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Preparation method of submicron spherical silica powder

A spherical silica, sub-micron technology, applied in the direction of silica, silicon oxide, etc., can solve the problems of product purity decline, unsuitable for large-scale production, high equipment requirements, and achieve good filling and fluidity, The preparation process is safe and environmentally friendly, and the preparation method is simple.

Active Publication Date: 2018-04-13
JIANGSU NOVORAY NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The first two patents belong to the reaction in the solution. The organic matter, acid, alkali and the waste materials and waste water produced are relatively polluting to the environment. They are not suitable for large-scale production and do not meet the current environmental protection requirements. The third patent product is spherical Carbon, one of the raw materials used, is easily mixed into SiO gas, resulting in a decrease in product purity, and the conductivity of carbon causes serious failure of semiconductor packaging. The fourth patent uses metal silicon to prepare submicron spherical silica powder. During the process Explosion will occur, the temperature will rise sharply, and the requirements for equipment are high. At the same time, it will also cause dust explosion, and the safety is poor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1, a preparation method of submicron spherical silica powder, the steps are as follows:

[0017] (1) Raw material: select silica powder as raw material, the specific surface area of ​​the raw material = 6.8 m 2 / g, the ratio of D90 to D10 is 3.6;

[0018] (2) Preparation: Use oxygen as the carrier gas, liquefied natural gas as combustible gas, and oxygen as the combustion aid. The liquefied natural gas and oxygen are separately introduced into the burner and ignited. The temperature of the flame in the burner is greater than 1800°C, and the raw material is in the carrier gas. It enters into the combustion furnace under protection and spheroidizes to obtain spherical silica powder with average particle size D50=1.8μm; the flow of combustible gas is 250Nm 3 / h, the flow of combustion-supporting agent is 500 Nm 3 / h, the carrier gas flow rate is 150 Nm 3 / h, the feeding frequency is 50Hz.

Embodiment 2

[0019] Embodiment 2, a method for preparing submicron spherical silica powder, the steps are as follows:

[0020] (1) Raw material: select silica powder as the raw material, the specific surface area of ​​the raw material = 10.5m 2 / g, the ratio of D90 to D10 is 11.0;

[0021] (2) Preparation: Use oxygen as the carrier gas, liquefied natural gas as combustible gas, and oxygen as the combustion promoter. The liquefied natural gas and oxygen are respectively introduced into the combustion furnace and ignited. The raw materials enter the combustion furnace under the protection of the carrier gas. The temperature of the flame is greater than 1800°C, spheroidization, that is, spherical silica powder with an average particle size D50=0.6μm is obtained; the flow of combustible gas is 90Nm 3 / h, the flow of combustion-supporting agent is 180Nm 3 / h, the carrier gas flow rate is 180 Nm 3 / h, the feeding frequency is 30Hz.

Embodiment 3

[0022] Example 3, a method for preparing submicron spherical silica powder, the steps are as follows:

[0023] (1) Raw material: select silicon nitride powder as the raw material, the specific surface area of ​​the raw material =9.8m 2 / g, the ratio of D90 to D10 is 3.0;

[0024] (2) Preparation: Air is used as carrier gas, LNG is used as combustible gas, and oxygen is used as combustion aid. Liquefied natural gas and oxygen are separately introduced into the combustion furnace and ignited. The temperature of the flame in the combustion furnace is greater than 1800°C, and the raw materials are in the carrier gas. It enters the combustion furnace under protection and spheroidizes to obtain spherical silica powder with an average particle size of D50=0.4μm; the flow of combustible gas is 120Nm 3 / h, the flow of combustion-supporting agent is 240 Nm 3 / h, the carrier gas flow is 130 Nm 3 / h, the feeding frequency is 60Hz.

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Abstract

The present invention is a preparation method of submicron spherical silica powder, which uses silicon-containing inorganic compound powder as a raw material, and the ratio of D90 to D10 is less than 15; Using oxygen or air as the carrier gas, liquefied natural gas as the combustible gas, and oxygen as the combustion aid, the liquefied natural gas and oxygen are respectively introduced into the combustion furnace and ignited. The raw materials enter the combustion furnace under the protection of the carrier gas and are spheroidized to obtain Silica powder with average particle size D50=0.3‑3μm. The silicon dioxide micropowder prepared by the invention has a high sphericity and can obtain an average particle diameter D50=0.3-3 μm, so the filling amount and fluidity are good, the preparation method is simple, and the preparation process is safe and environment-friendly.

Description

Technical field [0001] The invention relates to a method for preparing silicon dioxide, in particular to a method for preparing submicron spherical silicon dioxide powder using silicon-containing inorganic compound powder as a raw material. Background technique [0002] With the development of electronic equipment in the direction of miniaturization and thinning, the particle size of the filler for semiconductor packaging is expected to be smaller and smaller. In order to improve the filling amount and fluidity of the filler in the semiconductor packaging, it is necessary to prepare submicron fillers with high sphericity. [0003] In the prior art: The patent No. 200410012854.8 is based on the reaction of silicate or alkaline silica sol with acid, stirring, standing and aging, then separating, washing and drying to obtain a particle size of 5μm -10nm submicron and nanometer Spherical silica powder; [0004] The patent with application number 201410015493.6 is based on organosilicate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18
Inventor 张建平姜兵
Owner JIANGSU NOVORAY NEW MATERIAL CO LTD