IP Library Granted Patent US 11,078,080
Granted Patent B2
US 11,078,080 · App. 16/647,756 · Granted Aug 3, 2021

Hexagonal boron nitride powder and method for producing the same, and composition and heat dissipation material using the same

Inventors: Boanerges Thendie (Shiojiri, JP); Masaru Fukasawa (Shiojiri, JP)
Assignee: SHOWA DENKO K.K.
C01B21/0648C01P2002/74C01P2004/30C01P2004/51C01P2004/61C01P2006/12C01P2006/16C01P2006/32
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Quick Facts
Patent No.
US 11,078,080
App. No.
16/647,756
Granted
Aug 3, 2021
Kind
B2
Abstract

A hexagonal BN powder including aggregates of primary particles of hexagonal BN containing boron and oxygen as impurity elements at a content of 1.00 to 30.00% and 0 to 1.00% by mass, respectively, which has a peak A in a predetermined particle diameter range and a 50% volume cumulative particle diameter D 50 (d1) of 30.0 to 200.0 μl in a particle size distribution curve, and in which a ratio of a height (a1) of the peak A before treatment to a height (a2) of the peak A after treatment is 0.80 to 1.00 and a ratio of D 50 (d1) before treatment to D 50 (d2) after treatment is 0.80 to 1.00 when the hexagonal BN powder is ultrasonically treated under a predetermined condition for 1 minute. Also disclosed is a method for producing the hexagonal BN powder, a composition and a heat dissipation material.

Claims (23)

1. A hexagonal boron nitride powder comprising an aggregate of primary particles of hexagonal boron nitride,

comprising boron as an impurity element at a content of 1.00 to 30.00% by mass and oxygen as an impurity element at a content of 0 to 1.00% by mass, and

having a peak in a particle diameter range of 10.0 μm or more and less than 100.0 μm and a 50% volume cumulative particle diameter D 50 (d1) of 30.0 to 200.0 μm in a particle size distribution curve representing volume-based frequency distribution,

wherein the hexagonal nitride powder has a structure such that, when the hexagonal boron nitride powder is ultrasonically treated under the following condition 1 for 1 minute, a ratio of a height (a1) of the peak before the ultrasonic treatment to a height (a2) of the peak after treatment, a2/a1, being 0.80 to 1.00 and a ratio of a 50% volume cumulative particle diameter D 50 (d1) before ultrasonic treatment to a 50% volume cumulative particle diameter D 50 (d2) after the ultrasonic treatment, d2/d1, being 0.80 to 1.00,

[condition 1] a powder sample dispersion obtained by mixing 0.06 g of the hexagonal boron nitride powder, 0.005 g of a detergent (“Mama Lemon (registered trademark)”, manufactured by Lion Corporation) and 50 g of water (20° C.) is placed in a 50 mL glass beaker having a barrel inner diameter of 40 mm and a height of 60 mm, and an end of a tip of a vibrator of an ultrasonic generator is set at a height of 1 cm from a bottom surface of a central portion of the beaker, and ultrasonic treatment is performed at an output of 150 W and an oscillation frequency of 19.5 kHz, and

wherein the boron as an impurity element is a boron atom not bound to a nitrogen atom and which does not form a hexagonal boron nitride molecule.

2. The hexagonal boron nitride powder according to claim 1 , having a BET specific surface area of 0.1 m 2 /g or more and less than 5.0 m 2 /g, and the primary particles each having a smooth surface.

3. The hexagonal boron nitride powder according to claim 1 , having a crystallite diameter derived from a (002) plane of hexagonal boron nitride, as determined by powder X-ray diffraction measurement, of 250 Å or more and less than 375 Å.

4. The hexagonal boron nitride powder according to claim 1 , having a BET specific surface area of 0.1 m 2 /g or more and less than 5.0 m 2 /g.

5. The hexagonal boron nitride powder according to claim 1 , wherein the content of the boron as the impurity element is 5.00 to 28.00% by mass.

6. The hexagonal boron nitride powder according to claim 1 , wherein the content of the boron as the impurity element is 10.00 to 25.00% by mass.

7. A composition comprising a base material comprising one or two or more selected from the group consisting of a resin and a rubber, and the hexagonal boron nitride powder according to claim 1 .

8. A heat dissipation material comprising the composition according to claim 7 .

9. The heat dissipation material according to claim 8 , being a heat dissipation sheet.

10. The heat dissipation material according to claim 9 , wherein a ratio of a diffraction peak intensity (I(002)) of a (002) plane to a diffraction peak intensity (I(100)) of a (100) plane, I(002)/I(100), of primary particles of hexagonal boron nitride, as determined in a direction perpendicular to a thickness direction of the heat dissipation sheet by X-ray diffraction measurement, is 7.0 to 15.

11. A method for producing the hexagonal boron nitride powder according to claim 1 , comprising:

step 1 of preparing a mixed powder comprising a boron powder and one or two or more boron compounds selected from the group consisting of a boron oxoacid and boron oxide,

step 2 of calcining the mixed powder under a noble gas atmosphere at 1200° C. or more and less than 1800° C. to obtain a calcined powder,

step 3 of granulating the calcined powder to obtain a granulated powder having a particle diameter of 10 to 200 μm,

step 4 of melting the granulated powder under a noble gas atmosphere at 1800 to 2300° C. to obtain a molten powder, and

step 5 of firing the molten powder under a nitrogen gas atmosphere at 2000 to 2300° C. to obtain a hexagonal boron nitride powder.

12. The method for producing the hexagonal boron nitride powder according to claim 11 , wherein the calcined powder obtained in the step 2 comprises boron suboxide.

13. The method for producing the hexagonal boron nitride powder according to claim 11 , wherein in the step 3, at least any of boron oxide and hexagonal boron nitride is added to the calcined powder for granulation.

Assignments (3)
CHANGE OF ADDRESS Recorded Feb 14, 2024
From: RESONAC CORPORATION
To: RESONAC CORPORATION
Reel/Frame 066599/0037 →
CHANGE OF NAME Recorded Jun 23, 2023
From: SHOWA DENKO K.K.
To: RESONAC CORPORATION
Reel/Frame 064082/0513 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 16, 2020
From: THENDIE, BOANERGES; FUKASAWA, MASARU
To: SHOWA DENKO K.K.
Reel/Frame 052127/0823 →