Low dielectric silica powder, resin composition containing the silica powder, and method for manufacturing low dielectric silica powder

Patent metadata

Field	Value
Publication number	US-12441892-B2
Application number	US-202418432451-A
Country	US
Kind code	B2
Filing date	Feb 5, 2024
Priority date	Jun 2, 2020
Publication date	Oct 14, 2025
Grant date	Oct 14, 2025

Abstract

A method for manufacturing a low dielectric silica powder incudes heat-treating a silica powder at a temperature of 500° C. to 1500° C. to achieve 0.0005 or less of a dielectric loss tangent of the silica powder at 10 GHz, and etching a surface of the heat-treated silica powder with an etching solution. A silica powder with an extremely small dielectric loss tangent, a resin composition containing the same, and a method for manufacturing a silica powder with a low dielectric loss tangent and strong adhesion at the interface to resin are achieved.

First claim

The invention claimed is:

1. A method for manufacturing a low dielectric silica powder, comprising:
heat-treating a silica powder at a temperature of 500° C. to 1500° C. to achieve 0.0005 or less of a dielectric loss tangent of the silica powder at 10 GHZ; and
etching a surface of the heat-treated silica powder with an etching solution, wherein the low dielectric silica powder has an average particle size of 0.1 to 30 μm and a dielectric loss tangent of 0.0005 or less at 10 GHz, has, inside and on a surface thereof, 200 ppm or less of a metal and/or a metal oxide in terms of mass of each metal, the metal selected from aluminum, magnesium, and titanium, and 10 ppm or less of an alkali metal and an alkaline earth metal in terms of mass of each, and wherein a hydroxy group (Si-OH) content of the low dielectric silica powder is from 135 ppm or more to 300 ppm or less in terms of mass, wherein the hydroxy group content is quantified by measuring the transmittance of a peak near 3680 cm −1 by infrared spectroscopic analysis, and wherein the hydroxy group is inner silanol.

2. The method for manufacturing a low dielectric silica powder according to claim 1 , wherein the heat treatment is performed for 30 minutes to 72 hours.

3. The method for manufacturing a low dielectric silica powder according to claim 2 , wherein an aqueous solution is used as the etching solution, the aqueous solution selected from an aqueous hydrofluoric acid solution, an aqueous ammonium fluoride solution, an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, an aqueous sodium carbonate solution, ammonia water, and alkaline electrolyzed water.

4. The method for manufacturing a low dielectric silica powder according to claim 3 , wherein a basic aqueous solution with a pH of 11 or higher is used as the etching solution.

5. The method for manufacturing a low dielectric silica powder according to claim 2 , wherein a basic aqueous solution with a pH of 11 or higher is used as the etching solution.

6. The method for manufacturing a low dielectric silica powder according to claim 1 , wherein an aqueous solution is used as the etching solution, the aqueous solution selected from an aqueous hydrofluoric acid solution, an aqueous ammonium fluoride solution, an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, an aqueous sodium carbonate solution, ammonia water, and alkaline electrolyzed water.

7. The method for manufacturing a low dielectric silica powder according to claim 6 , wherein a basic aqueous solution with a pH of 11 or higher is used as the etching solution.

8. The method for manufacturing a low dielectric silica powder according to claim 1 , wherein a basic aqueous solution with a pH of 11 or higher is used as the etching solution.

9. The method for manufacturing a low dielectric silica powder according to claim 8 , wherein alkaline electrolyzed water with a pH of 12 or higher is used as the basic aqueous solution.

10. The method for manufacturing a low dielectric silica powder according to claim 1 , further comprising treating the etched surface of the silica powder with a coupling agent.

Assignees

• Shinetsu Chemical Co

Inventors

• Shiobara Toshio
• Itokawa Hajime

Classifications

• C01P2006/40

  Electric properties · CPC title

• C01P2006/80

  Compositional purity · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C01P2004/03

  obtained by SEM · CPC title