Preparation method of high-purity silica sol

A silica sol, high-purity technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of mechanical damage, semiconductor material pollution, high impurity content, etc., and achieve low cost, simple preparation steps, and high purity Effect

Inactive Publication Date: 2016-07-20
JIANGSU SHIKONG COATING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention: Aiming at the high impurity content in the high-purity silica sol prepared from water glass as raw material, which will cause semiconductor material pollution or mechanical damage, a kind of quartz sand as the main raw material is provided. Under the action of sodium, sodium metasilicate is generated, and

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0018] First, weigh 150g of quartz sand, rinse it with clean water, pulverize it into a 120-mesh powder in a pulverizer, and then soak it in 23% hydrochloric acid for 50 minutes, and filter it with deionization. After rinsing the filtered material with water for 3 times, place it in an oven at 50℃ and dry it for 50min. After the drying is complete, place it in a calcination furnace. Under the protection of nitrogen, the calcination time is 50min and the temperature is 500℃. After the end, let it cool to room temperature naturally to obtain pure quartz sand powder; then weigh 40 g of pure quartz sand powder prepared above and 250 mL of 30% sodium hydroxide solution with mass fraction, mix and stir for 40 minutes, and then mix The turbid liquid was transferred to the reaction kettle, heated to 550°C, and the pressure of the reaction kettle was adjusted to 10MPa. When there was no precipitation in the reaction kettle, the temperature was lowered to 50°C, and 15% of the mixed liquid...

example 2

[0021] First, weigh 100g of quartz sand, rinse it with clean water, place it in a pulverizer and pulverize it into 100 mesh powder, and then soak it in 23% hydrochloric acid for 40 minutes, and filter it with deionization. After rinsing the suction filter twice with water, place it in an oven at 40℃ and dry it for 40min. After the drying is completed, place it in a calcination furnace. Under the protection of nitrogen, the calcination time is 40min and the temperature is 400℃. After calcination, let it cool to room temperature naturally to obtain pure quartz sand powder; then weigh 30 g of pure quartz sand powder prepared above and 200 mL of a 30% sodium hydroxide solution with a mass fraction of 30%, mix and stir for 30 minutes, and then The mixed turbid liquid is transferred to the reaction kettle, heated to 500°C, and the pressure of the reaction kettle is adjusted to 9MPa. When there is no precipitation in the reaction kettle, after cooling it to 45°C, add 10% hydrogen by ma...

example 3

[0023] First, weigh 120g of quartz sand, rinse it with clean water, place it in a pulverizer and pulverize it into 110 mesh powder, and then soak it in 23% hydrochloric acid for 45 minutes, and filter it with deionization. After rinsing the filtered material twice with water, it was placed in an oven at 45℃ and dried for 45min. After the drying was completed, it was calcined in a calcining furnace. Under the protection of nitrogen, the calcination time was 45min and the temperature was 450℃. After the calcination, let it cool naturally to room temperature to obtain pure quartz sand powder; then weigh 35 g of pure quartz sand powder prepared above and 210 mL of 30% sodium hydroxide solution with mass fraction, mix and stir for 35 minutes, and then The mixed turbid liquid is transferred to the reactor, heated to 520℃, and the pressure of the reactor is adjusted to 9MPa. When there is no precipitation in the reactor, after cooling it to 47℃, add 12% hydrogen by mass of the mixed li...

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Abstract

The invention relates to a preparation method of high-purity silica sol and belongs to the technical field of silica sol preparation. The preparation method includes: flushing and smashing quartz sand, disposing in hydrochloric acid for soaking, performing suction filtering, flushing a suction filtering product, drying, calcining, and cooling to room temperature to obtain quartz sand powder; mixing the quartz sand powder with a sodium hydroxide solution, transferring into a reaction kettle, heating, cooling when no precipitate exists in the reaction kettle, adding sodium hydroxide into the reaction kettle, stirring well, cooling to room temperature to obtain sodium metasilicate mixed turbid liquid, mixing the sodium metasilicate mixed turbid liquid with deionized water, heating, cooling, filtering, and collecting filtrate; mixing the filtrate with hydrofluoric acid, feeding hydrogen, heating, cooling to room temperature, filtering, collecting filtrate, disposing the filtrate in hydrochloric acid for soaking, filtering, and drying. Content of metal in the high-purity silica sol is 7-8 ppm, and the high-purity silica sol is high in purity and can be widely used in the manufacturing process of semiconductor devices, polycrystallized modules and flat panel displays.

Description

Technical field [0001] The invention relates to a method for preparing high-purity silica sol, and belongs to the technical field of silica sol preparation. Background technique [0002] Silica sol is a colloidal solution formed by uniformly dispersing aggregated amorphous silica particles in water. It is a nanomaterial with a special structure. Its molecular formula is mSiO2·nH2O, and its colloidal particle size is generally 5-100nm. Due to the large number of hydroxyl groups on the surface of silica particles in silica sol, it has a large reactivity, so it is widely used in textiles, coatings, papermaking, rubber, paint, ceramics, precision casting and electronics industries. Silica sol is a suspended dispersion of silica particles in water. Ultra-high purity silica sol is mainly used for precision polishing of semiconductor materials, such as silicon wafers, germanium wafers, etc., and the chemistry of integrated circuit multilayer wiring The mechanical planarization (CMP) pr...

Claims

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Application Information

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IPC IPC(8): C01B33/141
CPCC01B33/141C01P2006/80
Inventor陈明生薛红娟
OwnerJIANGSU SHIKONG COATING