# US 12,759,041 B2 · Spherical niobium alloy powder, products containing the same, and methods of making the same

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- Number: US 12,759,041 B2
- Document ID: US12759041B2
- Status: Granted
- Kind: B2
- Application number: 17/299,799
- Filed: 2019-12-06
- Published: 2022-01-27
- Granted: 2026-10-13
- Earliest claimed: 2018-12-12
- Assignees: Global Advanced Metals USA, Inc.
- Applicants: Global Advanced Metals USA, Inc.
- Inventors: Craig M. Sungail; Aamir Dawood Abid
- Web page: https://patentgrep.com/patent/US12759041B2

## CPC

- B22F 1/142: Thermal or thermo-mechanical treatment
- B22F 1/052: characterised by a mixture of particles of different sizes or by the particle size distribution
- B22F 1/065: Spherical particles
- 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 10/25: Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
- B22F 10/28: Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
- B33Y 40/10: Pre-treatment
- B33Y 70/00: Materials specially adapted for additive manufacturing
- C22C 27/02: Alloys based on vanadium, niobium, or tantalum
- B22F 10/22: Direct deposition of molten metal
- B22F 10/36: of energy beam parameters
- B22F 10/366: Scanning parameters, e.g. hatch distance or scanning strategy
- B22F 10/62: by chemical means
- B22F 10/66: by mechanical means
- B22F 10/73: of powder
- B22F 2301/20: Refractory metals
- B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy
- B22F 2201/10: Inert 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
- 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
- C22C: ALLOYS (treatment of alloys C21D, C22F)

## Abstract

Niobium alloy powder that is highly spherical is described. The niobium alloy powder can be useful in additive manufacturing and other uses. Methods to make the niobium alloy powder are further described as well as methods to utilize the niobium alloy powder in additive manufacturing processes. Resulting products and articles using the niobium alloy powder are further described.

## Claims

### Claim 1

Niobium alloy powder comprising
a. a spherical shape wherein the powder has an average aspect ratio of from 1.0 to 1.25;
b. a purity of niobium alloy of at least 99.99 wt % Nb-alloy based on total weight of said niobium alloy powder, excluding gas impurities;
c. an average particle size of from about 0.5 micron to about 250 microns;
d. an apparent density from about 2 g/cc to about 18 g/cc;
e. a true density of from 8.2 g/cc to 20 g/cc; and
f. a Hall flow rate of 20 sec or less, wherein
said niobium alloy powder is a Nb alloy that contains Nb and two or more other metals to form said niobium alloy powder,
the niobium metal is present at a highest percent based on the weight of the niobium alloy powder, and
a wt % of the two or more other metals is from 0.1 wt % to 70 wt %, based on the total weight of the niobium alloy powder;
and wherein the two or more other metals must be and only can be Ti, W, Mo, Re, Rh, Ta, V, Th, Zr, Hf, Cr, Mn, Sc, Y, Ni, Fe, Co, Al, Sn, Au, Th, U, Pu, and rare earth elements, and, optionally, a wt % of metals other than the two or more other metals and the Nb is less than 0.1 wt %.

### Claim 2 (depends on 1)

The niobium alloy powder of claim 1, wherein said niobium alloy powder is plasma heat-treated.

### Claim 3 (depends on 1)

The niobium alloy powder of claim 1, wherein said niobium alloy powder wherein said average aspect ratio is from 1.0 to 1.05.

### Claim 4 (depends on 1)

The niobium alloy powder of claim 1, wherein said average particle size is from about 0.5 micron to about 10 microns.

### Claim 5 (depends on 1)

The niobium alloy powder of claim 1, wherein said average particle size is from about 5 microns to about 25 microns.

### Claim 6 (depends on 1)

The niobium alloy powder of claim 1, wherein said average particle size is from about 105 microns to about 250 microns.

### Claim 7 (depends on 1)

The niobium alloy powder of claim 1, wherein said niobium alloy powder has at least one of the following properties:
a. a D10 size of from about 5 microns to 25 microns;
b. a D90 size of from about 20 microns to 80 microns; or
c. oxygen between 10 ppm to 1000 ppm.

### Claim 8 (depends on 1)

An article comprising the niobium alloy powder of claim 1.

### Claim 9 (depends on 8)

The article of claim 8, wherein said article is a boss for a coil set for a physical vapor deposition process.

### Claim 10 (depends on 9)

The article of claim 9, wherein said boss comprises open cellular structures and solid structures.

### Claim 11 (depends on 8)

The article of claim 8, wherein said article is a coil set or part thereof for a physical vapor deposition process.

### Claim 12 (depends on 8)

The article of claim 8, wherein said article is an orthopedic implant or part thereof wherein said orthopedic implant comprises open cellular structures and solid structures.

### Claim 13 (depends on 8)

The article of claim 8, wherein said article is a dental implant wherein said dental implant comprises open cellular structures and solid structures.

### Claim 14 (depends on 8)

The article of claim 8, wherein said article is a radiation shielding component.

### Claim 15 (depends on 8)

The article of claim 8, wherein said article is a superconducting cavity.

### Claim 16 (depends on 1)

A method for forming an article, said method comprising additive manufacturing said article by utilizing the niobium alloy powder of claim 1 to form the shape of said article or part thereof.

### Claim 17 (depends on 1)

A method to make to the niobium alloy powder of claim 1, said method comprising:
a. plasma heat-treating a starting niobium alloy powder to at least partially melt at least an outer surface of said starting niobium alloy powder in an inert atmosphere to obtain a heat-treated niobium alloy powder, and
b. cooling said heat-treated niobium alloy powder in an inert atmosphere to obtain said niobium alloy powder.

### Claim 18 (depends on 17)

The method of claim 17, wherein said starting niobium alloy powder has a first particle size distribution, and said niobium alloy powder has a second particle size distribution, and said first particle size distribution and said second particle size distribution are within 10% of each other.

### Claim 19 (depends on 17)

The method of claim 17, wherein prior to step a, the starting niobium alloy powder is formed by sintering a first niobium alloy powder to obtain a sintered powder, and then e-beam melting of said sintered powder to obtain an ingot, and then reducing said ingot to said starting niobium alloy powder.

### Claim 20 (depends on 1)

The niobium alloy powder of claim 1, wherein said purity is at least 99.995 wt. % Nb-alloy.

### Claim 21 (depends on 1)

The niobium alloy powder of claim 1, wherein the niobium alloy powder has an iron content of from about 1 ppm to 5 ppm.

### Claim 22 (depends on 1)

The niobium alloy powder of claim 1, wherein said niobium alloy powder has an oxygen level of less than 400 ppm, an oxygen in ppm to BET in m2/g ratio is from 2,000 to 4,000, and the niobium metal is present at from 30 wt % to 99.9 wt %, based on the total weight of the niobium alloy powder, wherein the two or more other metals are selected from Ti, W, Mo, Re, Rh, Ta, V, Th, Zr, Hf, Cr, Mn, Sc, Y, Ni, Fe, Co, Al, Sn, Au, Th, U, Pu, and rare earth elements.

### Claim 23 (depends on 22)

The niobium alloy powder of claim 22, wherein said niobium alloy powder has an oxygen level of less than 300 ppm.

### Claim 24 (depends on 1)

The niobium alloy powder of claim 1, wherein the niobium alloy powder has a single phase.

### Claim 25

Niobium alloy powder comprising
a. a spherical shape wherein the powder has an average aspect ratio of from 1.0 to 1.25;
b. a purity of niobium alloy of at least 99.99 wt % Nb-alloy based on total weight of said niobium alloy powder, excluding gas impurities;
c. an average particle size of from about 0.5 micron to about 250 microns;
d. an apparent density from about 2 g/cc to about 18 g/cc;
e. a true density of from 8.2 g/cc to 20 g/cc; and
f. a Hall flow rate of 20 sec or less, wherein
said niobium alloy powder is a Nb alloy that contains at least 65.5 wt % Nb, based on the total weight of the niobium alloy powder, and two or more other metals to form said niobium alloy powder;
and wherein said niobium alloy powder has an oxygen level of less than 400 ppm, an oxygen in ppm to BET in m2/g ratio is from 2,000 to 4,000, and the two or more other metals are selected from Ti, W, Mo, Re, Rh, Ta, V, Th, Zr, Hf, Cr, Mn, Sc, Y, Ni, Fe, Co, Al, Sn, Au, Th, U, Pu, and rare earth elements.