Method for producing non-oxide ceramic powders

Patent metadata

Field	Value
Publication number	US-11542204-B2
Application number	US-201816622312-A
Country	US
Kind code	B2
Filing date	Jun 7, 2018
Priority date	Jul 13, 2017
Publication date	Jan 3, 2023
Grant date	Jan 3, 2023

Abstract

The invention relates to a method for producing a non-oxide ceramic powder comprising a nitride, a carbide, a boride or at least one MAX phase with the general composition Mn+1AXn, where M=at least one element from the group of transition elements (Sc, Ti, V, Cr, Zr, Nb, Mo, Hf and Ta), A=at least one A group element from the group (Si, Al, Ga, Ge, As, Cd, In, Sn, Tl and Pb), X=carbon (C) and/or nitrogen (N) and/or boron (B), and n=1, 2 or 3. According to the invention, corresponding quantities of elementary starting materials or other precursors are mixed with at least one metal halide salt (NZ), compressed (pellet), and heated for synthesis with a metal halide salt (NZ). The compressed pellet is first enveloped with another metal halide salt, compressed again, arranged in a salt bath and heated therewith until the melting temperature of the salt is exceeded. Optionally, melted silicate can be added, which prevents the salt from evaporating at high temperatures. Advantageously, the method can be carried out in the presence of air.

First claim

The invention claimed is:

1. A method for producing a non-oxide ceramic powder comprising at least one nitride, one carbide, one boride or at least one MAX phase having the general composition M n+1 AX n , comprising
mixing stoichiometric quantities of elemental starting materials or other precursors comprising the necessary elements for forming the nitride, carbide, boride or at least one MAX phase with at least one metal halide salt to form a mixture;
compressing the mixture to form a compressed pellet
encapsulating the compressed pellet with at least one metal halide salt and compressing again to form an encapsulated pellet and then
heating the encapsulated pellet in a metal-halide salt bed;
wherein M=is at least one element selected from the group consisting of Sc, Ti, V, Cr, Zr, —Nb, Mo, Hf and Ta;
A=is at least one element selected from the group consisting of Si, Al, Ga, Ge, As, Cd, In, Sn, —Tl and Pb;
X is=C, N, B, or any combination thereof; and
n is=1, 2, or 3.

2. The method according to claim 1 , wherein the mixing of the starting materials or other precursors with the at least one metal halide salt takes place either in a non-reactive solvent or dry.

3. The method according to claim 1 , wherein the mixing takes place in a ball mill.

4. The method according to claim 1 , where the heating takes place at least up to a temperature which is above the melting temperature of the at least one metal halide salt used.

5. The method according to claim 1 , wherein the at least one metal halide salt comprises NZ, wherein N is=at least one element selected from the group consisting of Li, Na, K, Rb, Cs, Mg, Be, Ca, and Ba, and Z=is at least one element selected from the group consisting of F, Cl, Br, and I.

6. The method according to claim 1 , wherein the mixture comprising the elemental starting materials or other precursors and at least one metal halide salt is first compressed into the compressed pellet as a dry mixture.

7. The method according to claim 6 , wherein the mixture is first uniaxially and then cold-isostatically pressed to form a pellet.

8. The method according to claim 1 , wherein a pressure between 10 MPA and 1000 MPA, is applied during the first compressing step.

9. The method according to claim 1 , wherein a pressure between 10 MPA and 1000 MPA, is applied during the second compressing step.

10. The method according to claim 1 , wherein the encapsulated pellet is arranged in the metal-halide salt bed and is heated to temperatures above the melting temperature of the metal halide salt.

11. The method according to claim 1 , wherein the heating of the encapsulated pellet in the metal-halide salt bed takes place in the presence of oxygen.

12. The method according to claim 10 , wherein a molten metal-halide salt bed is produced and wherein the molten metal-halide salt bed comprises a molten silicate which floats as a layer on top of the molten metal-halide salt bed.

13. The method according to claim 12 , where the molten metal-halide salt bed and the molten silicate are heated to the same temperature before the molten silicate is added to the molten metal-halide salt bed.

14. The method according to claim 1 , further comprising cooling the encapsulated pellet in a metal-halide salt bed after the heating step, and subsequently dissolving the metal halide salt in a liquid.

15. The method according to the preceding claim 14 , wherein the metal halide salt is dissolved in water, an aqueous solution, or a short-chain alcohol.

Assignees

• Forschungszentrum Juelich Gmbh

Inventors

• Dash Apurv
• Gonzalez Jesus
• Vassen Robert
• Guillon Olivier

Classifications

• C01B35/04

  Metal borides · CPC title

• C04B2235/658

  Atmosphere during thermal treatment · CPC title

• C04B2235/404

  Refractory metals · CPC title

• C04B2235/5436

  micrometer sized, i.e. from 1 to 100 micron · CPC title

• C04B2235/3201

  Alkali metal oxides or oxide-forming salts thereof · CPC title