Surface-treated aggregated boron nitride powder, aggregated boron nitride powder, and thermally conductive resin composition

Patent metadata

Field	Value
Publication number	US-11732173-B2
Application number	US-202217588757-A
Country	US
Kind code	B2
Filing date	Jan 31, 2022
Priority date	Oct 7, 2016
Publication date	Aug 22, 2023
Grant date	Aug 22, 2023

Abstract

A surface-treated aggregated boron nitride powder is prepared by using the boron nitride powder as the raw material, adding an oxidizer to the boron nitride aggregated grains, wet-pulverizing or wet-crushing the grains for surface modification treatment of the particles and allowing reaction of the particles with a metal coupling agent. The surface-treated boron nitride aggregated grains are formed by aggregation of hexagonal h-BN primary particles; (B) have any one or more of Si, Ti, Zr, Ce, Al, Mg, Ge, Ga, and V in an amount of 0.1 atm % or more and 3.0 atm % or less in its composition on the surface of 10 nm; (C) have a crushing strength of 5 MPa or more; and (D) have an average particle diameter of 20 μm or more and 100 μm or less.

First claim

The invention claimed is:

1. A surface-treated aggregated boron nitride powder comprising surface-treated boron nitride aggregated grains, wherein the surface-treated boron nitride aggregated grains are prepared by
adding an oxidizer to boron nitride aggregated grains,
wet-pulverizing or wet-crushing the boron nitride aggregated grains for surface modification treatment and allowing reaction of the boron nitride aggregated grains with a metal coupling agent to form surface-treated boron nitride aggregated grains,
wherein the boron nitride aggregated grains are formed by aggregation of scaly hexagonal boron nitride primary particles, and have the following characteristics (a) to (c):
(a) the scaly hexagonal boron nitride primary particles have an average long side length of 1.5 μm or more and 3.5 μm or less and a standard deviation of 1.2 μm or less;
(b) the boron nitride aggregated grains have a grain strength of 8.0 MPa or more at a cumulative breakdown rate of 63.2% and a grain strength of 4.5 MPa or more at a cumulative breakdown rate of 20.0%; and
(c) boron nitride powder of the surface-treated aggregated boron nitride powder has an average particle diameter of 20 μm or more and 100 μm or less,
and wherein the surface-treated aggregated boron nitride aggregated grains have the following characteristics (A) to (C):
(A) the surface-treated boron nitride aggregated grains are formed by aggregation of hexagonal h-BN primary particles;
(B) the surface-treated boron nitride aggregated grains have any one or more of Si, Ti, Zr, Ce, Al, Mg, Ge, Ga, and V in an amount of 0.1 atm % or more and 3.0 atm % or less in its composition on a surface of 10 nm; and
(C) the surface-treated boron nitride aggregated grains have a crushing strength of 5 MPa or more.

2. The surface-treated aggregated boron nitride powder according to claim 1 , wherein the oxidizer and a water-soluble solvent are added during the surface modification treatment.

3. The surface-treated aggregated boron nitride powder according to claim 1 , wherein the metal coupling agent is one or more coupling agents selected form the group consisting of titanium coupling agents, silane coupling agents, zirconium coupling agents, and aluminum coupling agents.

4. An aggregated boron nitride powder comprising boron nitride aggregated grains, wherein the boron nitride aggregated grains have the following characteristics (A) to (D):
(A) the boron nitride aggregated grains are formed by aggregation of hexagonal h-BN primary particles;
(B) the boron nitride aggregated grains have any one or more of Si, Ti, Zr, Ce, Al, Mg, Ge, Ga, and V in an amount of 0.1 atm % or more and 3.0 atm % or less in its composition on a surface of 10 nm,
(C) the boron nitride aggregated grains have a crushing strength of 5 MPa or more; and
(D) the aggregated boron nitride powder has an average particle diameter of 20 μm or more and 100 μm or less.

5. The aggregated boron nitride powder according to claim 4 , wherein the boron nitride aggregated grains further have organic functional groups on the surface.

6. The aggregated boron nitride powder according to claim 5 , wherein the organic functional group present on the surface of the boron nitride aggregated grains is one or more groups selected from epoxy groups that may be substituted, styryl groups that may be substituted, alkyl groups that may be substituted, vinyl groups that may be substituted, acetylacetate groups that may be substituted, acyl groups that may be substituted, isocyanate groups that may be substituted, cyclohexyl groups that may be substituted and tetraoctyl bis(ditridecyl phosphite) groups that may be substituted.

7. A thermally conductive composition, comprising the surface-treated aggregated boron nitride powder according to claim 1 .

8. A thermally conductive composition, comprising the aggregated boron nitride powder according to claim 4 .

Assignees

• Denka Company Ltd

Inventors

• Takeda Go
• Taniguchi Yoshitaka

Classifications

• C09K5/14 Primary

  Solid materials, e.g. powdery or granular · CPC title

• C01B21/0645

  Preparation by carboreductive nitridation · CPC title

• C01B21/0648 Primary

  After-treatment, e.g. grinding, purification (transformation of hexagonal into cubic or wurtzitic boron nitride C04B35/5831) · CPC title

• C08K3/38

  Boron-containing compounds · CPC title

• C08K9/02

  Ingredients treated with inorganic substances · CPC title