CN102989723A - Method for washing high-resistivity and low-resistivity silicon materials - Google Patents

Method for washing high-resistivity and low-resistivity silicon materials Download PDF

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Publication number
CN102989723A
CN102989723A CN2012104099820A CN201210409982A CN102989723A CN 102989723 A CN102989723 A CN 102989723A CN 2012104099820 A CN2012104099820 A CN 2012104099820A CN 201210409982 A CN201210409982 A CN 201210409982A CN 102989723 A CN102989723 A CN 102989723A
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CN
China
Prior art keywords
silicon
acid
resistivity
hydrofluoric acid
water
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Pending
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CN2012104099820A
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Chinese (zh)
Inventor
裘永恒
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JIAXING JIAJING ADVANSIL ELECTRONIC CO Ltd
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JIAXING JIAJING ADVANSIL ELECTRONIC CO Ltd
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Priority to CN2012104099820A priority Critical patent/CN102989723A/en
Publication of CN102989723A publication Critical patent/CN102989723A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for washing high-resistivity and low-resistivity silicon materials. The method comprises the following steps of: soaking the silicon material into hydrofluoric acid or a mixed solution of hydrofluoric acid and ammonium fluoride, after soaking, taking out the silicon material and washing the silicon material to be neutral with water; preparing the mixed solution of hydrofluoric acid and hydrogen nitrate, adding the silicon material into a plastic container, adding the prepared mixed solution, after reaction, lightly swashing the silicon material with clean water, enabling the low-resistivity silicon material to float on water surface, thereby realizing separation of high-resistivity silicon material and low-resistivity silicon material; mixing the mixed solution of hydrofluoric acid, hydrogen nitrate and glacial acetic acid, adding the separated high-resistivity material into the mixed solution, stirring and adding hydrogen peroxide at intervals, then, taking out the material and washing the material to be neutral with water; adding the high-resistivity material into an alkali wash basin, adding solid sodium hydroxide, adding a sodium hydroxide solution simultaneously, stirring for reaction, then, washing the alkali liquor away by the clean water; soaking the high-resistivity material into electronic grade hydrochloric acid, after soaking, washing the high-resistivity material to be clean with pure water; and finally, executing ultrasonic treatment with pure water, and then, fishing out the high-resistivity material, and drying.

Description

The silicon material cleaning method that contains simultaneously high low-resistance
Technical field
The present invention relates to solar power silicon industry cleaning treatment technical field, especially a kind of silicon material cleaning method that contains simultaneously high low-resistance.
Background technology
Traditional processing method is to reach sorting purpose (such as universal meter, electroprobe etc.) by its resistivity of manual testing, for undersized silicon material conventional process, when not only taking a lot of work, output does not increase but also have the uncertain of artificial factor, cause low-resistance to fail to pick out fully, this all is disadvantageous to the materials of next producing.
Summary of the invention
The objective of the invention is to provide for the deficiency that solves above-mentioned technology a kind of high low-resistance that size is less to mix the silicon material cleaning method that contains high low-resistance when low resistance material in the silicon material is effectively removed.
In order to achieve the above object, the silicon material cleaning method that contains high low-resistance that the present invention is designed, cleaning step is as follows:
(1), the silicon material dropped into concentration soak in the mixed solution greater than 40% hydrofluoric acid and ammonium fluoride greater than 40% hydrofluoric acid or concentration, soaked rear taking-up water punching to neutrality;
(2), again the silicon material is dropped in the chloroazotic acid and soak, soaked rear taking-up water punching to neutral;
(3), the mixed solution of configuration hydrofluoric acid and nitric acid, the silicon material is put into plastic containers, add the mixed solution that has just prepared, after both reactions, gently rush with clear water, low resistance material is bubbled through the water column, the low resistance material of bubbling through the water column is poured in the screen cloth, realized that the height resistance material separates;
(4), the mixed solution of configuration hydrofluoric acid, nitric acid, glacial acetic acid, isolated high resistance material is dropped in the mixed solution, stir and the adding hydrogen peroxide at interval, then take out the water punching to neutral;
(5), high resistance material is dropped in the alkali cleaning basin, add sodium hydrate solid, add simultaneously sodium hydroxide solution, wash away alkali lye with clear water behind the stirring reaction;
(6), high resistance material dropped in the electronic grade hydrochloric acid soaks, soaked rear clean with pure water rinsing;
(7), at last use pure water ultrasonic, fish for oven dry after complete.
As optimization, the weight ratio of hydrofluoric acid and ammonium fluoride is 6-10:1 in the first step, and soak time is 48 hours simultaneously; Silicon material soak time in chloroazotic acid is 24 hours in the second step; The concentration of hydrofluoric acid is 49 ± 1% in the 3rd step, the concentration of nitric acid is 68 ± 2%, the mass ratio of hydrofluoric acid and nitric acid is 6-10:1, and both reaction time are 0.5-1 minute, and the concentration of hydrofluoric acid is 49% in the 4th step, and the concentration of nitric acid is 70%, hydrofluoric acid, the volume ratio of nitric acid and glacial acetic acid is 1:3:7-9, and to add volume every 1 hour in the agitation be the hydrogen peroxide of 1/10th equivalent hydrofluoric acid, continues 10 hours; Sodium hydroxide solution and sodium hydrate solid equivalent in the 5th step, stirring reaction 1-3 minute; Hydrochloric acid is 8% electronic grade hydrochloric acid in the 6th step, and soak time is 15-20 minute; Use ultrasonic 2 hours of pure water in the 7th step.
The resulting silicon material cleaning method that contains simultaneously high low-resistance of the present invention, the low resistance material that can be effectively that size is less high low-resistance is mixed in the silicon material effectively separates removal, and the pollutant on high resistance material surface is thoroughly removed, and reaches the cleaning requirement of solar power silicon industry.It is simple to operate, is applicable to mass disposal, has reduced production cost, increases economic efficiency.
The specific embodiment
The present invention is further described by the following embodiment.
Embodiment 1:
Present embodiment contains the silicon material cleaning method of high low-resistance when describing, its step is as follows: configuration concentration is that the mixed solution of 6~10 ︰ 1 is in acid bubble pond greater than 40% hydrofluoric acid solution or concentration greater than the weight ratio of 40% Qing Fu Suan ︰ ammonium fluoride, the silicon material that will give up drops into wherein, soaks 48h.In this process, can remove completely the oxide layer of silicon face; Take out the water punching to neutral, the configuration chloroazotic acid drops into the silicon material in the chloroazotic acid in another acid bubble pond, soaks 24h.This process can be removed the metal contamination on useless silicon material and surface thereof completely; Take out the water punching to neutral, 49 ± 1% Qing Fu Suan ︰, 68 ± 2% nitric acid mixed solutions of configuration 6~10 ︰ 1 are in transferring box, the silicon material is put into plastic tub, add the nitration mixture reaction 0.5~1min that has prepared, water gently rushes, low resistance material is bubbled through the water column, and along with the mobile of water poured in the screen cloth, repetitive operation height group is well separated with the low resistance material of keeping afloat; 49 ± 1% Qing Fu Suan ︰, 68 ± 2% Xiao Suan ︰ glacial acetic acid mixed solutions of configuration volume ratio 1 ︰ 3 ︰ 7~9, High Resistivity Si material on isolating is thrown in wherein, stir, and to add volume every 1 hour be the hydrogen peroxide of 1/10th equivalent hydrofluoric acid, take out the water punching after 10 hours to neutral.This process is high resistance material etch stop, and low-resistance obtains removing thoroughly; High resistance material is dropped in the alkali cleaning basin, add sodium hydrate solid, add simultaneously equivalent in the water of NaOH, stirring reaction 1~3min, water washes out alkali lye.This process will be removed the process layer on useless silicon material surface fully; The silicon material is dropped in 8% the electronic grade hydrochloric acid soaking compartment and soaks 15~20min, totally then use the ultrasonic 2h of pure water with pure water rinsing, fish for oven dry.

Claims (2)

1. silicon material cleaning method that contains high low-resistance, it is characterized in that: cleaning step is as follows:
(1), the silicon material dropped into concentration soak in the mixed solution greater than 40% hydrofluoric acid and ammonium fluoride solid greater than 40% hydrofluoric acid or concentration, soaked rear taking-up water punching to neutrality;
(2), again the silicon material is dropped in the chloroazotic acid and soak, soaked rear taking-up water punching to neutral;
(3), the mixed solution of configuration hydrofluoric acid and nitric acid, the silicon material is put into plastic containers, add the mixed solution that has just prepared, after both reactions, gently rush with clear water, low resistance material is bubbled through the water column, the low resistance material of bubbling through the water column is poured in the screen cloth, realized that the height resistance material separates;
(4), the mixed solution of configuration hydrofluoric acid, nitric acid, glacial acetic acid, isolated high resistance material is dropped in the mixed solution, stir and the adding hydrogen peroxide at interval, then take out the water punching to neutral;
(5), high resistance material is dropped in the alkali cleaning basin, add sodium hydrate solid, add simultaneously sodium hydroxide solution, wash away alkali lye with clear water behind the stirring reaction;
(6), high resistance material dropped in the electronic grade hydrochloric acid soaks, soaked rear clean with pure water rinsing;
(7), at last use pure water ultrasonic, fish for oven dry after complete.
2. the silicon material cleaning method that contains high low-resistance according to claim 1, it is characterized in that: the weight ratio of hydrofluoric acid and ammonium fluoride is 6-10:1 in the first step, soak time is 48 hours simultaneously; Silicon material soak time in chloroazotic acid is 24 hours in the second step; The concentration of hydrofluoric acid is 49 ± 1% in the 3rd step, the concentration of nitric acid is 68 ± 2%, the mass ratio of hydrofluoric acid and nitric acid is 6-10:1, and both reaction time are 0.5-1 minute, and the concentration of hydrofluoric acid is 49% in the 4th step, and the concentration of nitric acid is 70%, hydrofluoric acid, the volume ratio of nitric acid and glacial acetic acid is 1:3:7-9, and to add volume every 1 hour in the agitation be the hydrogen peroxide of 1/10th equivalent hydrofluoric acid, continues 10 hours; Sodium hydroxide solution and sodium hydrate solid equivalent in the 5th step, stirring reaction 1-3 minute; Hydrochloric acid is 8% electronic grade hydrochloric acid in the 6th step, and soak time is 15-20 minute; Use ultrasonic 2 hours of pure water in the 7th step.
CN2012104099820A 2012-10-24 2012-10-24 Method for washing high-resistivity and low-resistivity silicon materials Pending CN102989723A (en)

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CN2012104099820A CN102989723A (en) 2012-10-24 2012-10-24 Method for washing high-resistivity and low-resistivity silicon materials

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CN2012104099820A CN102989723A (en) 2012-10-24 2012-10-24 Method for washing high-resistivity and low-resistivity silicon materials

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106115715A (en) * 2016-06-26 2016-11-16 河南盛达光伏科技有限公司 Polycrystalline silicon ingot casting partly melts the circulation tailing cleaning treatment method that technique produces

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009088388A (en) * 2007-10-02 2009-04-23 Kagawa Univ Solar energy utilization device and its manufacturing method
CN101973552A (en) * 2010-09-21 2011-02-16 江西赛维Ldk太阳能高科技有限公司 Method for separating silicon from impurities
CN102004101A (en) * 2010-09-20 2011-04-06 邢台晶龙电子材料有限公司 Chromogenic solution and method for distinguishing P/N-type silicone materials
CN102351186A (en) * 2011-07-15 2012-02-15 浙江矽盛电子有限公司 Method for recovering silicon material with metal coating on surface
CN102502652A (en) * 2011-11-07 2012-06-20 江西旭阳雷迪高科技股份有限公司 Cleaning process for polycrystalline material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009088388A (en) * 2007-10-02 2009-04-23 Kagawa Univ Solar energy utilization device and its manufacturing method
CN102004101A (en) * 2010-09-20 2011-04-06 邢台晶龙电子材料有限公司 Chromogenic solution and method for distinguishing P/N-type silicone materials
CN101973552A (en) * 2010-09-21 2011-02-16 江西赛维Ldk太阳能高科技有限公司 Method for separating silicon from impurities
CN102351186A (en) * 2011-07-15 2012-02-15 浙江矽盛电子有限公司 Method for recovering silicon material with metal coating on surface
CN102502652A (en) * 2011-11-07 2012-06-20 江西旭阳雷迪高科技股份有限公司 Cleaning process for polycrystalline material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106115715A (en) * 2016-06-26 2016-11-16 河南盛达光伏科技有限公司 Polycrystalline silicon ingot casting partly melts the circulation tailing cleaning treatment method that technique produces

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