Polydisperse large-particle-size silica sol and preparing method thereof

A technology of silica sol and large particle size, which is applied in the field of chemical engineering, can solve the problems of environmental pollution, difficult removal of organic alkali, poor stability of silica sol system, etc., and achieve the effect of improving polishing efficiency and simple process

Active Publication Date: 2016-10-26
SHANGHAI XINANNA ELECTRONICS TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of non-spherical silica generally introduces a divalent or trivalent metal salt solution, which will cause the stability of the silica sol system to deteriorate; or the preparation process uses an organic alkali solution, which is not easy to remove in the silica sol system, which is easy to cause environmental pollution

Method used

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  • Polydisperse large-particle-size silica sol and preparing method thereof
  • Polydisperse large-particle-size silica sol and preparing method thereof
  • Polydisperse large-particle-size silica sol and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1 Polydisperse large particle size silica sol and preparation method thereof

[0029] Step (1) Dilute the concentrated water glass with pure water to a silicon dioxide content of 4%, stir evenly and add it into the regenerated strong acid type cation exchange resin (polybenzenesulfonic acid type) for cation exchange to obtain Active silicic acid, active silicic acid has a pH of 2.85 and a silica content of 4%.

[0030] Step (2) Take 1000mL of 1wt% potassium hydroxide solution, stir and heat to 98°C, and pump 4000ml of active silicic acid prepared in the above step (1) through a peristaltic pump at a speed of 8ml / min. After the addition of active silicic acid, the temperature was continued for 0.5 hours. Naturally cool to room temperature to prepare a monodisperse spherical silica sol with a particle size of 20nm-30nm as a seed crystal.

[0031] Step (3) Weigh 800ml of the seed crystal prepared in the above step (2) as the mother liquor, stir and heat to boi...

Embodiment 2

[0033] Embodiment 2 Polydisperse large particle size silica sol and preparation method thereof

[0034] Step (1) Dilute the concentrated water glass with pure water to a silica content of 2%, stir evenly and add it into the regenerated strong acid type cation exchange resin (polybenzenesulfonic acid type) for cation exchange to obtain active Silicic acid, active silicic acid has a pH of 3.0.

[0035] Step (2) Take 1500mL of 0.3wt% sodium hydroxide solution, stir and heat to 100°C, and pump 3500ml of active silicic acid prepared in the above step (1) through a peristaltic pump at a speed of 3.5ml / min. After the addition of silicic acid was completed, the temperature was continued for 1.5 hours. Naturally cool to room temperature to prepare a monodisperse small-diameter spherical silica sol with a particle diameter of 20nm-30nm as a seed crystal.

[0036] Step (3) Weigh 1000ml of the seed crystal prepared in the above step (2) as the mother liquor, stir and heat to boiling, ad...

Embodiment 3

[0038] Embodiment 3 Polydisperse large particle size silica sol and preparation method thereof

[0039]Step (1) Dilute the concentrated water glass with pure water to a silica content of 6%, stir evenly and add it into the regenerated strong acid type cation exchange resin (polybenzenesulfonic acid type) for cation exchange to obtain active Silicic acid, active silicic acid has a pH of 2.74.

[0040] Step (2) Take 1500mL of 0.3wt% sodium hydroxide solution, stir and heat to 100°C, and pump 3500ml of active silicic acid prepared in the above step (1) through a peristaltic pump at a speed of 3.5ml / min. After the addition of silicic acid was completed, the temperature was continued for 2 hours. Naturally cool to room temperature to prepare a monodisperse small-diameter spherical silica sol with a particle diameter of 20nm-30nm as a seed crystal.

[0041] Step (3) Weigh 800ml of the seed crystal prepared in the above step (2) as the mother liquor, stir and heat to boiling, add t...

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Abstract

The invention provides polydisperse large-particle-size silica sol and a preparing method thereof. The silica sol is mainly used as a polishing solution for increasing polishing speed. The preparing method includes the following steps that monodisperse spherical silica sol with the particle size of 20-30 nm is used as seed crystal, stirred and heated, the monodisperse spherical silica sol with the particle size of 20-30 nm and active silicic acid are continuously added into a reaction system dropwises, a heating concentration method is adopted in the whole reaction process to maintain constant liquid level, in the period, an inorganic base dilute solution is added dropwises to keep the pH value of the system at 9.5-10.5, and the mixed solution cooled after heat preservation. The silica sol prepared through the method is capable of effectively increasing polishing speed and reducing scratches.

Description

technical field [0001] The invention relates to a silica sol and a preparation method thereof, in particular to a polydisperse large particle size silica sol and a preparation method thereof, belonging to the field of chemical engineering. Background technique [0002] With the high development of integrated circuit technology, the requirements for the surface quality of the substrate materials used are getting higher and higher. Due to the reduction of device size and the reduction of focal depth of optical lithography equipment, the flatness of acceptable resolution on the wafer surface is required to reach the nanometer level. In order to solve this problem, the chemical mechanical polishing (CMP) technology capable of achieving global planarization has become one of the important key processes of semiconductor manufacturing in one fell swoop. At present, the polishing liquid products mainly use monodisperse silicon oxide as the abrasive, and there are two traditional si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/14B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B33/14C01P2004/03C01P2004/32C01P2004/64C01B33/145C09G1/02C09K3/1463H01L21/30625
Inventor 孔慧刘卫丽宋志棠
Owner SHANGHAI XINANNA ELECTRONICS TECH
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