Phase powders and process for manufacturing said powders

• US 9,023,246 B2
• Filed: 05/29/2007
• Issued: 05/05/2015
• Est. Priority Date: 05/30/2006
• Status: Expired due to Fees

• Current Assignee: Commissariat a L'Energie Atomique (AES Corporation)
• Original Assignee: Commissariat a L'Energie Atomique (AES Corporation)
• Inventors: Tenegal, Franois, Canel, Jrme
• Primary Examiner(s): Koslow, Carol M
• Assistant Examiner(s): EDMONDSON, LYNNE RENEE
• Application Number:
  US12/301,803
• Publication Number:
  US 20100247910A1
• Time in Patent Office: 2,898 Days
• Field of Search: 252/500, 423/279, 423/351, 423/414, 423/423, 117/2, 501/87, 501/92, 501/93, 501/96.4
• US Class Current: 252/500
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 21/0602 with two or more other elements chosen from metals, silicon or boron
• CPC Class Codes: C01B 32/90 Carbides
• CPC Class Codes: C01P 2004/62 Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C04B 2235/5224 Alumina or aluminates
• CPC Class Codes: C04B 2235/5244 Silicon carbide
• CPC Class Codes: C04B 2235/5248 Carbon, e.g. graphite
• CPC Class Codes: C04B 2235/5445 submicron sized, i.e. from 0,1 to 1 micron
• CPC Class Codes: C04B 2235/5454 nanometer sized, i.e. below 100 nm
• CPC Class Codes: C04B 2235/81 Materials characterised by the absence of phases other than the main phase, i.e. single phase materials
• CPC Class Codes: C04B 35/5607 based on refractory metal carbides
• CPC Class Codes: C04B 35/5611 based on titanium carbides
• CPC Class Codes: C04B 35/5615 based on titanium silicon carbides
• CPC Class Codes: C04B 35/5618 based on titanium aluminium carbides
• CPC Class Codes: C04B 35/5622 based on zirconium or hafnium carbides
• CPC Class Codes: C04B 35/58007 based on refractory metal nitrides
• CPC Class Codes: C04B 35/58014 based on titanium nitrides, e.g. TiAlON
• CPC Class Codes: C04B 35/58021 based on titanium carbonitrides
• CPC Class Codes: C04B 35/58028 based on zirconium or hafnium nitrides
• CPC Class Codes: C04B 35/58035 : based on zirconium or hafnium carbonitrides
• CPC Class Codes: C04B 35/6262 : of calcined, sintered clinker or ceramics
• CPC Class Codes: C04B 35/645 : Pressure sintering
• CPC Class Codes: C04B 35/80 : Fibres, filaments, whiskers, platelets, or the like
• CPC Class Codes: Y10T 428/292 : In coating or impregnation
• CPC Class Codes: Y10T 428/2982 : Particulate matter [e.g., sphere, flake, etc.]

Abstract

The invention relates to powder comprising at least one element M, at least one element A and at least one element X, in the respective proportions (n+1±ε₁), 1±ε₂ and n±ε₃, in which:

• • A is chosen from Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, P, As and S;
  • M is a transition metal;
  • X is chosen from B, C and N;
  • n is an integer equal to 1, 2 or 3; and
  • ε₁, ε₂ and ε₃ independently represent a number ranging from 0 to 0.2,
    said powder having a mean particle size of less than 500 nm.

Claims

1. A process for manufacturing a powder comprising an element M, an element A, and an element X, in the respective proportions (n+1±

ε

₁), 1±

ε

₂ and n±

ε

₃, wherein;

A is selected from the group consisting of Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, P, As, and S;

M is a transition metal;

X is selected from the group consisting of B, C, and N;

n is an integer equal to 1, 2, or 3; and

ε

₁, ε

₂, and ε

₃ independently represent a number ranging from 0 to 0.2,

said powder having a mean particle size ranging from 10 to 200 nm,

comprising;

a) mixing together, with no heating and in the absence of oxygen, a precursor of M, a precursor of A and a precursor of X to obtain a mixture, said precursors being in the form of a gas, a solid in suspension in a gas, and/or a liquid in suspension in a gas; and

b) heating said mixture obtained in step a) to a temperature effective for forming the powder.

2. The manufacturing process of claim 1, wherein the mixing together is carried out from a stream comprising a precursor of M, a stream comprising a precursor of A, and a stream comprising a precursor of X.

3. The manufacturing process of claim 1, wherein the precursor of M is selected from the group consisting of M halides, M oxyhalides, M carbonyls, M oxyalkyls, and M boranes.

4. The manufacturing process of claim 1, wherein the precursor of A is selected from the group consisting of A hydrides, A hydrohalides, and alkylated M complexes.

5. The manufacturing process of claim 1, wherein the precursor of X is a carbon precursor selected from the group consisting of acetylene and ethylene.

6. The manufacturing process of claim 1, wherein the precursor of X is a boron precursor selected from the group consisting of boron halides and boranes.

7. The manufacturing process of claim 1, wherein the precursor of X is NH₃.

8. The manufacturing process of claim 1, including, before step a), when the precursor of M is an M halide, preparing said precursor of M, consisting in heating a metal powder of M in the presence of haloacids at a temperature effective for obtaining the corresponding M halide.

9. The manufacturing process of claim 1, wherein heating said mixture is carried out at a temperature sufficient for creating a plasma or a temperature ranging from 1000 to 2000°

C.