which the niobium granulated powder has an atomic ratio of niobium to a metal element derived from the metal oxide falling within a range of from 997:3 to 970:30.

### Claim 6 (depends on 1)

The method of producing a niobium granulated powder according to claim 1, in which the niobium hydride to be used is composed of powder having passed through a sieve having an opening of 1 mm.

### Claim 7 (depends on 1)

The method of producing a niobium granulated powder according to claim 1, in which a stirring ball mill is used for mixing niobium hydride and a metal oxide.

### Claim 8 (depends on 1)

The method of producing a niobium granulated powder according to claim 1, comprising, after the mixing niobium hydride and a metal oxide, pulverizing the mixture so that a D50 value, which is a 50% particle size in a volume-based cumulative particle size distribution, measured with a laser diffraction particle size distribution analyzer is 0.7 μm or less.

### Claim 9 (depends on 1)

The method of producing a niobium granulated powder according to claim 1, in which an alkaline earth metal oxide is used as a pore forming material in the case of subjecting the mechanical alloy to heat treatment to thereby form a granulated product.

### Claim 10 (depends on 1)

A sintered body of the niobium granulated powder obtained by the production method claimed in claim 1.

### Claim 11 (depends on 10)

An anode body, which is produced from the sintered body claimed in claim 10.

### Claim 12 (depends on 10)

A capacitor, comprising the sintered body claimed in claim 10 as an anode.