IP Library Granted Patent US 7,976,941
Granted Patent B2
US 7,976,941 · App. 11/327,770 · Granted Jul 12, 2011

Boron nitride particles of spherical geometry and process for making thereof

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Quick Facts
Patent No.
US 7,976,941
App. No.
11/327,770
Filed
Jan 6, 2006
Granted
Jul 12, 2011
Kind
B2
Art Unit
1616
USPC
428/325
Abstract

A low viscosity filler boron nitride agglomerate particles having a generally spherical shape bound together by an organic binder and to a process for producing a BN powder composition of spherically shaped boron nitride agglomerated particles having a treated surface layer which controls its viscosity.

Claims (34)

1. A boron nitride powder comprising agglomerated particles of spherical geometry, wherein said spherical agglomerates particles have an average particle size of about 1 to 150 microns in diameter and a tap density of at least 0.289 g/cc, wherein the particles have a surface layer comprising organic binder and/or decomposition product thereof, and wherein the spherical agglomerates particles are prepared by spray drying an aqueous slurry of non-spherical shaped boron nitride particles in a binder selected from the group consisting of acrylics, acetates, and mixtures thereof.

2. The boron nitride powder of claim 1 , wherein said decomposition product comprises at least one of a hydroxide and an oxide.

3. The boron nitride powder of claim 1 , wherein the binder comprises aluminum acetate.

4. A composition comprising the boron nitride powder of claim 1 and a melt-processable polymer.

5. The composition of claim 4 , wherein the composition at a loading level of boron nitride powder of about 30 to 50 wt. % has a viscosity of below 300 cp at 25° C.

6. The composition of claim 4 wherein the melt-processable polymer is a polyester, phenolic, silicone, acrylic, wax, or an epoxy molding compound.

7. A spherical boron nitride powder consisting essentially of spherical agglomerates of boron nitride platelets.

8. A polymer composition comprising: a polymer selected from the group consisting of melt-processable polymers, polyesters, phenolics, silicone polymers, acrylics, waxes, thermoplastic polymers, epoxy molding compounds, and blends thereof; between 30-50 wt. % of a powder comprising spherical boron nitride agglomerates formed by a process of spray drying an aqueous slurry comprising non-spherical shaped boron nitride particles, water, an organic binder and a base for maintaining the pH of the slurry basic and adjusting the concentration of said organic binder in the slurry such that the viscosity of the filler polymer composition is below 300 cp at 25° C.

9. The polymer composition of claim 8 , wherein the binder is selected from the group consisting of an acrylic or an acetate.

10. The polymer composition of claim 8 , wherein the binder is selected from the group consisting of nickel acetate, aluminum acetate and titanium acetate.

11. The polymer composition of claim 8 , wherein the concentration of acetate binder in the slurry is above about 2.5 wt. %.

12. A method for making spherical boron nitride powder comprising:

providing a hexagonal boron nitride slurry including a binder;

spray drying the slurry under conditions of available residence time, inlet and outlet temperatures, slurry pH, and slurry feed rate effective to produce spherical boron nitride powder comprising spherical agglomerates of boron nitride platelets; and

sintering the spherical boron nitride powder.

13. The method of claim 12 , further comprising surface treating the spherical boron nitride powder by at least one of heat treating and surface functionalization.

14. The method of claim 12 , wherein the sintering is carried out at a temperature of from about 1800° C. to about 2400° C.

15. The method according to claim 12 , wherein the hexagonal boron nitride slurry comprises from about 30 wt. % to about 50 wt. % hexagonal boron nitride powder.

16. The method according to claim 12 , wherein the spherical agglomerates of boron nitride platelets have an average agglomerate diameter of from about 1 to about 500 microns.

17. The method according to claim 12 , wherein the spherical agglomerates of boron nitride platelets have an average agglomerate diameter of from about 3 microns to about 150 microns.

18. The method according to claim 12 , further comprising classifying the spherical boron nitride powder under conditions effective to obtain a desired agglomerate size distribution.

19. The method according to claim 18 , wherein the classifying is selected from the group consisting of screening, milling, air classifying, and elutriation.

20. The method of claim 12 wherein the binder is a material which bonds the hexagonal boron nitride particles during spray drying and/or modifies the slurry viscosity.

21. The method of claim 12 wherein the binder is organic.

22. The method of claim 12 wherein the slurry comprises water.

23. The method of claim 12 wherein the slurry comprises a non-aqueous medium.

24. The method of claim 12 wherein pH of the slurry is above 7.0.

25. The method of claim 12 wherein the pH of the slurry is above 7.3.

26. The method of claim 12 wherein the slurry additionally comprises one or more of a polycarboxylic acid, an organometallic compound, a polyoxyethylene based non-ionic surfactant, a ammonium persulfate, potassium persulfate, sodium persulfate, or a peroxide.

27. The method of claim 12 wherein the binder comprises at least one of oxides, nitrates, acetates, sulfates of boron, aluminum, titanium, zirconium, silicon, nickel, rare earth and alkaline earth metallic elements, organic binders, decomposition products of organic binders, decomposition products of oxides, nitrates, acetates, and sulfates of boron, aluminum, rare earth and alkaline earth metallic elements, and mixtures thereof.

28. The method of claim 12 wherein the binder is selected from the group consisting of methyl acrylate, ethyl acrylate, butyl acrylate, methyl methacrylate, ethyl methacrylate, butyl methacrylate, isobutyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, acrylamide, methacrylamide; N-tertiarybutylacrylamide, N-methacrylamide and N,N-dimethacrylamide, dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, acrylonitrile and methacrylonitrile.

29. A process for forming a boron nitride powder comprising agglomerated particles of spherical geometry having an average particle size of about 1 to 150 microns in diameter, said process comprising the steps of: mixing an aqueous slurry including irregular shaped boron nitride particles, water, an organic binder and a base for maintaining the pH of the slurry basic; spray drying the aqueous slurry into a powder composition of agglomerated boron nitride particles.

30. The process of claim 29 , wherein the organic binder is selected from the group consisting of acrylics, acetates, and mixtures thereof.

31. The process of claim 30 , wherein said organic binder is selected from the group consisting of nickel acetate, aluminum acetate and titanium acetate.

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