Method for rapidly preparing large-particle-size silica sol

A large particle size, silica sol technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of unstable roughness, prolong the use time of polishing liquid, etc., to reduce the existence of small particle size particles, Quantitative control savings, the effect of accelerating the speed of polymerization

Inactive Publication Date: 2015-04-08
SHENZHEN LEAGUER MATERIAL +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention includes three steps of chemical mechanical polishing, polishing pad cleaning and polishing liquid treatment, and the use of the present inventio

Method used

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  • Method for rapidly preparing large-particle-size silica sol
  • Method for rapidly preparing large-particle-size silica sol
  • Method for rapidly preparing large-particle-size silica sol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Selecting high-purity sodium silicate prepared from fumed silica as a raw material to prepare a water glass solution with a concentration of 6%, the prepared water glass solution is exchanged with a cationic resin to obtain a concentration of 5.3% active silicic acid; Silicic acid passes through anion exchange resin to obtain active silicic acid with higher purity. Take 10 wt% of the prepared active silicic acid, add alkali solution to adjust its pH value to 8.2. Add 0.1wt% stabilizer, heat to 90°C, and keep for 0.5 hours to obtain a silica sol mother solution with a particle size of 8nm. Under constant stirring, keep the silica sol mother liquor in a slightly boiling state (the temperature is 100C), add the remaining active silicic acid therein, add the mixed solution of 0.9wt% stabilizer and 10wt% polymerization inhibitor, and react for 4 hours to obtain granules Silica sol solution with a diameter of 90-140nm. During the reaction, the volume of the reaction solutio...

Embodiment 2

[0032] Selecting high-purity sodium silicate prepared from fumed silica as a raw material to prepare a water glass solution with a concentration of 10%, the prepared water glass solution is exchanged with a cationic resin to obtain a concentration of 8.6% active silicic acid; Silicic acid passes through anion exchange resin to obtain active silicic acid with higher purity. Take part 10wt% of the prepared active silicic acid, add alkali solution to adjust its pH value to 9. Add 0.5wt% stabilizer, heat to 100°C, and keep for 1 hour to obtain a silica sol mother solution with a particle size of 3.4nm. Under constant stirring, keep the silica sol mother liquor in a slightly boiling state, add the remaining active silicic acid to it, add a mixed solution of 0.5wt% stabilizer and 5wt% polymerization inhibitor, and react for 4 hours to obtain a silica sol with a particle size of 90-140nm. Sol solution. During the reaction, the volume of the reaction solution was kept constant by ad...

Embodiment 3

[0034] Select the high-purity sodium silicate prepared by fumed silica as raw material to prepare a water glass solution with a concentration of 1%, and exchange the prepared water glass solution with a cationic resin to obtain a concentration of 0.9% active silicic acid; Silicic acid passes through anion exchange resin to obtain active silicic acid with higher purity. Take part 10wt% of the prepared active silicic acid, add alkali solution to adjust its pH value to 7. Add 0.01wt% stabilizer, heat to 95° C., and keep for 1 hour to obtain a silica sol mother solution with a particle size of 10 nm. Under constant stirring, keep the silica sol mother liquor in a slightly boiling state, add the remaining active silicic acid to it, add a mixed solution of 0.1wt% stabilizer and 0.5wt% polymerization inhibitor, and react for 2 hours to obtain a particle size of 90-140nm Silica sol solution. During the reaction process, the volume of the reaction solution was kept constant by adding...

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Abstract

The invention discloses a method for rapidly preparing large-particle-size silica sol, belongs to the field of inorganic application materials and in particular relates to an ion exchange method for rapidly preparing the large-particle-size silica sol. High-purity sodium silicate prepared by fumed silica is selected as a raw material, activated silica acid and silica mother solution are prepared by virtue of an ion exchange method, the pH value of the silica mother solution is regulated so as to compress a double electrode layer of silica sol particles, and the distance among the nanoparticles is further shortened so as to increase the silica particle size increase rate. Therefore, rapid formation of particle size of large-particle-size silica sol is promoted, narrow particle size distribution can be obtained, and the production efficiency and quality are greatly improved. According to the addition of a stabilizer and a polymerization inhibitor, the effects of preventing aggregation of silica sol and ending the reaction can be respectively achieved, and nanometer silica sol with uniform dispersion and controllable particle size is finally obtained. Compared with the traditional ion exchange method, the method disclosed by the invention has the advantages that the prepared silica sol is high in purity, the particle size distribution is narrow, and the production efficiency is doubled.

Description

technical field [0001] The invention relates to a method for preparing silica sol, in particular to a method for quickly preparing silica sol with large particle size and high purity by an ion exchange method. Background technique [0002] So far, silica sol is still the most important abrasive particle in the planarization process of integrated circuits. Large particle size silica sol can increase the planarization rate, thereby improving manufacturing efficiency and increasing production capacity. In addition, the particle size distribution of silica sol in the planarization process also has a greater impact on integrated circuits: for silica sol with the same solid content and large particle size, a narrower particle size distribution can obtain higher planarization efficiency and surface quality; if the particle size distribution of silica sol is wide, the mechanical effect of the smaller particle size part in the grinding process is very limited, and the larger particl...

Claims

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Application Information

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IPC IPC(8): C01B33/141
Inventor 潘国顺陈高攀顾忠华罗桂海王鑫
Owner SHENZHEN LEAGUER MATERIAL
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