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Preparation method for SiO2 sol with high evenness degree

A technology of silica and silica sol, applied in the directions of silica and silica, can solve the problems of difficult to obtain silica sol with particle size distribution, application limitation of silica sol, etc., to improve the reaction rate, eliminate local concentration unevenness, high uniformity

Inactive Publication Date: 2011-09-07
TSINGHUA UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of intense mechanical stirring, with the increase of thermal energy and mechanical energy, the probability of silica powder particles and silica sol particles colliding with each other also increases, which leads to further agglomeration, making it difficult to obtain silica sol with a more uniform particle size distribution. Applications in IC polishing are limited

Method used

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  • Preparation method for SiO2 sol with high evenness degree
  • Preparation method for SiO2 sol with high evenness degree
  • Preparation method for SiO2 sol with high evenness degree

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) In a 1000ml three-necked bottle, add 200ml of water, add 20g of metal silicon powder with 300 mesh purity of 98% and 4g of sodium hydroxide, adjust the reaction temperature to 60°C, stir at 200rpm, and react under 50KHZ ultrasonic conditions 2 hours, 15 minutes of ultrasound every 1 hour to prepare silica sol seed liquid;

[0036] (2) In the above-mentioned prepared seed liquid, the reaction temperature was adjusted to 80°C, the stirring rate was 250rpm, and the reaction was carried out under 50KHZ ultrasonic conditions for 2 hours, and 100g of 1wt% sodium hydroxide solution was added for every 1 hour of ultrasonication for 20 minutes. 8g of metal silicon powder with 300 mesh purity of 98%;

[0037] (3) Repeat step (2) twice again, after cooling, get 600g concentration after filtration and be the silica sol of 15wt% uniform particle size distribution, use SEM test particle size to be 35nm, test result is as follows figure 1 , figure 2 It is the SEM picture of the...

Embodiment 2

[0039] (1) In a 1000ml three-necked bottle, add 200ml of water, add 16g of metal silicon powder with 300 mesh purity of 98% and 2g of sodium hydroxide, adjust the reaction temperature to 70°C, stir at 200rpm, and react under 50KHZ ultrasonic conditions 4 hours, 20 minutes of ultrasound every 1 hour to prepare silica sol seed liquid;

[0040] (2) In the seed liquid prepared above, adjust the reaction temperature to 85°C, the stirring rate is 400rpm, and react under 50KHZ ultrasonic conditions for 2 hours, ultrasonic for 15 minutes every hour, and add 120g of 0.8wt% sodium hydroxide solution And 300 mesh purity is 8g of metal silicon powder of 98%;

[0041] (3) repeat step (2) three times again, after cooling, get 600g concentration after filtering and be the silica sol of 16wt% uniform particle size distribution, use SEM test particle size to be 55nm, test result is as follows image 3 .

Embodiment 3

[0043] (1) In a 1000ml three-necked bottle, add 200ml of water, add 17g of 300-mesh metal silicon powder with a purity of 98% and 3g of sodium hydroxide, adjust the reaction temperature to 80°C, stir at 200rpm, and react under 50KHZ ultrasonic conditions 4 hours, 20 minutes of ultrasound every 1 hour to prepare silica sol seed liquid;

[0044] (2) In the seed liquid prepared above, adjust the reaction temperature to 90°C, the stirring rate is 400rpm, and react under 70KHZ ultrasonic conditions for 2 hours, ultrasonic for 15 minutes every hour, and add 120g of 0.6wt% sodium hydroxide solution and 300 meshes of 98% metallic silicon powder 6g;

[0045] (3) repeat step (2) four times again, after cooling, get 800g concentration after filtering and be the silica sol of 12wt% uniform particle size distribution, use SEM test particle size to be 65nm, test result is as follows Figure 4 .

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Abstract

The invention discloses a preparation method for the silica sol with a high evenness degree, belonging to the technical field of electronic manufacturing and SiO2 sol preparation. Under an ultrasonic influence, a silica sol seed solution is prepared and a reaction material is added to the silica sol solution in batches; aqueous solution and metallic silicon powder that serve as basic catalysts are chosen as the reaction material for each batch, and the basic catalyst in each batch is 2-40% of the basic catalyst previously added into the silica sol seed solution, and the metallic silicon powder in each batch is 2-40% of the metallic silicon powder previously added in the silica sol seed solution. After the reaction finishes, the unreacted metallic silicon powder is removed, and the SiO2 sol is produced. The ultrasonic sound adopted for the invention ranges from 20 to 50 kHz. By adopting the invention, production costs can be reduced and product purity is improved. In addition, the method disclosed by the invention has the advantages of safe technical process, simple equipment, and is easy to operate as well as is economic and has high efficiency.

Description

technical field [0001] The invention belongs to electronic manufacturing and SiO 2 The technical field of colloid preparation, in particular relates to a method for preparing silica sol with high uniformity. Background technique [0002] In the field of electronic manufacturing, with the continuous improvement of integrated circuit integration, the characteristic line width has been continuously reduced, and it has entered the nanometer era. While the line width continues to decrease, in order to increase chip output and reduce unit manufacturing costs, the diameter of silicon wafers is required to continue to increase. At present, the mainstream diameter of silicon single crystals in the world is gradually changing from 200mm to 300mm, and the requirements for the surface quality of silicon polished wafers are becoming more and more stringent. [0003] Currently, chemical mechanical polishing (CMP) technology is the main method capable of achieving local and global planar...

Claims

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Application Information

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IPC IPC(8): C01B33/14
Inventor 潘国顺顾忠华雒建斌路新春刘岩
Owner TSINGHUA UNIV
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