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Preparation method of large-size silicon nitride crucible

A silicon nitride crucible and large-scale technology, applied in the field of crucibles, can solve rare problems and other problems, and achieve the effects of simple operation, stable resistivity and high quality of silicon crystals

Inactive Publication Date: 2015-10-28
烟台同立高科新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, silicon nitride crucibles with large size and low impurity content have become the preferred crucibles for silicon crystal ingots, but at present, there are few reports on such crucibles

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) After uniformly mixing silicon nitride powder, polyacrylic acid, silicon dioxide powder, silicon magnesium nitride, polyvinyl alcohol and a solvent, a slurry is obtained;

[0029] Among them, the α phase content in silicon nitride powder is ≥80%, the purity is ≥99.99%, and the particle size is submicron; the amount of polyacrylic acid added is 3% of the weight of the silicon nitride powder; the purity of silicon dioxide is ≥99.99%, and the particle size It is submicron, the mass ratio of silicon dioxide and silicon magnesium nitride is 1:3, and the addition amount of the two is 2% of the weight of silicon nitride powder; the purity of polyvinyl alcohol is ≥99.9%, and the degree of polymerization is 1000 , the addition amount is 1.5‰ of the weight of the silicon nitride powder; the addition amount of the solvent is 30% of the weight of the silicon nitride powder, and the solvent is a mixture of water and ethanol with a volume fraction ≥ 95% in a volume ratio of 1:1; t...

Embodiment 2

[0034] (1) After uniformly mixing silicon nitride powder, polyethylene glycol, silicon dioxide powder, silicon magnesium nitride, polyvinyl alcohol and a solvent, a slurry is obtained;

[0035] Among them, the content of α phase in the silicon nitride powder is ≥80%, the purity is ≥99.99%, and the particle size is submicron; the amount of polyethylene glycol added is 1% of the weight of the silicon nitride powder; the purity of silicon dioxide is ≥99.99% , the particle size is submicron, the mass ratio of silicon dioxide and magnesium silicon nitride is 1:1, and the addition amount of the two is 10% of the weight of the silicon nitride powder; polyvinyl alcohol, the degree of polymerization is 1000, and the addition amount is 1‰ of the weight of silicon nitride powder; the amount of solvent added is 70% of the weight of silicon nitride powder, and the solvent is a mixture of water and ethanol with a volume fraction ≥ 95% in a volume ratio of 1:1; the solid of the obtained slurr...

Embodiment 3

[0040] (1) Add silicon nitride powder, humic acid, silicon dioxide powder, magnesium silicon nitride, carboxymethyl cellulose and solvent into the ball mill, and wet mix with 100r / min ball mill for 10 hours. After mixing evenly, a slurry is obtained. ;

[0041] Among them, the α-phase content in the silicon nitride powder is ≥80%, the purity is ≥99.99%, and the particle size is submicron; the amount of humic acid added is 1% of the weight of the silicon nitride powder; the purity of silicon dioxide is ≥99.99%, and the particle size is It is submicron, the mass ratio of silicon dioxide and silicon nitride magnesium is 1:9, and the addition amount of the two is 1% of the weight of the silicon nitride powder; the addition amount of carboxymethyl cellulose is 1% of the silicon nitride powder 3‰ of the weight; the amount of solvent added is 50% of the weight of the silicon nitride powder, and the solvent is a mixture of water and ethanol with a volume fraction ≥ 95% in a volume rat...

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Abstract

The invention discloses a preparation method of a large-size silicon nitride crucible. According to the method, (1) silicon nitride powder, a dispersing agent, sintering aids, a binding agent and a solvent are well mixed, such that a slurry is obtained; (2) the slurry is added into a mold cavity of a gypsum mold under stirring; the mold is placed in an environment with constant temperature and constant humidity, such that the mold can absorb and discharge water; and a molded cured blank is obtained; (3) a mold core and side molds of the mold are removed, and the molded cured blank is placed in a curing furnace, such that the product is cured and dried, and a green body is obtained; (4) the green body is placed in a gas pressure sintering furnace, and is subjected to segmented sintering; when sintering is finished, the temperature is reduced, the pressure is released and the product is fetched from the furnace, such that the silicon nitride crucible is obtained. According to the invention, silicon dioxide and magnesium silicon nitride are adopted as sintering aids, such that the prepared silicon nitride crucible has low oxygen impurity and metal impurity contents, large bulk density, high high-temperature strength, and large size. The crucible can be widely applied in various non-ferrous metal smelting and silicon crystal ingot casting. The preparation method is simple to operate, and is easy to popularize.

Description

technical field [0001] The invention relates to a method for preparing a large-size silicon nitride crucible, which belongs to the technical field of crucibles. Background technique [0002] As a renewable resource, solar energy has attracted more and more people's attention, and the development of solar energy resources has become one of the new driving forces for economic development. Among the solar cells using solar energy, polycrystalline silicon cells are more cost-effective and become the most advantageous solar power generation device, with a market share of more than 80%. The preparation process of silicon crystal directly affects the performance, quality and production cost of solar cells. Quartz crucible (the main component is silicon dioxide) is a necessity for polycrystalline silicon ingot production. However, there are many problems in using quartz crucible. [0003] Quartz crucibles are mainly used to make silicon into a molten state in a high temperature env...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/584C04B35/622
Inventor 郭大为陆宁宋丽岑吕东
Owner 烟台同立高科新材料股份有限公司
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