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Preparation method of high-purity low-uranium submicron spherical silicon dioxide micropowder

A spherical silica, sub-micron technology, applied in the direction of silica, silicon oxide, etc., can solve the problems of high raw material requirements, difficulty in making products, unstable U content of products, etc., and achieve the effect of low raw material requirements

Pending Publication Date: 2022-02-11
JIANGSU NOVORAY NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, the existing low-uranium spherical silica powder preparation methods have the following problems: Although high-purity low-uranium products can be obtained through chemical synthesis by selecting high-purity organic silicon sources and solvents, this method will bring environmental problems ; Choose 1ppm low-uranium natural quartz alone, only micron-scale products can be obtained, and the requirements for raw materials are relatively high, and it is difficult to achieve products below 0.5ppb; select raw material Si that has been strictly screened, and undergo simple acid treatment. The U content of the product is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Under the protection of argon, 10 kg and 80 mm of elemental silicon (purity 99.6%, uranium content 15 ppb) were calcined in a high-temperature furnace at 1250 ° C for 15 h. After the calcination, it is quenched with water, broken into sand materials below 1mm, and dried by sedimentation. The calcining-crushing-sedimentation drying step is recycled once. Collect the dried sand material several times for later use.

[0028] (2) Weigh 250kg of dried sand and add it to 230kg of water, and add 0.05kg of 1.5% hydrofluoric acid solution, and wet ball mill to obtain a powder slurry with an average particle size of 35 μm.

[0029] (3) Transfer the slurry to the reactor, add 15kg, 1.5% HF solution and 15kg, 0.5% HCl solution, add 0.1% hydrogen peroxide accounting for the mass of the mixed acid solution, and add flotation agent and collector to recover Uranium element was stirred at 60°C for 24 hours to obtain a slurry.

[0030] (4) Press-filter, wash and dry the powder slu...

Embodiment 2

[0033] (1) Under the protection of argon, 10kg and 35mm of silicon nitride (purity 99.8%) and elemental silicon (purity 99.6%) were calcined in a high-temperature furnace at 900°C for 5 hours. After the calcination, it is quenched with water, broken into sand materials below 1mm, and dried by sedimentation. The calcining-crushing-sedimentation drying step is recycled once. Collect the dried sand material several times for later use.

[0034] (2) Add 250kg of dried sand material to 230kg of water, and add 0.05kg of 1.5% hydrofluoric acid solution, and wet ball mill to obtain a powder slurry with an average particle size of 30 μm.

[0035] (3) Transfer the slurry to the reactor, add 15kg, 1.5% HF solution and 15kg, 0.5% HCl solution, add 0.3% hydrogen peroxide accounting for the mass of the mixed acid solution, and add flotation agent and collector to recover Uranium element was stirred at 60°C for 24 hours to obtain a slurry.

[0036] (4) Press-filter, wash and dry the powde...

Embodiment 3

[0039] (1) Under the protection of argon, 10kg and 70mm of silicon nitride (purity 99.6%) were calcined in a high-temperature furnace at 850°C for 15h. After the calcination, it is quenched with water, broken into sand materials below 1mm, and dried by sedimentation. The calcining-crushing-sedimentation drying step is recycled once. Collect the dried sand material several times for later use.

[0040] (2) Add 250kg of dried sand material into 230kg of water, and add 0.05kg of 1.5% hydrofluoric acid solution, and wet ball mill to obtain a powder slurry with an average particle size of 35 μm.

[0041] (3) Transfer the slurry to the reactor, add 15kg, 1.5% HF solution and 15kg, 1.5% HCl solution, add 0.1% hydrogen peroxide accounting for the mass of the mixed acid solution, and add flotation agent and collector to recover Uranium element was stirred at 35°C for 12 hours to obtain a slurry.

[0042] (4) Press-filter, wash and dry the powder slurry to obtain a powder with a uran...

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Abstract

The invention discloses a preparation method of high-purity low-uranium submicron spherical silicon dioxide micropowder. The method comprises the following steps: calcining, crushing, settling and drying a blocky raw material into a sand material with the particle size of less than 1mm, carrying out wet ball milling on the sand material into powder slurry, adding a mixed acid composed of hydrofluoric acid and hydrochloric acid into the powder slurry, adding hydrogen peroxide, recovering uranium element, carrying out filter pressing, washing and drying on the powder slurry to prepare powder with the uranium content being less than 1.0 ppb, and finally carrying out flame balling to obtain the submicron spherical silicon dioxide micro powder. The method has low requirements on raw materials and is suitable for various industrial grade silicon sources, and the prepared submicron grade spherical silicon dioxide micro powder is low in U content and stable.

Description

technical field [0001] The invention belongs to the technical field of preparation of heat-conducting fillers, and relates to a preparation method of high-purity and low-uranium submicron spherical silica powder. Background technique [0002] Electronic equipment is developing towards small and thin, and the particle size of fillers for semiconductor packaging is getting smaller and smaller. At the same time, in order to improve the filling amount and fluidity of the filler in the semiconductor package, it is necessary to add a submicron filler with a high degree of sphericity (generally considered to be 0.1 μm to 1 μm). However, with the continuous improvement of the integration of ultra-large integrated circuits, the distance between wires is getting smaller and smaller, and packaging materials such as memory chips, when the α rays in the packaging materials are strong, will cause soft errors in signal transmission, thereby reducing the reliability of integrated circuits. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/32C01P2006/80C01P2004/62C01P2004/61Y02E30/30
Inventor 张建平曹家凯李晓冬阮建军姜兵朱刚
Owner JIANGSU NOVORAY NEW MATERIAL CO LTD