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Preparation method of cerium-doped silica sol

A silicon dioxide and cerium doping technology, applied in polishing compositions containing abrasives and other directions, can solve problems such as low hardness, and achieve the effects of reducing equipment cost, simple process and high removal rate

Inactive Publication Date: 2012-02-08
JIANGSU TIANHENG NANO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the problem that the hardness of silica sol abrasives used in microelectronics industry polishing is small, and to carry out metal doping experiments without changing the original process of preparing silica sol to obtain silica with higher hardness. Abrasives, thereby improving the polishing rate of abrasives, meeting the surface quality requirements of the electronic industry for aluminum nitride substrates, and providing a preparation method for cerium-doped silica sol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation method of the cerium-doped silica sol of the present embodiment comprises the following steps:

[0028] 1) 20g of 20nm silica sol obtained by ion exchange method is used as seed crystal, and diluted with water to 500g. Add 4g of NaOH to make the pH value of the seed crystals in the range of 9-10, and raise the temperature to 60-90°C;

[0029] 2) Dissolve 1.5 g of ceric ammonium nitrate and 3 g of pure water into an aqueous solution of ceric ammonium nitrate for subsequent use;

[0030] 3) Heat the seed crystal in step (1) to 60-90°C with stirring, start adding 20g of silicon powder, and then add 10g of silicon powder, 5g 5wt% NaOH and 0.2g of nitric acid prepared in step (2) every 30 minutes Cerium ammonium aqueous solution;

[0031] 4) According to the sequential feeding method of step (3), repeat adding 10 times;

[0032] 5) After the feeding is completed, continue to stir and react for 1h; the reaction is completed;

[0033] Experi...

Embodiment 2

[0035] The preparation method of the cerium-doped silica sol of the present embodiment comprises the following steps:

[0036] 1) 20g of 20nm silica sol obtained by ion exchange method is used as seed crystal, and diluted with water to 500g. Add 4g of NaOH to make the pH value of the seed crystals in the range of 9-10, and raise the temperature to 60-90°C;

[0037] 2) Dissolve 1.5 g of ceric ammonium nitrate and 3 g of pure water into an aqueous solution of ceric ammonium nitrate for subsequent use;

[0038] 3) Heat the seed crystal in step (1) to 60-90°C with stirring, start adding 20g of silicon powder, and then add 10g of silicon powder, 5g 5wt%NaOH and 0.3g of nitric acid prepared in step (2) every 30 minutes Cerium ammonium aqueous solution;

[0039] 4) According to the sequential feeding method of step (3), repeat adding 10 times;

[0040] 5) After the feeding is completed, continue to stir and react for 1h; the reaction is completed;

[0041] Experime...

Embodiment 3

[0043] The preparation method of the cerium-doped silica sol of the present embodiment comprises the following steps:

[0044] 1) 20g of 20nm silica sol obtained by ion exchange method is used as seed crystal, and diluted with water to 500g. Add 4g of NaOH to make the pH value of the seed crystals in the range of 9-10, and raise the temperature to 60-90°C;

[0045] 2) Dissolve 1.5 g of ceric ammonium nitrate and 3 g of pure water into an aqueous solution of ceric ammonium nitrate for subsequent use;

[0046] 3) Heat the seed crystal in step (1) to 60-90°C with stirring, start adding 20g of silicon powder, and then add 10g of silicon powder, 5g 5wt%NaOH and 0.1g of nitric acid prepared in step (2) every 30 minutes Cerium ammonium aqueous solution;

[0047] 4) According to the sequential feeding method of step (3), repeat adding 10 times;

[0048] 5) After the feeding is completed, continue to stir and react for 1h; the reaction is completed;

[0049] Experimental...

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Abstract

The invention provides a preparation method of cerium-doped silica sol, which comprises the following steps: 1) using silica sol with different particle sizes obtained by an ion exchange method as a seed, adding a certain amount of an alkali catalyst for controlling the seed with pH value of 9-10, heating to the temperature of 60-90 DEG C; 2) dissolving a certain amount of ammonium ceric nitrate to an ammonium ceric nitrate aqueous solution by adding pure water for standby; 3) heating by using water-bath, heating the seed in a step 1) while stirring to the temperate of 60-90 DEG C, adding a certain amount of silicon powder, adding a certain amount of silicon powder and a certain amount of the ammonium ceric nitrate aqueous solution in a step 2) every 30-45 minutes; 4) repeatedly adding for 5-10 times according to a charging mode in a step 3); 5) continuously stirring and reacting for 1-2 hours after the charging is finished. The invention has the following technical effects: 1, the growth period is short, the technology is simple, and the method of the invention can be used in grinding and polishing of a CMP technology rough polishing process; 2, the method is beneficial to the equipment cost reduction and safe production; 3, the method enables higher removal rate to the medium materials during the polishing process.

Description

technical field [0001] The invention relates to a method for preparing metal cerium-doped silica sol, which belongs to the technical field of microelectron chemical mechanical polishing or planarization. Background technique [0002] With the development of microelectronics technology towards device miniaturization and multi-layer structure, in order to make the surface of semiconductor substrate materials and integrated circuit chips achieve nanometer or even atomic level flatness, chemical mechanical polishing (CMP) or planarization is required. chemical process. [0003] Chemical mechanical polishing uses the synergistic effect of chemical etching and mechanical grinding to achieve rapid global planarization of the material surface. In the chemical mechanical polishing process, the polishing fluid plays a dual role of chemical corrosion and mechanical grinding. The polishing fluid consists of abrasives, soluble chemicals and water medium. The abrasives provide mechanica...

Claims

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Application Information

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IPC IPC(8): C09G1/02
Inventor 李家荣唐会明徐功涛马超
Owner JIANGSU TIANHENG NANO SCI & TECH
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