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A kind of silica sol with controllable particle shape and preparation method thereof

A particle morphology, silica sol technology, applied in chemical instruments and methods, silicon compounds, other chemical processes, etc., can solve the problems of large residual metal ions, reduced production efficiency, and low polishing efficiency.

Active Publication Date: 2021-07-20
河北硅研电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the monodisperse spherical colloidal silica used as the grinding medium of the polishing liquid still has the disadvantage of low polishing efficiency, while cocoon-shaped, long-chain and other non-spherical colloidal silica with approximately the same cut surface diameter and a certain degree of association Silicon oxide, due to its large drag area and not easy to cause scratches, has a good application prospect in semiconductor CMP
[0004] The method commonly used in the existing non-spherical silica sol preparation technology is to be converted into silica sol by water glass, and contains a large amount of sodium ions and other metal ions in the raw material, although can remove a part of metal ions by ion exchange resin, but this method is harmful to metal ions. The removal of ions has a certain upper limit, and the residual amount of metal ions is large, which limits the application of silica sol in semiconductor polishing
In addition, if the alkoxysilane hydrolyzate is used as the raw material, because the silicic acid solution has a strong tendency to gel, generally only the mass concentration of silica can be prepared below 5%, and the primary solid content of the final silica sol is too low. lead to lower production efficiency

Method used

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  • A kind of silica sol with controllable particle shape and preparation method thereof
  • A kind of silica sol with controllable particle shape and preparation method thereof
  • A kind of silica sol with controllable particle shape and preparation method thereof

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preparation example Construction

[0049] The embodiment of the present invention provides a preparation method of silica sol with controllable particle shape, comprising the following steps:

[0050] S1: Prepare several groups of acidic combination solutions with a mass content of alkoxysilanes ≥ 95% and mother solutions containing alkali catalysts, high-purity water and organic solvents and 7

[0051] S2: adding a group of the acidic combination liquid to the mother liquor to obtain the first silica sol;

[0052] S3: adding high-purity water and a set of the acidic combination solution to the obtained first silica sol sequentially at least once to obtain a silica sol primary solution;

[0053] S4: The obtained silica sol primary solution is concentrated and solvent replaced to obtain a silica sol product.

[0054] After the acidic combination solution is quickly added to the mother liquor, with the continuous hydrolysis of the alkoxysilane, the concentration of silicic acid and silanol groups in the s...

Embodiment 1

[0058] A preparation method of silica sol with controllable particle shape, comprising the steps of:

[0059] S1: Add 123.8g of tetraethoxysilane with a water content of 0.23% into a 500ml flask with a condensing reflux tube, the condensing tube is connected to the atmosphere through a glass tube containing a desiccant, and the acidity is 0.01mol after heating and reflux under normal pressure / L of acidic liquid. Take 665.3g of tetraethoxysilane and 47.5g of the above acidic liquid as the first group of two-component acidic combination liquid; the above-mentioned acidic liquid of 76.3g and 1068.5g of tetraethoxysilane as the second group of two-component Group acidic combination liquid; mother liquor is made up of 1460.2 ethanol, 572.4 g high-purity water, 8.6 g 26% ammonia water;

[0060] S2: Add the two components of the first group of acidic combination liquid to the above mother liquid in a 10L four-neck flask containing a reflux device, a thermometer and two feeding port...

Embodiment 2

[0069] A preparation method of silica sol with controllable particle shape, comprising the steps of:

[0070]S1: Add 990g of tetraethoxysilane with a water content of 0.23% into a 1000ml flask with a condensing reflux tube, the condensing tube is connected to the atmosphere through a glass tube containing a desiccant, and the acidity is 0.00167mol / The first group of alkoxysilane acidic combination liquid of L; add 1145g of tetraethoxysilane with a water content of 0.23% into a 2000ml flask with a condensing reflux tube, and the condensing tube communicates with the atmosphere through a glass tube containing a desiccant, Heating to reflux under normal pressure to obtain the second group of alkoxysilane acidic combination liquid with an acidity of 0.00077mol / L; add 1145g of tetraethoxysilane with a water content of 0.23% into a 2000ml flask with a condensing reflux tube, and the condensing tube passes through The glass tube containing the desiccant was connected to the atmosphe...

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Abstract

The invention relates to the technical field of semiconductor chemical mechanical polishing, and specifically discloses a silica sol with controllable particle shape and a preparation method thereof. The preparation method comprises the following steps: preparing several sets of acidic combination solutions with a mass content of alkoxysilane ≥ 95% and a mother solution containing an alkali catalyst, high-purity water and an organic solvent; adding a group of the acidic combination solutions to the mother solution In the process, the first silica sol is obtained; at least once, high-purity water and a group of the acidic combination liquid are sequentially added to the obtained first silica sol to obtain the primary silica sol solution; concentration and solvent replacement are obtained to obtain the silica sol product. The preparation method provided by the present invention realizes the controllable shape of silica sol particles by regulating the acid value of the acidic combination liquid of alkoxysilane, and adjusting the change of the acid value of each group of acidic combination liquids added, and obtains spherical and non-spherical Spherical silica sol, the primary solid content of the obtained silica sol is >10%, and the metal ion content is <1ppm.

Description

technical field [0001] The invention relates to the technical field of semiconductor chemical mechanical polishing, in particular to a silica sol with controllable particle shape and a preparation method thereof. Background technique [0002] In recent years, with the continuous development of semiconductor technology, the requirements for the surface quality of the substrate materials used are getting higher and higher. In order to solve this problem, how to realize global planarization chemical mechanical polishing (Chemical Mechanical Polishing, CMP) technology has become one of the key processes in semiconductor manufacturing. [0003] At present, the monodisperse spherical colloidal silica used as the grinding medium of the polishing liquid still has the disadvantage of low polishing efficiency, while cocoon-shaped, long-chain and other non-spherical colloidal silica with approximately the same cut surface diameter and a certain degree of association Silicon oxide, due...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/145C01B33/146C01B33/141C09K3/14B82Y40/00
CPCC01B33/145C01B33/1465C01B33/141C09K3/1409B82Y40/00C01P2004/32C01P2004/30C01P2004/10C01P2004/64C01P2006/10C01P2006/22C01P2006/40C01P2006/80C01P2006/90
Inventor 朱斌仵靖
Owner 河北硅研电子材料有限公司