Refractory metal silicide nanoparticle ceramics

Patent metadata

Field	Value
Publication number	US-11339097-B2
Application number	US-201816216279-A
Country	US
Kind code	B2
Filing date	Dec 11, 2018
Priority date	May 3, 2016
Publication date	May 24, 2022
Grant date	May 24, 2022

Abstract

Particles of a refractory metal or a refractory-metal compound capable of decomposing or reacting into refractory-metal nanoparticles, elemental silicon, and an organic compound having a char yield of at least 60% by weight are combined to form a precursor mixture. The mixture is heating, forming a thermoset and/or metal nanoparticles. Further heating form a composition having nanoparticles of a refractory-metal silicide and a carbonaceous matrix. The composition is not in the form of a powder

First claim

What is claimed is:

1. A composition comprising:
a metal component selected from:
particles of a refractory metal; and
a refractory-metal compound capable of decomposing into refractory-metal nanoparticles;

elemental silicon; and
an organic component selected from:
an organic compound having a char yield of at least 60% by weight; and
a thermoset made from the organic compound.

2. The composition of claim 1 , wherein the refractory metal is titanium, zirconium, hafnium, molybdenum, tungsten, niobium, tantalum, or vanadium.

3. The composition of claim 1 , wherein the metal component is a salt, a hydride, a carbonyl compound, a halide, or particles of the refractory metal.

4. The composition of claim 1 , wherein the organic compound:
contains only carbon and hydrogen;
contains aromatic and acetylene groups;
contains only carbon, hydrogen, and nitrogen;
contains no oxygen; or
contains a heteroatom other than oxygen.

5. The composition of claim 1 , wherein the organic compound is 1,2,4,5-tetrakis(phenylethynyl)benzene or a prepolymer thereof.

6. The composition of claim 1 , wherein the composition is milled.

7. A method comprising:
combining particles of a refractory metal or a refractory-metal compound capable of decomposing or reacting into refractory-metal nanoparticles, elemental silicon, and an organic compound having a char yield of at least 60% by weight to form a precursor mixture.

8. The method of claim 7 , further comprising:
milling the precursor mixture.

9. The method of claim 7 , further comprising:
placing the precursor mixture into a mold or shaped reactor.

10. The method of claim 7 , further comprising:
heating the precursor mixture in an inert atmosphere or vacuum at a temperature that causes decomposition or reaction of the refractory-metal compound or particles to form refractory-metal nanoparticles to form a metal nanoparticle composition.

11. The method of claim 10 , wherein heating the precursor mixture causes polymerization of the organic compound to a thermoset.

12. The method of claim 10 , further comprising:
heating the metal nanoparticle composition in an inert atmosphere or vacuum at a temperature that causes formation of a ceramic comprising nanoparticles of a refractory-metal silicide in a carbonaceous matrix.

13. The method of claim 12 , wherein heating the metal nanoparticle composition causes formation of nanoparticles comprising a carbide of the refractory metal, a nitride of the refractory metal, or silicon carbide.

14. A method comprising:
providing a precursor mixture of particles of a refractory metal or a refractory-metal compound capable of decomposing into refractory-metal nanoparticles, elemental silicon, and an organic compound;
heating the precursor mixture in a first inert atmosphere at an elevated pressure at a temperature that causes decomposition of the refractory-metal compound to form refractory-metal nanoparticles to form a metal nanoparticle composition; and
heating the metal nanoparticle composition in a second inert atmosphere or vacuum at a temperature that causes formation of a ceramic comprising nanoparticles of a refractory-metal silicide in a carbonaceous matrix;
wherein the organic compound has a char yield of at least 60% by weight when heated at the elevated pressure.

15. The method of claim 12 , wherein the inert atmosphere is argon or nitrogen.

16. The method of claim 14 , wherein the first inert atmosphere or the second inert atmosphere is argon or nitrogen.

17. The composition of claim 1 , wherein the metal component is the refractory-metal compound capable of decomposing into refractory-metal nanoparticles.

18. The method of claim 12 , wherein the precursor mixture comprises the refractory-metal compound capable of decomposing into refractory-metal nanoparticles.

19. The method of claim 14 , wherein the precursor mixture comprises the refractory-metal compound capable of decomposing into refractory-metal nanoparticles.

Assignees

• Us Gov Sec Navy

Inventors

• Keller Teddy M
• Laskoski Matthew

Classifications

• C04B35/78 Primary

  containing non-metallic materials · CPC title

• C04B2235/6567

  Treatment time · CPC title

• C04B2235/5454

  nanometer sized, i.e. below 100 nm · CPC title

• C04B2235/5436

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

• C04B2235/48

  Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins · CPC title