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Preparation method of ultrahigh-purity quartz ceramic crucible

A technology of quartz ceramics and quartz crucibles, which is applied in the field of preparation of ultra-high-purity quartz ceramic crucibles, can solve the problems of restricting the development of polysilicon batteries, low photoelectric conversion efficiency, and the quality of silicon ingots, etc., and achieve improved yield, high strength, and energy saving cost effect

Active Publication Date: 2015-09-09
SINOMA JIANGSU SOLAR ENERGY NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the purity of polysilicon is greater than 6N (99.9999wt%) while the purity of ordinary quartz crucible is less than 3N (99.9wt%). Although there is a silicon nitride coating to isolate the ingot, there are still a lot of impurities that penetrate into the silicon ingot, especially Fe, etc. The metal has a serious impact on the quality of the silicon ingot, resulting in a low minority carrier lifetime, which appears red in the scan image of the minority carrier lifetime, which is called the red zone
As a result, the photoelectric conversion efficiency of the small square ingot near the four corners of the crucible (A region) and the small silicon ingot near the front side (B region) is much lower than that of the center (C region), so that the conversion of the whole ingot The efficiency will be greatly reduced, and it will become a bottleneck restricting the development of polysilicon cells. Reducing or even eliminating the pollution of crucibles to silicon ingots is a key part of improving the conversion efficiency of polysilicon cells.
The purity of high-purity quartz sand on the market is mostly 4.5N, and the price is expensive. The high-purity quartz sand above 6N is hundreds or even thousands of yuan per kilogram, and the cost of making an overall high-purity crucible is too unbearable.

Method used

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  • Preparation method of ultrahigh-purity quartz ceramic crucible

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Ultra-high purity quartz ceramic crucible 1

[0041] The preparation process is:

[0042] In step ①, choose an ordinary quartz crucible (purity less than 3N) for backup;

[0043] Step ②, select high-purity silicon powder with different particle sizes: among them, D50 is 700g of 25μm, D50 is 300g of 20μm, D50 is 1000g of 8μm, add 2000g of ultra-pure water and mix to obtain high-purity silicon powder slurry, add 4g Hydrofluoric acid with a concentration of 5wt%, soaked for 5 hours, and the high-purity silicon powder after vacuum drying is set aside;

[0044] In step ③, 1000g of high-purity silicon powder obtained in step ②, 1000g of ultrapure water, and 1000g of silica sol are uniformly mixed, and 1g of sodium polyacrylate, 1g of triethylhexyl phosphoric acid, 1g of fatty acid polyethylene glycol ester, and 1g of melon are added. Er gum, and add 1g polyoxypropylene glyceryl ether, 1g simethicone oil, fully stir for 5 hours and let stand for 10 hours to obtain ...

Embodiment 2

[0049] Example 2 Ultra-high purity quartz ceramic crucible 2

[0050] Its preparation process is:

[0051] In step ①, select an ordinary quartz crucible (purity less than 3N), rinse it with ultrapure water, and soak the rinsed crucible in a mixed solution with a concentration of 5% for 15 hours for later use; the mixed solution is NaF, hydrochloric acid , 1,4-dioxane, hydrogen peroxide mixed solution, its mass ratio is: 1:1.5:0.3:0.5.

[0052] The second step is to select high-purity silicon powder with different particle sizes, wherein the purity of high-purity silicon powder is greater than 6N, D50 is 800g of 25μm, D50 is 300g of 15μm, D50 is 900g of 8μm, and mixed with 2000g of ultrapure water to obtain High-purity silicon powder slurry, add 4g concentration and be the mixed acid of 5wt% hydrofluoric acid, hydrochloric acid, nitric acid, its mass ratio is: 1:2:2, soak 10 hours, the high-purity silicon powder after the vacuum drying waits use;

[0053] In step ③, 1000g of...

Embodiment 3

[0058] Example 3 Ultra-high purity quartz ceramic crucible 3

[0059] Its preparation process is:

[0060] In step ①, select an ordinary quartz crucible (purity less than 3N), rinse it with ultrapure water, and soak the rinsed crucible in a mixed solution with a concentration of 10% for 10 hours, and set aside; the mixed solution is NaF, hydrochloric acid , 1,4-dioxane, hydrogen peroxide mixed solution, its mass ratio is: 1:1:0.3:0.5.

[0061] In step ②, ethyl acetate, molybdenum disulfide, lanthanum oxide, carbon black, γ-(2,3-propylene oxide) propyl trimethoxysilane, diphenyl ether formaldehyde resin, sodium hydroxymethyl cellulose Mix with a certain mass ratio of 0.5:0.1:0.2:0.1:0.5:0.2:0.2, add 0.5 times the amount of ultrapure water to the mixture, stir evenly for 3 hours to form a mixture, and spray the mixture evenly through the spray equipment on the first ① The thickness of the inner surface of the crucible obtained in the first step is controlled at 0.2mm;

[0062...

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Abstract

The invention mainly discloses an ultrahigh-purity quartz ceramic crucible and a preparation method thereof. The ultrahigh-purity quartz ceramic crucible is mainly applied to polycrystalline silicon ingots in the solar photovoltaic industry. The preparation method comprises the steps of treating solar-grade purity silica powder (6N) with different grain sizes, and then, adding silica sol, deionized water, additives and the like according to a certain ratio to prepare slurry with good dispersibility, wherein the solar-grade purity silica powder (6N) with different grain sizes is used as the main raw material; after further treating a common quartz crucible, placing the slurry on the inner surface of the common quartz crucible in a way of coating, brushing and the like; and after drying, oxidizing and sintering in a kiln with an oxidizing atmosphere to obtain the ultrahigh-purity quartz ceramic crucible. By using the preparation method, the ultrahigh-purity quartz ceramic crucible can be obtained, an ultrahigh-purity crucible is produced by breaking the bottleneck of an ultrahigh-purity quartz raw material, impurities are more effectively prevented from entering ingots, side red areas are thoroughly eliminated, bottom red areas are reduced, the conversion efficiency is increased, the cost is reduced while the stability is kept, the porosity is lower, the volume density is higher, the property is more stable, the service life is greatly prolonged, and the using cost is effectively reduced.

Description

technical field [0001] The invention relates to a method for manufacturing a quartz crucible, in particular to a method for preparing an ultrahigh-purity quartz ceramic crucible. Background technique [0002] The polysilicon ingot uses a quartz crucible as a container, and successively undergoes processes such as heating, melting, crystal growth, annealing, and cooling. At present, the purity of polysilicon is greater than 6N (99.9999wt%) while the purity of ordinary quartz crucible is less than 3N (99.9wt%). Although there is a silicon nitride coating to isolate the ingot, there are still a lot of impurities that penetrate into the silicon ingot, especially Fe, etc. Metals have a serious impact on the quality of silicon ingots, resulting in a low minority carrier lifetime, which appears red in the scan image of the minority carrier lifetime, which is called the red zone. As a result, the photoelectric conversion efficiency of the small square ingot near the four corners ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/89C04B35/14
Inventor 孙健谢炎穆荣升
Owner SINOMA JIANGSU SOLAR ENERGY NEW MATERIALS
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