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Preparation method of nonspherical nanometer-scale silica sol

A nano-scale silica sol, non-spherical technology, applied in the chemical industry, can solve the problems of easy sedimentation, affecting product use, high viscosity, etc., and achieve the effect of good stability and high polishing rate

Inactive Publication Date: 2012-03-28
JIANGSU TIANHENG NANO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high production cost of large particle size silica sol, and its high viscosity, it is easy to settle, which affects the use of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Preparation of non-spherical nano-scale silica sol

[0021] Weigh 850g of industrial water glass, add 6375g of pure water, add the diluted water glass solution into the activated strong-acid cation exchange resin under the condition of stirring, and carry out ion exchange to obtain active silicic acid, whose pH value is 3 ~4.

[0022] Weigh 300g of active silicic acid, add it into a three-necked bottle, adjust its pH value to 10 with 20% mixed alkali (potassium carbonate: pyridine = 1:1), stir and heat to 90-100°C, keep warm for 0.5h , and then add 600g of active silicic acid within 2h, during which the above-mentioned mixed alkali aqueous solution is added dropwise to keep the pH value of the reaction system in the range of 9-10, and keep warm for 0.5h after the dropwise addition.

[0023] Weigh 500g of the above-mentioned small particle size non-spherical silica sol with a concentration of 2.48% as a mother liquor, add it into a three-neck bottle, adjust i...

Embodiment 2

[0025] Example 2 Preparation of non-spherical nano-scale silica sol

[0026] Weigh 1200g of industrial water glass, add 6000g of pure water, add the diluted water glass solution into the activated strong acid cation exchange resin under the condition of stirring, and carry out ion exchange to obtain active silicic acid, whose pH value is 3 ~4.

[0027] Weigh 300g of active silicic acid, add it into a three-necked bottle, adjust its pH value to 10 with a 15% mixed alkali (potassium carbonate:pyridine=1:2) solution, stir and heat to 90-100°C, keep it warm for 1h, Then add 400g of active silicic acid within 1h, during which the above mixed alkali solution is added dropwise to keep the pH value of the reaction system in the range of 9-10, and keep warm for 1h after the dropwise addition.

[0028] Weigh 500g of the above-mentioned small particle size non-spherical silica sol with a concentration of 2.48% as a mother liquor, add it into a three-neck bottle, adjust its pH value to...

Embodiment 3

[0031] Example 3 Preparation of non-spherical nano-scale silica sol

[0032] Weigh 850g of industrial water glass, add 6375g of pure water, add the diluted water glass solution into the activated strong-acid cation exchange resin under the condition of stirring, and carry out ion exchange to obtain active silicic acid, whose pH value is 3 ~4.

[0033] Weigh 300g of active silicic acid, add it into a three-necked bottle, adjust its pH value to 10 with 20% mixed alkali (potassium carbonate: pyridine = 1:1), stir and heat to 90-100°C, keep warm for 0.5h , and then add 1000g of active silicic acid within 3 hours, add 20% potassium carbonate solution dropwise in the early stage of the reaction process, and add 20% pyridine solution dropwise in the later stage to keep the pH value of the reaction system in the range of 9 to 10, and keep warm for 0.5h after the dropwise addition .

[0034] Weigh 500g of the above-mentioned small particle size non-spherical silica sol with a conce...

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Abstract

The invention provides a preparation method of nonspherical nanometer-scale silica sol. The preparation method comprises the following steps of: with 2-5 percent of small-size nonspherical silica sol as seed crystals, dropwise adding a 5-40% mixed base solution, adjusting the pH value to 10, stirring and heating to 90-100 DEG C; and then dropwise adding active silicic acid to the system, maintaining a constant liquid level by adopting a heating concentration method, reacting for 10-40h and dropwise adding the mixed base solution to keep the pH value of the reaction system to 9-11 in the reaction peroid. The preparation method of the nonspherical nanometer-scale silica sol has the beneficial effects that: the nonspherical silica sol with grain size of 30-50nm is prepared by using the small-size nonspherical silica sol as the seed crystals, therefore the stability is good; the preparation method is suitable for chemically mechanical polishing and high polishing speed, and the polishing speed is accelerated by more than 10 percent compared with the polishing speed of the spherical silica sol with large size (130nm).

Description

technical field [0001] The invention relates to a preparation method of non-spherical nano-scale silica sol, which belongs to the technical field of chemical industry. Background technique [0002] With the development of integrated circuit technology, it puts forward very high requirements on the surface quality of the substrate materials used. Chemical-mechanical polishing (CMP) technology achieves surface planarization during integrated circuit manufacturing through the joint action of chemistry and machinery, and obtains high-precision, low-roughness and non-damaging material surfaces. At present, the polishing liquid products mainly use spherical silica as the abrasive. In order to improve the polishing rate of the silica-based polishing liquid, large particle size silica sol is mostly used at home and abroad, and its particle size is usually greater than 100nm. However, due to the high production cost of large particle size silica sol, and its high viscosity, it is ea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/14B82Y40/00
Inventor 李家荣唐会明张金平
Owner JIANGSU TIANHENG NANO SCI & TECH
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