# US 10,373,764 B2 · Process for manufacturing agglomerated particles of tantalum, mixed tantalum powder and process for manufacturing same, tantalum pellet and process for manufacturing same, and capacitor

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- Number: US 10,373,764 B2
- Document ID: US10373764B2
- Status: Granted
- Kind: B2
- Application number: 15/792,785
- Filed: 2017-10-25
- Published: 2018-02-15
- Granted: 2019-08-06
- Earliest claimed: 2009-05-15
- Assignees: Global Advanced Metals USA, Inc.
- Applicants: Global Advanced Metals USA, Inc.
- Inventors: Ryosuke Matsuoka; Eiji Kataoka; Yoshikazu Noguchi; John Koenitzer; Sridhar Venigalla
- Web page: https://patentgrep.com/patent/US10373764B2

## CPC

- H01G 9/0525: {Powder therefor}
- B22F 1/148: Agglomerating
- H01G 9/052: Sintered electrodes
- B22F 2998/10: Processes characterised by the sequence of their steps
- B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy
- H01G 9/15: Solid electrolytic capacitors (H01G11/00 takes precedence)
- 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

## Abstract

A method for producing agglomerated tantalum particles, comprising: a step for grinding secondary tantalum particles, which are obtained by reducing a tantalum salt, and adding water thereto to give a water-containing mass; a step for drying said water-containing mass to give a dry mass; a step for sieving said dry mass to give spherical particles; and a step for heating said spherical particles. A mixed tantalum powder comprising a mixture of agglomerated tantalum particles (X) with agglomerated tantalum particles (Y), wherein said agglomerated tantalum particles (X) show a cumulative percentage of particles with particle size of 3 μm or less of 5 mass % or less after 25 W ultrasonic radiation for 10 min, while said agglomerated tantalum particles (Y) show a cumulative percentage of particles with particle size of 3 μm or less of 10 mass % or more after 25 W ultrasonic radiation for 10 min.

## Claims

### Claim 1

A process for manufacturing a mixed tantalum powder including the steps of:
obtaining agglomerated tantalum particles (X) using the manufacturing process (a) described below;
obtaining agglomerated tantalum particles (Y) using any manufacturing process among the manufacturing processes (b)-(d) described below; and mixing the resultant agglomerated tantalum particles (X) and agglomerated tantalum particles (Y),
manufacturing process (a):
a process for manufacturing agglomerated particles of tantalum including the steps of: obtaining hydrated aggregates by stirring secondary particles of tantalum produced by tantalum salt reduction while adding water thereto in a granulating apparatus provided with a low-speed impeller and a high-speed impeller rotating at a rotational speed that is at least 10 times higher than that of the low-speed impeller; further stirring the hydrated aggregates in the granulating apparatus without adding water; and, after that, obtaining dry aggregates by drying the hydrated aggregates, and sintering the dry aggregates,
manufacturing process (b):
a process for manufacturing agglomerated particles of tantalum including the steps of: obtaining hydrated aggregates by stirring secondary particles of tantalum produced by tantalum salt reduction while adding water thereto in a granulating apparatus provided with a low-speed impeller and a high-speed impeller rotating at a rotational speed that is at least 10 times higher than that of the low-speed impeller; and, after that, obtaining dry aggregates by drying the hydrated aggregates; spheronizing the dry aggregates by passing them through screens; and sintering the spheronized dry aggregates,
manufacturing process (c):
a process for manufacturing agglomerated particles of tantalum including the steps of: obtaining hydrated aggregates by adding water to secondary particles of tantalum produced by tantalum salt reduction and pulverizing them in a pulverizing machine other than the above granulating apparatus; and, after that, obtaining dry aggregates by drying the hydrated aggregates; spheronizing the dry aggregates by passing them through screens; and sintering the spheronized dry aggregates,
manufacturing process (d):
a process for manufacturing agglomerated particles of tantalum including the steps of: obtaining hydrated aggregates by adding water to secondary particles of tantalum obtained by tantalum salt reduction; and, after that, obtaining dry aggregates by drying the hydrated aggregates; obtaining sintered aggregates by sintering the dry aggregates; and micronizing the sintered aggregates.

### Claim 2 (depends on 1)

The process for manufacturing a mixed tantalum powder according to claim 1, wherein the step of obtaining the agglomerated tantalum particles (Y) is the manufacturing process (b) described above and, in addition, in the step of obtaining hydrated aggregates in the manufacturing process (b), stirring in the granulating apparatus is accomplished simultaneously with the addition of water.

### Claim 3 (depends on 1)

The process for manufacturing a mixed tantalum powder according to claim 1, wherein a deoxidation treatment step is included after the step of mixing the agglomerated tantalum particles (X) with the agglomerated tantalum particles (Y).

### Claim 4 (depends on 1)

The process for manufacturing a mixed tantalum powder according to claim 1, wherein either one or both of the steps of deoxidizing agglomerated tantalum particles (X) and deoxidizing agglomerated tantalum particles (Y) are included prior to the step of mixing the agglomerated tantalum particles (X) with the agglomerated tantalum particles (Y).

### Claim 5 (depends on 1)

A process for manufacturing tantalum pellets involving molding a mixed tantalum powder manufactured in accordance with the process for manufacturing a mixed tantalum powder according to claim 1.

### Claim 6

A mixed tantalum powder containing a mixture of the following agglomerated tantalum particles (X) and agglomerated tantalum particles (Y),
agglomerated tantalum particles (X):
agglomerated tantalum particles, wherein the cumulative fraction of particles with a particle size of 3 μm or less after a 10-minute irradiation with 25-Watt ultrasound is 5 wt % or less,
agglomerated tantalum particles (Y):
agglomerated tantalum particles, wherein the cumulative fraction of particles with a particle size of 3 μm or less after a 10-minute irradiation with 25-Watt ultrasound is 10 wt % or more.

### Claim 7 (depends on 6)

A tantalum pellet obtained by molding the mixed tantalum powder according to claim 6.