Spherical boron nitride particles and method for preparing them

• US 6,652,822 B2
• Filed: 05/17/2001
• Issued: 11/25/2003
• Est. Priority Date: 05/17/2001
• Status: Expired due to Term

• Current Assignee: UNM Rainforest Innovations (f/k/a STC.UNM) (The University of New Mexico), TRIAD National Security, LLC
• Original Assignee: Regents of the University of California (University of California)
• Inventors: Chen, Chun-Ku, Gleiman, Seth S., Phillips, Jonathan
• Primary Examiner(s): Langel, Wayne A.
• Application Number:
  US09/860,016
• Publication Number:
  US 20020172635A1
• Time in Patent Office: 922 Days
• Field of Search: 423/290, 232/93.R, 233/13.R
• US Class Current: 423/290
• CPC Class Codes: C01B 21/064 with boron
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/30 extending in three dimensions
• CPC Class Codes: C01P 2004/32 Spheres
• CPC Class Codes: C01P 2004/42 (bi)pyramid-like
• CPC Class Codes: C01P 2004/52 highly monodisperse size distribution
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer

Abstract

Spherical and polyhedral particles of boron nitride and method of preparing them. Spherical and polyhedral particles of boron nitride are produced from precursor particles of hexagonal phase boron nitride suspended in an aerosol gas. The aerosol is directed to a microwave plasma torch. The torch generates plasma at atmospheric pressure that includes nitrogen atoms. The presence of nitrogen atoms is critical in allowing boron nitride to melt at atmospheric pressure while avoiding or at least minimizing decomposition. The plasma includes a plasma hot zone, which is a portion of the plasma that has a temperature sufficiently high to melt hexagonal phase boron nitride. In the hot zone, the precursor particles melt to form molten particles that acquire spherical and polyhedral shapes. These molten particles exit the hot zone, cool, and solidify to form solid particles of boron nitride with spherical and polyhedral shapes. The molten particles can also collide and join to form larger molten particles that lead to larger spherical and polyhedral particles.

Claims

1. A method for producing crystalline or partially crystalline particles of boron nitride (BN), comprising the steps of:

(a) generating an aerosol comprising precursor particles of boron nitride (BN) suspended in an aerosol gas;

(b) generating a plasma from a plasma gas, the plasma comprising nitrogen atoms, the plasma including a plasma hot zone having a temperature sufficiently high to melt boron nitride;

(c) directing the aerosol into the plasma hot zone and allowing the precursor particles of boron nitride to melt; and

(d) allowing the molten particles to exit the hot zone, whereby they cool and solidify to form crystalline or partially crystalline product particles of boron nitride.

2. The method of claim 1, where the plasma is generated from plasma gas at a gas pressure of about 0.01-100 atmospheres.

3. The method of claim 1, wherein the plasma is generated from plasma gas at a pressure of about 1 atmosphere.

4. The method of claim 1, wherein the plasma is generated by a DC discharge.

5. The method of claim 1, wherein the plasma is generated by supplying electromagnetic energy to the plasma gas.

6. The method of claim 5, wherein the plasma is generated using radiofrequency energy.

7. The method of claim 5, wherein the plasma is generated using microwave energy.

8. The method of claim 7, wherein the plasma is generated using about 300-30,000 watts of microwave power.

9. The method of claim 8, wherein the plasma is generated using about 300-1200 watts of power.

10. The method of claim 1, wherein the plasma comprising nitrogen atoms is generated by first producing argon plasma from argon plasma gas and then introducing nitrogen plasma gas into the argon plasma.

11. The method of claim 1, wherein the plasma gas comprising nitrogen atoms is produced from a plasma gas stream mixture comprising about 95-0% argon gas and about 5-100% nitrogen gas.

12. The method of claim 1, wherein the precursor boron nitride particles comprise hexagonal solid phase boron nitride.

13. The method of claim 1, wherein the precursor boron nitride particles comprise platelet-shaped particles.

14. The method of claim 1, wherein the precursor boron nitride particles comprise spherical particles.

15. The method of claim 1, wherein the precursor boron nitride particles comprise agglomerates.

16. The method of claim 1, wherein the solid particles recovered in step (d) comprise spherical shaped particles with a diameter of about 1-1000 microns.

17. The method of claim 1, wherein the solid particles recovered in step (d) comprise polyhedral shaped particles.

18. A method for generating larger particles of boron nitride from smaller particles of boron nitride, comprising the steps of:

(a) generating an aerosol comprising precursor particles of boron nitride suspended in an aerosol gas;

(b) generating a plasma from a plasma gas, the plasma comprising nitrogen atoms, the plasma including a plasma hot zone having a temperature sufficiently high to melt boron nitride;

(c) directing the aerosol into the plasma hot zone and allowing the precursor particles of boron nitride to melt, collide, and join to form larger particles; and

(d) allowing the molten particles to exit the hot zone, whereby they cool and solidify to form solid particles of boron nitride that are larger than the precursor particles.

19. The method of claim 18, where the plasma is generated from plasma gas at a gas pressure of about 0.01-100 atmospheres.

20. The method of claim 18, wherein the plasma is generated from plasma gas at a pressure of about 1 atmosphere.

21. The method of claim 18, wherein the plasma is generated by a DC discharge.

22. The method of claim 18, wherein the plasma is generated by supplying electromagnetic energy to the plasma gas.

23. The method of claim 18, wherein the plasma is generated using radiofrequency energy.

24. The method of claim 23, wherein the plasma is generated using microwave energy.

25. The method of claim 24, wherein the plasma is generated using about 300-30,000 watts of microwave power.

26. The method of claim 25, wherein the plasma is generated using about 300-1200 watts of power.

27. The method of claim 18, wherein the plasma comprising nitrogen atoms is generated by first producing an argon plasma from argon plasma gas and then introducing nitrogen plasma gas into the argon plasma.

28. The method of claim 18, wherein the plasma gas comprising nitrogen atoms is produced from a plasma gas stream mixture comprising about 95-0% argon gas and about 5-100% nitrogen gas.

29. The method of claim 18, wherein the precursor boron nitride particles are in the hexagonal solid phase.

30. The method of claim 18, wherein the precursor boron nitride particles are platelet-shaped.

31. The method of claim 18, wherein the precursor boron nitride particles are spherical shaped.

32. The method of claim 18, wherein the precursor boron nitride particles comprise agglomerates.

33. The method of claim 18, wherein the solid particles recovered in step (d) comprise spherical shaped particles with a diameter of about 1-1000 microns.

34. The method of claim 18, wherein the solid particles recovered in step (d) comprise polyhedral shaped particles.

35. The method of claim 18, wherein the solid particles recovered in step (d) comprise agglomerates arising from the joining of partially melted BN particles.

36. A method for melting boron nitride (BN), comprising the steps of:

(a) generating a plasma comprising nitrogen atoms, the plasma including a plasma hot zone having a temperature sufficiently high to melt hexagonal phase boron nitride; and

(b) exposing precursor particles of boron nitride (BN) to the plasma, whereby boron nitride melts.

37. The method of claim 36, where the plasma is generated from plasma gas at a gas pressure of about 0.01-100 atmospheres.

38. The method of claim 36, wherein the plasma is generated from plasma gas at a pressure of about 1 atmosphere.

39. The method of claim 36, wherein the plasma is generated by a DC discharge.

40. The method of claim 36, wherein the plasma is generated by supplying electromagnetic energy to the plasma gas.

41. The method of claim 36, wherein the plasma is generated using radiofrequency energy.

42. The method of claim 36, wherein the plasma is generated using microwave energy.

43. The method of claim 36, wherein the plasma is generated using about 100-30,000 watts of microwave power.

44. The method of claim 36, wherein the plasma is generated using about 300-1200 watts of power.

45. The method of claim 36, wherein the plasma comprising nitrogen atoms is generated by first producing an argon plasma from argon plasma gas and then introducing nitrogen plasma gas into the argon plasma.

46. The method of claim 36, wherein the plasma gas comprising nitrogen atoms is produced from a plasma gas stream mixture comprising about 95-0% argon gas and about 5-100% nitrogen gas.

47. The method of claim 36, wherein the precursor boron nitride comprises particles in the hexagonal solid phase.

48. The method of claim 36, wherein the precursor boron nitride particles are platelet-shaped.

49. The method of claim 36, wherein the precursor boron nitride particles comprise spherical particles.

50. The method of claim 36, wherein the precursor boron nitride particles comprise agglomerates.

51. Crystalline or partially crystalline boron nitride (BN) particles made by the process comprising the steps of:

(a) generating an aerosol comprising precursor particles of boron nitride (BN) suspended in an aerosol gas;

(b) generating a plasma from a plasma gas, the plasma comprising nitrogen atoms, the plasma including a plasma hot zone having a temperature sufficiently high to melt boron nitride;

(c) directing the directing the aerosol into the plasma hot zone and allowing the precursor particles of boron nitride to melt; and

(d) allowing the molten particles to exit the hot zone, whereby they cool and solidify to form crystalline or partially crystalline solid particles of boron nitride.

52. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, where the plasma is generated from plasma gas at a gas pressure of about 0.01-100 atmospheres.

53. The crystalline or partially crystalline boron nitride (BN) particles of claim 52, wherein the plasma is generated from plasma gas at a pressure of about 1 atmosphere.

54. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the plasma is generated by a DC discharge.

55. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the plasma is generated by supplying electromagnetic energy to the plasma gas.

56. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the plasma is generated using radiofrequency energy.

57. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the plasma is generated using microwave energy.

58. The crystalline or partially crystalline boron nitride (BN) particles of claim 57, wherein the plasma is generated using about 100-30,000 watts of microwave power.

59. The crystalline or partially crystalline boron nitride (BN) particles of claim 58, wherein the plasma is generated using about 300-1200 watts of power.

60. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the plasma comprising nitrogen atoms is generated by first producing an argon plasma from argon plasma gas and then introducing nitrogen plasma gas into the argon plasma.

61. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the plasma gas comprising nitrogen atoms is produced from a plasma gas stream mixture comprising about 95-0% argon gas and about 5-100% nitrogen gas.

62. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the precursor boron nitride particles are in the hexagonal solid phase.

63. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the precursor boron nitride particles are platelet-shaped.

64. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the precursor boron nitride particles comprise spherical particles.

65. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the precursor boron nitride particles comprise agglomerates.

66. The crystalline or partially crystalline boron nitride (BN) particles of claim 51, wherein the solid particles recovered in step (d) comprise spherical shaped particles with a diameter of about 1-1000 microns.

67. The crystalline boron nitride (BN) particles of claim 51, wherein the solid particles recovered in step (d) comprise polyhedral shaped particles.

68. Crystalline or partially crystalline boron nitride particles made by the method comprising the steps of:

(a) generating an aerosol comprising precursor particles of boron nitride suspended in an aerosol gas;

(b) generating a plasma from a plasma gas, the plasma comprising nitrogen atoms, the plasma including a plasma hot zone having a temperature sufficiently high to melt boron nitride but not high enough to decompose the boron nitride;

(c) directing the aerosol into the plasma hot zone and allowing the precursor particles of boron nitride to melt, collide, and join to form larger particles; and

(d) allowing the molten particles to exit the hot zone, whereby they cool and solidify to form crystalline or partially crystalline solid particles of boron nitride that are larger than the precursor particles.

69. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma is generated from plasma gas at a gas pressure of about 0.01-100 atmospheres.

70. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma is generated from plasma gas at a pressure of about 1 atmosphere.

71. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma is generated by a DC discharge.

72. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma is generated by supplying electromagnetic energy to the plasma gas.

73. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma is generated using radiofrequency energy.

74. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma is generated using microwave energy.

75. The crystalline or partially crystalline boron nitride particles of claim 74, wherein the plasma is generated using about 300-30,000 watts of microwave power.

76. The crystalline or partially crystalline boron nitride particles of claim 75, wherein the plasma is generated using about 300-1200 watts of power.

77. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma comprising nitrogen atoms is generated by first producing an argon plasma from argon plasma gas and then introducing nitrogen plasma gas into the argon plasma.

78. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the plasma gas comprising nitrogen atoms is produced from a plasma gas stream mixture comprising about 95-0% argon gas and about 5-100% nitrogen gas.

79. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the precursor boron nitride particles are in the hexagonal solid phase.

80. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the precursor boron nitride particles are platelet-shaped.

81. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the precursor boron nitride particles comprise spherical particles.

82. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the precursor boron nitride particles comprise agglomerates.

83. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the solid particles recovered in step (d) comprise spherical shaped particles with a diameter of about 10-100 microns.

84. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the solid particles recovered in step (d) comprise polyhedral shaped particles.

85. The crystalline or partially crystalline boron nitride particles of claim 68, wherein the solid particles recovered in step (d) comprises not-fully-dense agglomerates that arise from the incomplete melting of at least two partially melted, joined, precursor BN particles.