# US 11,077,497 B2 · Deoxidation of metal powders

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- Number: US 11,077,497 B2
- Document ID: US11077497B2
- Status: Granted
- Kind: B2
- Application number: 15/852,211
- Filed: 2017-12-22
- Published: 2018-12-13
- Granted: 2021-08-03
- Earliest claimed: 2017-06-07
- Assignees: Global Titanium Inc.
- Applicants: Global Titanium Inc.
- Inventors: Charles A. Motchenbacher; Robert L. Swenson; Jesse Z. Oliver
- Web page: https://patentgrep.com/patent/US11077497B2

## CPC

- 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 1/065: Spherical particles
- B22F 1/145: Chemical treatment, e.g. passivation or decarburisation
- B33Y 70/00: Materials specially adapted for additive manufacturing
- B22F 10/20: Direct sintering or melting
- B22F 2201/20: Use of vacuum
- B22F 2301/205: Titanium, zirconium or hafnium
- B22F 2304/10: Micron size particles, i.e. above 1 micrometer up to 500 micrometer
- B22F 2998/10: Processes characterised by the sequence of their steps
- B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy
- Y02P 10/25: Process efficiency
- 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
- B33Y: ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Systems, methods, and compositions disclosed herein provide for low-oxygen metal powders. These metal powders, such as very-fine powders and spherical powders of titanium and titanium alloys, can be effectively deoxidized through use of vapor deoxidation without requiring the powder to undergo re-sizing or re-shaping subsequent to the deoxidation. Systems, methods, and compositions in accordance with the present disclosure can produce low-cost, low-oxygen, metal powders, such as very-fine powders and spherical powders of, for example, titanium and titanium alloys. Moreover, systems, methods, and compositions in accordance with the present disclosure can provide for reducing the number of processes or cost of processes required to produce these low-oxygen metal powders.

## Claims

### Claim 1

A method comprising:
obtaining a high-oxygen very-fine powder including titanium;
adding an amount of deoxidant to the high-oxygen very-fine powder to thereby produce a powder blend;
applying a vacuum to the powder blend;
heating the powder blend to a predetermined temperature sufficient to at least partially vaporize the deoxidant at a pressure of the vacuum to produce a vaporized deoxidant;
vapor deoxidizing the high-oxygen very-fine powder using the vaporized deoxidant to produce a low-oxygen very-fine powder and an oxidized deoxidant;
wherein the low-oxygen very-fine powder has an oxygen content less than the high-oxygen very-fine powder;
maintaining the powder blend at the predetermined temperature for a predetermined time to produce a very-fine-powder cake, the very-fine-powder cake including the low-oxygen very-fine powder and the oxidized deoxidant, the low-oxygen very-fine powder including the titanium, the predetermined time being sufficient to convert the high-oxygen very-fine powder to the low-oxygen very-fine powder;
milling the very-fine-powder cake to produce a low-oxygen very-fine-powder blend; and
removing the oxidized deoxidant from the low-oxygen very-fine-powder blend to thereby produce the low-oxygen very-fine powder.

### Claim 2 (depends on 1)

The method of claim 1, wherein the low-oxygen very-fine powder has an oxygen content of less than about 2000 parts-per-million.

### Claim 3 (depends on 1)

The method of claim 1, wherein the low-oxygen very-fine powder has an oxygen content of less than about 1300 parts-per-million.

### Claim 4

A method comprising:
obtaining a high-oxygen spherical powder including titanium, the high-oxygen spherical powder defining a first particle-size distribution;
adding an amount of deoxidant to the high-oxygen spherical powder to thereby produce a powder blend;
applying a vacuum to the powder blend;
heating the powder blend to a predetermined temperature sufficient to at least partially vaporize the deoxidant at a pressure of the vacuum to produce a vaporized deoxidant;
vapor deoxidizing the high-oxygen spherical powder using the vaporized deoxidant to produce a low-oxygen spherical powder and an oxidized deoxidant;
wherein the low-oxygen spherical powder has an oxygen content less than the high-oxygen spherical powder; and
maintaining the powder blend at the predetermined temperature for a predetermined time to produce a spherical-powder cake, the spherical-powder cake including the low-oxygen spherical powder and the oxidized deoxidant, the low-oxygen spherical powder including the titanium, the low-oxygen spherical powder defining a second particle-size distribution that is substantially equal to the first particle-size distribution, the predetermined time being sufficient to convert the high-oxygen spherical powder to the low-oxygen spherical powder;
milling the spherical-powder cake to produce a low-oxygen spherical-powder blend; and
removing the oxidized deoxidant from the low-oxygen spherical-powder blend to thereby produce the low-oxygen spherical powder.

### Claim 5 (depends on 4)

The method of claim 4, wherein the low-oxygen spherical powder has an oxygen content of less than about 1300 parts-per-million.

### Claim 6 (depends on 4)

The method of claim 4, wherein the low-oxygen spherical powder has an oxygen content of less than about 1100 parts-per-million.

### Claim 7 (depends on 4)

The method of claim 4, wherein the low-oxygen spherical powder has an oxygen content of less than about 800 parts-per-million.

### Claim 8 (depends on 4)

The method of claim 4, wherein the low-oxygen spherical powder has an oxygen content of less than about 500 parts-per-million.

### Claim 9 (depends on 4)

The method of claim 4, wherein the predetermined temperature is less than about 1700° F.

### Claim 10 (depends on 4)

The method of claim 4, wherein the predetermined temperature is less than about 1500° F.

### Claim 11 (depends on 4)

The method of claim 4, wherein the low-oxygen spherical powder has an oxygen content of less than about 2,000 parts-per-million such that the low-oxygen spherical powder is configured for use in additive manufacturing processes without further alteration to physical properties of the low-oxygen spherical powder.

### Claim 12 (depends on 4)

The method of claim 4, wherein the high-oxygen spherical powder defines an average particle size of less than about 105 μm.

### Claim 13 (depends on 4)

The method of claim 4, wherein the high-oxygen spherical powder defines an average particle size of less than about 63 μm.

### Claim 14 (depends on 4)

The method of claim 4, wherein the high-oxygen spherical powder defines an average particle size of less than about 45 μm.

### Claim 15 (depends on 4)

The method of claim 4, wherein the high-oxygen spherical powder defines an average particle size of less than about 25 μm.

### Claim 16

A method comprising:
obtaining a high-oxygen spherical powder including titanium;
wherein the high-oxygen spherical powder includes spent powder from an additive manufacturing process;
adding an amount of deoxidant to the high-oxygen spherical powder to thereby produce a powder blend;
applying a vacuum to the powder blend;
heating the powder blend to a predetermined temperature sufficient to at least partially vaporize the deoxidant at a pressure of the vacuum to produce a vaporized deoxidant;
vapor deoxidizing the high-oxygen spherical powder using the vaporized deoxidant to produce a low-oxygen spherical powder and an oxidized deoxidant;
wherein the low-oxygen spherical powder has an oxygen content less than the high-oxygen spherical powder;
maintaining the powder blend at the predetermined temperature for a predetermined time to produce a spherical-powder cake, the spherical-powder cake including the low-oxygen spherical powder and the oxidized deoxidant, the low-oxygen spherical powder including the titanium, the predetermined time being sufficient to convert the high-oxygen spherical powder to the low-oxygen spherical powder;
milling the spherical-powder cake to produce a low-oxygen spherical-powder blend; and
removing the oxidized deoxidant from the low-oxygen spherical-powder blend to thereby produce the low-oxygen spherical powder.

### Claim 17 (depends on 16)

The method of claim 16, wherein the low-oxygen spherical powder has an oxygen content of less than about 2000 parts-per-million.