# US 11,993,829 B2 · Powders based on niobium-tin compounds for producing superconductive components

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- Number: US 11,993,829 B2
- Document ID: US11993829B2
- Status: Granted
- Kind: B2
- Application number: 17/427,920
- Filed: 2020-02-05
- Published: 2022-04-21
- Granted: 2024-05-28
- Earliest claimed: 2019-02-08
- Assignees: Taniobis GmbH
- Applicants: Taniobis GmbH
- Inventors: Holger Brumm; Markus Weinmann; Christoph Schnitter
- Web page: https://patentgrep.com/patent/US11993829B2

## CPC

- B22F 9/22: using gaseous reductors
- B22F 1/05: Metallic powder characterised by the size or surface area of the particles
- B22F 1/145: Chemical treatment, e.g. passivation or decarburisation
- B22F 1/148: Agglomerating
- B22F 3/20: by extruding
- 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 10/34: of powder characteristics, e.g. density, oxidation or flowability
- B33Y 70/00: Materials specially adapted for additive manufacturing
- C22C 13/00: Alloys based on tin
- C22C 21/04: Modified aluminium-silicon alloys
- C22C 21/08: with silicon
- C22C 21/10: with zinc as the next major constituent
- C22C 27/02: Alloys based on vanadium, niobium, or tantalum
- B22F 1/065: Spherical particles
- B22F 5/12: of wires {(of tubes B22F5/10)}
- B22F 9/082: {atomising using a fluid (using centrifugal force B22F9/10)}
- 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]
- B22F 10/73: of powder
- B22F 2301/20: Refractory metals
- B22F 2304/058: Particle size above 300 nm up to 1 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
- C22C: ALLOYS (treatment of alloys C21D, C22F)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A powder for the production of a superconducting component. The powder includes NbxSny, where 1≤x≤6 and 1≤y≤5, and three-dimensional agglomerates having a particle size D90 of less than 400 μm, as determined via a laser light scattering. The three-dimensional agglomerates have primary particles which have an average particle diameter of less than 15 μm, as determined via a scanning electron microscopy, and pores of which at least 90% have a diameter of from 0.1 to 20 μm, as determined via a mercury porosimetry.

## Claims

### Claim 1

A powder for the production of a superconducting component, the powder comprising:
a proportion of Nb3Sn of >90% based on all crystallographic phases detected as determined via a Rietveld analysis of an X-ray powder diffraction pattern of the powder, or
a proportion of Nb6Sn5 of >90% based on all crystallographic phases detected as determined via a Rietveld analysis of an X-ray powder diffraction pattern of the powder, or
a proportion of NbSn2 of >90% based on all crystallographic phases detected as determined via a Rietveld analysis of an X-ray powder diffraction pattern of the powder; and
three-dimensional agglomerates having a particle size D90 of less than 400 μm, as determined via a laser light scattering, the three-dimensional agglomerates comprising,
primary particles having an average particle diameter of less than 15 μm, as determined via a scanning electron microscopy, and
pores of which at least 90% have a diameter of from 0.1 to 20 μm, as determined via a mercury porosimetry.

### Claim 2 (depends on 1)

The powder as recited in claim 1, wherein,
the proportion of Nb3Sn is ≥93% based on all crystallographic phases detected as determined via the Rietveld analysis of the X-ray powder diffraction pattern of the powder, or
the proportion of Nb6Sn5 is ≥94% based on all crystallographic phases detected as determined via the Rietveld analysis of the X-ray powder diffraction pattern of the powder, or
the proportion of NbSn2 is ≥94% based on all crystallographic phases detected as determined via a Rietveld analysis of an X-ray powder diffraction pattern of the powder.

### Claim 3 (depends on 1)

The powder as recited in claim 1, wherein the powder further comprises a specific surface area of from 0.5 to 5 m2/g as determined by a BET method.

### Claim 4 (depends on 1)

The powder as recited in claim 1, wherein the powder further comprises:
an oxygen content of less than 1.8 wt. % based on a total weight of the powder.

### Claim 5 (depends on 1)

The powder as recited in claim 1, wherein,
the three-dimensional agglomerates of the powder are subjected to a milling step in an oxygen-free environment so as to provide milled three-dimensional agglomerates, and
after the milling step, the milled three-dimensional agglomerates have a particle size D99 of less than 15 μm as determined via a laser light scattering.

### Claim 6 (depends on 1)

The powder as recited in claim 1, wherein the powder further comprises:
a proportion of metallic tin of less than 3%, based on all crystallographic phases detected as determined via a Rietveld analysis of an X-ray diffraction pattern of the powder.

### Claim 7 (depends on 1)

The powder as recited in claim 1, wherein,
the powder is subjected to an atomization step after which the powder further comprises powder particles, and
95% of all of the powder particles have a Feret diameter of from 0.7 to 1, the Feret diameter being a smallest diameter of a particle of the powder particles divided by a greatest diameter of the particle of the powder particles as determined via an evaluation of SEM images.

### Claim 8 (depends on 1)

A process for producing the powder as recited in claim 1, the process comprising:
obtaining a niobium metal powder via a reduction of niobium oxide using a gaseous reducing agent; and
reacting the niobium metal powder with a tin metal powder.

### Claim 9 (depends on 8)

The process as recited in claim 8, wherein the obtaining of the niobium metal powder via the reduction of niobium oxide using the gaseous reducing agent and the reacting of the niobium metal powder with the tin metal powder is performed in a combined process step.

### Claim 10 (depends on 8)

The process as recited in claim 8, wherein the niobium metal powder comprises pores having a size of from 0.1 to 20 μm, as determined via a mercury porosimetry.

### Claim 11 (depends on 8)

The process as recited in claim 8, wherein the niobium metal powder comprises three-dimensional agglomerates having a size with a D90 of less than 400 μm, as determined via a laser light scattering, and the three-dimensional agglomerates comprise primary particles having an average particle diameter of less than 10 μm, as determined via a scanning electron microscopy.

### Claim 12 (depends on 8)

The process as recited in claim 8, wherein the niobium metal powder has a bimodal distribution of a pore size.

### Claim 13 (depends on 8)

The process as recited in claim 8, wherein the niobium oxide is a compound selected from the group consisting of Nb2O5, NbO2, NbO, and mixtures thereof.

### Claim 14 (depends on 8)

The process as recited in claim 8, wherein the gaseous reducing agent is magnesium vapor.

### Claim 15 (depends on 8)

The process as recited in claim 8, wherein the niobium metal powder further comprises at least one dopant.

### Claim 16 (depends on 1)

A method of using the powder as recited in claim 1 for producing a superconducting component, the method comprising:
providing the powder as recited in claim 1; and
producing at least one of a superconducting wire and a superconducting coil as the superconducting component using the powder.

### Claim 17 (depends on 16)

The method of using as recited in claim 16, wherein the superconducting component is produced via a powder-metallurgical process.

### Claim 18 (depends on 17)

The method of using as recited in claim 17, wherein the powder-metallurgical process is a PIT process or an additive manufacturing process.

### Claim 19 (depends on 1)

A method of using the powder as recited in claim 1 in an additive manufacturing process, the method comprising:
providing the powder as recited in claim 1; and
using the powder in the additive manufacturing process,
wherein,
the additive manufacturing process is a laser beam melting, an electron beam melting, or a laser cladding.

### Claim 20 (depends on 1)

A method of using the powder as recited in claim 1 in a powder-metallurgical process, the method comprising:
providing the powder as recited in claim 1; and
using the powder in the powder-metallurgical process.