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A kind of preparation method of ultrahigh-purity amorphous spherical silica powder

A technology of spherical silicon micropowder and amorphous state, applied in the direction of silicon oxide, silicon dioxide, etc., can solve the problems of high equipment cost, low spheroidization rate, corrosion of metal equipment, etc., and achieve uniform particle size distribution, high spheroidal rate, and dispersed high degree of effect

Active Publication Date: 2016-09-07
苏州西丽卡电子材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method disclosed in Japanese patent JPA58145613 uses natural quartz powder as raw material to melt-spray to prepare spherical silica powder. Since natural quartz powder contains a large amount of impurities, the purity is not high, especially radioactive elements cannot be removed, and the product quality cannot be guaranteed.
Chinese patent CN102826550 discloses that natural quartz minerals are used to prepare ultra-fine angular quartz powder, which is then calcined into spherical silica powder by flame method. The spherical silica powder prepared by this method has high impurity content and SiO 2 content Only 99.9%, the spheroidization rate is low, and radioactive elements cannot be removed, and the production process is complicated and the equipment cost is high
This method cannot cleanly remove harmful chloride ions. In addition, SiCl 4 is a highly dangerous chemical that easily corrodes metal equipment and introduces impurities
Chinese patents CN1188075 and CN101704528 use organic solvent as the reaction medium and silicate / sulfuric acid as raw material to prepare spherical silicon micropowder by water-in-oil emulsification method. The alkali metal in the silicate raw material in this method cannot be removed cleanly, and the purity cannot be reached. very high
Utilizing a large amount of organic solvent as the reaction medium also increases the preparation cost of spherical silica powder
In addition, the spherical silicon micropowder prepared by using water glass as raw material has a high metal impurity content. It is very difficult to reduce the impurity content in silicate to 10PPM by using ion exchange resin technology, and the Al, B, High-valent metal ions such as Zr cannot be removed by ion exchange, so it is impossible to prepare high-purity or ultra-high-purity spherical silica powder using previous methods

Method used

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  • A kind of preparation method of ultrahigh-purity amorphous spherical silica powder
  • A kind of preparation method of ultrahigh-purity amorphous spherical silica powder
  • A kind of preparation method of ultrahigh-purity amorphous spherical silica powder

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Experimental program
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Effect test

Embodiment 1

[0028] Mix 30g of purified tetramethoxysilane (TMOS) with 4g of pure water and a small amount of hydrochloric acid evenly. After the reaction is completed, methanol is distilled off to obtain a silane polymer. Add 100g of pure water and 4g of Tween to the prepared silane polymer. -80 and 0.2g polyether modified silicone oil, stir well with a mixer, emulsify with a homogeneous emulsifier for 10 minutes, add 4g of 25% ammonia water and stir for 3 hours, and add the filter cake obtained by vacuum filtration to an aqueous solution containing 8% ammonia water Reflux for 2 hours, filter and wash with ethanol twice, dry at 80°C for 6h, and calcined at 900°C for 1 hour to obtain spherical silica powder.

[0029] The spherical silica powder prepared by the above steps is analyzed by X-ray diffraction to be pure amorphous silica, and no crystallization occurs when calcined at 900 °C; the particle size distribution is uniform as shown in Figure 1, and the median diameter of the silica pow...

Embodiment 2

[0034]Mix 20g of purified tetraethoxysilane (TEOS) with 3g of pure water and a small amount of nitric acid evenly. After the reaction is completed, distill off ethanol to obtain a silane polymer. Add 100g of pure water and 2g of Op-10 to the silane polymer and 0.1g of silicone antifoaming agent, stir evenly with a mixer, emulsify with a homogeneous emulsifier for 30 minutes, add 5g of 15% tetramethylammonium hydroxide, stir for 4 hours, and centrifuge to obtain SiO 2 The microspheres were added to an aqueous solution containing 10% tetramethylammonium hydroxide and refluxed for 3 hours. After centrifugation, they were washed 3 times with propylene glycol monomethyl ether, dried at 100 °C for 6 hours, and calcined at 1000 °C for 1 hour to obtain spherical silica powder. .

[0035] The spherical silicon micropowder prepared by the above steps is analyzed by X-ray diffraction to be pure amorphous silica, and no crystallization occurs when calcined at 1000 ℃; the particle size ...

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Abstract

The invention discloses a method for preparing ultra-high-purity amorphous spherical silicon micropowder, which comprises the following steps: adding water and a catalyst to condense high-purity organosilane purified by rectification into a polymer; silane polymer, pure water, emulsifier and The additives are mixed evenly and emulsified into an emulsion using a homogeneous emulsifier; ammonia water or an organic base is added to the emulsion to make the silane polymer react under alkaline conditions to form spherical silicon micropowder; after the reaction, the emulsion is separated from the solid and liquid to obtain SiO2 microspheres , and then place the SiO2 microspheres in an alkaline aqueous solution to heat and reflux; the SiO2 microspheres obtained by solid-liquid separation after reflux are washed with a water-miscible organic solvent and then dried, and the dried SiO2 microspheres are calcined in a high-temperature furnace, that is Obtain spherical silica powder. Its purity is extremely high, the content of all metal impurities is below 1PPM, there is no radioactive α-ray pollution, the nodularization rate is over 95%, and the particle size is controllable within the range of 2um‑30um.

Description

technical field [0001] The invention relates to a preparation method of ultra-high-purity amorphous spherical silicon micropowder Background technique [0002] High-purity molten spherical silica powder is a new type of inorganic non-metallic material with excellent properties such as high insulation, high heat resistance, high humidity resistance, acid and alkali corrosion resistance, low expansion, and good fluidity. Spherical silica powder is mainly used for large-scale integrated circuit packaging. The use of spherical silica powder in the preparation process of electronic packaging can greatly improve the rigidity, wear resistance, weather resistance, flame resistance, impact resistance, pressure resistance and durability of packaging products. Arc insulating and UV radiation resistant properties. Spherical microsilica powder has good fluidity and is easy to disperse evenly in the resin. The filling rate of spherical silica micropowder is high, which can be as high as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18
Inventor 刘亚王宇湖
Owner 苏州西丽卡电子材料有限公司
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