Phase Powders and Process for Manufacturing Said Powders

• US 20100247910A1
• Filed: 05/29/2007
• Published: 09/30/2010
• Est. Priority Date: 05/30/2006
• Status: Active Grant

• Current Assignee: Commissariat a L'Energie Atomique (AES Corporation)
• Original Assignee: Commissariat a L'Energie Atomique (AES Corporation)
• Inventors: Canel, Jérôme, Tenegal, François
• Granted Patent: US 9,023,246 B2
• Time in Patent Office: Days
• US Class Current: 428/368
• 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

1-30. -30. (canceled)

31. 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, Ti, 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 of less than 500 nm.

32. The powder of claim 31, wherein the powder has a mean particle size of less than 100 nm.

33. The powder of claim 31, wherein the powder has a mean particle size ranging from 10 to 200 nm.

34. The powder of claim 31, wherein the powder has a mean particle size ranging from 10 to 50 nm.

35. The powder of claim 31, wherein the elements M, A, and X are in proportions of 3, 1, and 2, respectively.

36. The powder of claim 35, wherein the powder corresponds to a phase selected from the group consisting of Ti₃SiC₂, Ti₃AlC₂, and Ti₃GeC₂.

37. The powder of claim 36, wherein the powder corresponds to a Ti₃SiC₂ phase.

38. The powder of claim 31, wherein the elements M, A, and X are in proportions of 2, 1, and 1, respectively.

39. The powder of claim 38, wherein the powder corresponds to a phase selected from the group consisting of:

Ti₂AlC, Ti₂AlN, Ti₂InN, Ti₂GeC, Ti₂SC, Ti₂GaN, Ti₂InC, Ti₂TlC, Ti₂SnC, Ti₂GaC, Ti₂CdC, Ti₂PbC, Zr₂InN, Zr₂SnC, Zr₂SC, Zr₂InC, Zr₂TlC, Zr₂PbC, Zr₂TlN, Hf₂PbC, Hf₂InN, Hf₂SnN, Hf₂SnC, Hf₂SC, Hf₂TlC, Hf₂InC, Cr₂GaC, Cr₂AlC, Cr₂GaN, V₂AsC, V₂AlC, V₂PC, V₂GaN, V₂GaC, V₂GeC, Nb₂AlC, Nb₂GaC, Nb₂AsC, Nb₂SnC, Nb₂PC, Nb₂InC, Nb₂SC, Ta₂AlC, Ta₂GaC, Mo₂GaC, and Nb₂SC.

40. The powder of claim 31, wherein the elements M, A, and X are in proportions of 4, 1, and 3, respectively.

41. The powder of claim 40, wherein the powder corresponds to a phase selected from the group consisting of Ti₄AlN₃ and Ta₄AlC₃.

42. The powder of claim 31, wherein M is partially substituted with one or more transition metals or another metal and/or A is partially substituted with another element belonging to the list of alternatives for A in claim 31 and/or X is partially substituted with another element belonging to the list of alternatives for X in claim 31.

43. The powder of claim 42, wherein the powder corresponds to a phase selected from the group consisting of:

(Ti,Zr)₃SiC₂, (Ti,Hf)₃SiC₂, (Ti,Hf)₃(Si,Ge)C₂, (Ti,Zr)₃(Si,Ge)(C,N)₂, (Ti,V)₃SiC₂, (Ti,V)₃Si(C,N)₂, Ti₃(Si,Al)C₂, (Ti,V)₃(Si,Ge)(C,N)₂, (Ti,V,Hf)₃(Si,Ge)(C,N)₂, (Ti,V,Hf)₃(Si,Ge,Al)(C,N)₂, (Nb,Ti)₂AlC, and TiAlN_0.5C_0.5.

44. The powder of claim 31, further including a sintering agent.

45. A process for manufacturing the powder of claim 31, 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.

46. The manufacturing process of claim 45, 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.

47. The manufacturing process of claim 45, wherein the precursor of M is selected from the group consisting of M halides, M oxyhalides, M carbonyls, M oxyalkyls, and M boranes.

48. The manufacturing process of claim 45, wherein the precursor of A is selected from the group consisting of A hydrides, A hydrohalides, and alkylated M complexes.

49. The manufacturing process of claim 45, wherein the precursor of X is a carbon precursor selected from the group consisting of acetylene and ethylene.

50. The manufacturing process of claim 45, wherein the precursor of X is a boron precursor selected from the group consisting of boron halides and boranes.

51. The manufacturing process of claim 45, wherein the precursor of X is NH₃.

52. The manufacturing process of claim 45, 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.

53. The manufacturing process of claim 45, wherein heating said mixture is carried out at a temperature sufficient for creating a plasma or a temperature ranging from 1000 to 2000°

C.

54. A process for manufacturing a nanostructured single-phase material, comprising:

compressing the powder of claim 31 to obtain an intermediate material; and

sintering the intermediate material obtained by the compressing step thereby creating a nanostructured single-phase material.

55. A nanostructured single-phase material obtained by the process of claim 54.

56. A process for manufacturing a composite having particulate reinforcing elements and/or short fibers for reinforcing elements, said process comprising:

mixing powders of claim 31 with a reinforcing element; and

sintering.

57. The manufacturing process of claim 56, wherein the reinforcing element is selected from particles or short fibers consisting of carbon, silicon carbide, and other ceramics.

58. A composite obtained by the process of claim 56.

59. A process for manufacturing a composite having long fibers as reinforcing elements, said process comprising:

suspending powders of claim 31 to form a suspension;

infiltrating a preform consisting of said long fibers with said suspension; and

sintering to consolidate the composite.

60. A composite obtained by the process of claim 59.