Spherical boron nitride particles and method for preparing them

• US 20020172635A1
• Filed: 05/17/2001
• Published: 11/21/2002
• Est. Priority Date: 05/17/2001
• Status: Active Grant

• 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: Gleiman, Seth S., Phillips, Jonathan, Chen, Chun-Ku
• Granted Patent: US 6,652,822 B2
• Time in Patent Office: Days
• 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, 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; 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.

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.

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.

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.

36. A method for melting boron nitride, 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 to the plasma, whereby boron nitride melts.

52. Crystalline or partially crystalline boron nitride particles made by the process 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 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.

53. Boron nitride particles made by the method of claim 52, where the plasma is generated from plasma gas at a gas pressure of about 0.01-100 atmospheres.

54. Boron nitride particles made by the method of claim 53, wherein the plasma is generated from plasma gas at a pressure of about 1 atmosphere.

55. Boron nitride particles made by the method of claim 52, wherein the plasma is generated by a DC discharge.

56. Boron nitride particles made by the method of claim 52, wherein the plasma is generated by supplying electromagnetic energy to the plasma gas.

57. Boron nitride particles made by the method of claim 52, wherein the plasma is generated using radiofrequency energy.

58. Boron nitride particles made by the method of claim 52, wherein the plasma is generated using microwave energy.

59. Boron nitride particles made by the method of claim 58, wherein the plasma is generated using about 100-30,000 watts of microwave power.

60. Boron nitride particles made by the method of claim 59, wherein the plasma is generated using about 300-1200 watts of power.

61. Boron nitride particles made by the method of claim 52, 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.

62. Boron nitride particles made by the method of claim 52, 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.

63. Boron nitride particles made by the method of claim 52, wherein the precursor boron nitride particles are in the hexagonal solid phase.

64. Boron nitride particles made by the method of claim 52, wherein the precursor boron nitride particles are platelet-shaped.

65. The method of claim 52, wherein the precursor boron nitride particles comprise spherical particles.

66. The method of claim 52, wherein the precursor boron nitride particles comprise agglomerates.

67. Boron nitride particles made by the method of claim 52, wherein the solid particles recovered in step (d) comprise spherical shaped particles with a diameter of about 1-1000 microns.

68. Boron nitride particles made by the method of claim 52, wherein the solid particles recovered in step (d) comprise polyhedral shaped particles.

70. Boron nitride particles made by the method of claim 69, wherein the plasma is generated from plasma gas at a gas pressure of about 0.01-100 atmospheres.

71. Boron nitride particles made by the method of claim 69, wherein the plasma is generated from plasma gas at a pressure of about 1 atmosphere.

72. The method of claim 69, wherein the plasma is generated by a DC discharge.

73. The method of claim 69, wherein the plasma is generated by supplying electromagnetic energy to the plasma gas.

74. The method of claim 69, wherein the plasma is generated using radiofrequency energy.

75. The method of claim 69, wherein the plasma is generated using microwave energy.

76. The method of claim 75, wherein the plasma is generated using about 300-30,000 watts of microwave power.

77. The method of claim 76, wherein the plasma is generated using about 300-1200 watts of power.

78. The method of claim 69, 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.

79. The method of claim 69, 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.

80. The method of claim 69, wherein the precursor boron nitride particles are in the hexagonal solid phase.

81. The method of claim 69, wherein the precursor boron nitride particles are platelet-shaped.

82. The method of claim 69, wherein the precursor boron nitride particles comprise spherical particles.

83. The method of claim 69, wherein the precursor boron nitride particles comprise agglomerates.

84. The method of claim 69, wherein the solid particles recovered in step (d) comprise spherical shaped particles with a diameter of about 10-100 microns.

85. The method of claim 69, wherein the solid particles recovered in step (d) comprise polyhedral shaped particles.

86. The method of claim 69, 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.

69. 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.

87. Crystalline or partially crystalline spherical particles of boron nitride having a diameter of about 1-1000 microns.