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Preparation method of electronic-level crystalline silicon powder

A silicon micropowder, crystalline technology, applied in the direction of silicon oxide, silicon dioxide, etc., to achieve the effect of reducing the process and reducing the cost

Inactive Publication Date: 2011-12-14
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cost of chemical synthesis is high; the preparation of electronic-grade crystalline silicon micropowder using natural quartz as raw material needs to be purified, and the currently disclosed purification methods generally use magnetic separation and hydrofluoric acid pickling for purification, and pickling will pollute the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 4), according to the ratio of step 2), add distilled water and sodium silicate to mix the slurry, and clean according to the method of step 2) and step 3);

[0018] 5), repeat step 4) three times;

[0019] 6) Ultrasonic cleaning: according to the weight ratio of silicon micropowder: deionized water = 35:65, add deionized water into the mixing tank to make slurry, and stir at the same time, stir for 15 minutes after adding the material and add ultrasonic vibration at the same time;

[0020] 7), stop stirring, after the slurry is clearly stratified, remove the cleaning water;

[0021] 8), repeat step 6), step 7) once;

[0022] 9) Dry the cleaned silicon micropowder in a drying oven until the water content is less than or equal to 0.05%, and obtain electronic grade crystalline silicon micropowder in a sub-circular shape.

[0023] Prepared silicon micropowder, SiO 2 99.89%, Al 2 o 3 0.089%, Fe 2 o 3 0.009%, loss on ignition 0.00%, density 2.67, conductivity of sil...

Embodiment 2

[0028] 4), according to the proportion of step 2), add distilled water and sodium silicate to stir and mix the slurry, and clean according to the method of step 2) and step 3).

[0029] 5), repeat step 4) three times.

[0030] 6) Ultrasonic cleaning: add deionized water into the mixing tank according to the weight ratio of silicon micropowder: deionized water = 30:70, and stir at the same time. After adding the materials, stir for 15 minutes and add ultrasonic vibration at the same time.

[0031] 7) Stop stirring, and drain the cleaning water after the slurry is clearly stratified.

[0032] 8), repeat step 6), step 7) once more.

[0033] 9) Dry the cleaned silicon micropowder in a drying oven until the water content is less than or equal to 0.05%, and obtain electronic grade crystalline silicon micropowder in a sub-circular shape.

[0034] Prepared silicon micropowder, SiO 2 99.89%, A1 2 o 3 0.074%, Fe 2 o 3 0.008%, loss on ignition 0.00%, density 2.65, conductivity ...

Embodiment 3

[0039] 4), according to the proportion of step 2), add distilled water and sodium silicate to stir and mix the slurry, and clean according to the method of step 2) and step 3).

[0040] 5), repeat step 4) three times.

[0041] 6) Ultrasonic cleaning: add deionized water into the mixing tank according to the weight ratio of silicon micropowder: deionized water = 25:75, and stir at the same time. After adding the materials, stir for 15 minutes and add ultrasonic vibration at the same time.

[0042] 7) Stop stirring, and drain the cleaning water after the slurry is clearly stratified.

[0043] 8), repeat step 6), step 7) once more.

[0044] 9) Dry the cleaned silicon micropowder in a drying oven until the water content is less than or equal to 0.05%, and obtain electronic grade crystalline silicon micropowder in a sub-circular shape.

[0045] Prepared silicon micropowder, SiO 2 99.89%, Al 2 o 3 0.066%, Fe 2 o 3 0.006%, loss on ignition 0.00%, density 2.68, conductivity ...

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PUM

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Abstract

The invention relates to a preparation method of electronic-level crystalline silicon powder, which comprises the following steps of: (1) crushing to obtain silicon powder of different grain diameters; (2) stirring and washing: putting the crushed silicon powder in a stirring barrel, adding distilled water and sodium silicate to mix, stir, precipitate and dewater and repeatedly washing 3 or 4 times; (3) ultrasonically cleaning: adding distilled water to the silicon powder obtained after stirring and washing to mix, stir, precipitate and dewater, repeating the washing step twice and using ultrasonic concussion in the stirring and precipitating processes; and (4) finally, drying the silicon powder obtained in the step (3) by ultrasonically cleaning. The invention has the technical advantages that natural quartz powder is used as a raw material, ultrasonic cleaning is adopted without acid cleaning or magnetic separation so as to avoid acid pollution, reduce working procedures and decrease the cost, and the electronic-level crystalline silicon powder product is subrounded. The method can be applied to the preparation of electrical-level and filler-level crystalline silicon powder.

Description

technical field [0001] The invention relates to a preparation method of electronic grade crystalline silicon micropowder. Background technique [0002] There are two types of electronic grade silica powder, one is electronic grade crystalline silica powder, the other is electronic grade fused silica powder (People's Republic of China Electronics Industry Standard SJ / T 10675-2002—Silicon dioxide for electronics and electrical industry Micropowder). Electronic grade silicon micropowder can be used in plastic packaging compound for integrated circuits and electronic components, epoxy castable and potting compound, with high added value and good market prospect. [0003] At present, there are two main methods for preparing electronic grade crystalline silicon micropowder: chemical synthesis method, natural quartz crushing and purification method. The cost of chemical synthesis is high; the preparation of electronic-grade crystalline silicon micropowder from natural quartz req...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18
Inventor 张德
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)