CN104843711A - Novel solar silicon material pickling method - Google Patents

Novel solar silicon material pickling method Download PDF

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Publication number
CN104843711A
CN104843711A CN201510196136.9A CN201510196136A CN104843711A CN 104843711 A CN104843711 A CN 104843711A CN 201510196136 A CN201510196136 A CN 201510196136A CN 104843711 A CN104843711 A CN 104843711A
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CN
China
Prior art keywords
hno
hno3
adopts
acid
pickling
Prior art date
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Pending
Application number
CN201510196136.9A
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Chinese (zh)
Inventor
张之栋
刘进
张广强
郑兵
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANXI LU'AN SOLAR ENERGY TECHNOLOGY Co Ltd
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SHANXI LU'AN SOLAR ENERGY TECHNOLOGY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by SHANXI LU'AN SOLAR ENERGY TECHNOLOGY Co Ltd filed Critical SHANXI LU'AN SOLAR ENERGY TECHNOLOGY Co Ltd
Priority to CN201510196136.9A priority Critical patent/CN104843711A/en
Publication of CN104843711A publication Critical patent/CN104843711A/en
Pending legal-status Critical Current

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Abstract

The invention relates to the field of solar battery production, and concretely relates to a novel solar silicon material pickling method. The novel solar silicon material pickling method is characterized in that a pickling solution used in an acid tank in the corrosion process is an HF, HNO3 and CH3COOH mixture, HNO3 adopts HNO3 with the mass percentage concentration of 66%, HF adopts HF with the mass percentage concentration of 49%, CH3COOH adopts CH3COOH with the mass percentage concentration of 99.5%, HF, HNO3 and CH3COOH are mixed according to a volume ratio of 5:3:4, and the corrosion time is 45-60s. Acetic acid is adopted as a buffering solvent in order to alleviate the reaction rate, make silicon stably react with the acid mixture and improve the utilization rate of HF and HNO3. The method has the advantages of production cost saving, short corrosion time and production cycle shortening.

Description

A kind of new type solar energy silicon material acid washing method
Technical field
The present invention relates to manufacture of solar cells field, specifically a kind of new type solar energy silicon material acid washing method.
Background technology
Current acid cleaning process adopts Full-automatic acid washing machine, comprises HF+HNO 3the fast floating row of burn into is washed, pure water overflow rinsing, pure water lock, ultrasonic cleaning, N 2cut water, heated drying.The HNO of 66% is used at acid tank 3, 49%HF solution, initially add HNO 3be 8:1 with the ratio of HF, acid tank reaction times parameter is 90s ~ 150s, temperature parameter is 15 DEG C ~ 35 DEG C.
Summary of the invention
Technical problem to be solved by this invention is: how to provide and a kind of pickle solution, the negative impact that this pickle solution energy offset silicon material and nitration mixture process cause soon, and etching time is short simultaneously, and the surface corrosion of silicon material is even, Wu Huangbian.
The technical solution adopted in the present invention is: a kind of new type solar energy silicon material acid washing method, adopts Full-automatic acid washing machine, carry out that the fast floating row of burn into is washed successively, pure water overflow rinsing, pure water lock, ultrasonic cleaning, N 2cut the step such as water, heated drying, temperature parameter is 15 DEG C ~ 35 DEG C, and the pickle solution used in corrosion process acid tank is HF, HNO 3, CH 3c00H tri-kinds of acid mix, wherein HNO 3mass percent concentration is adopted to be the HNO of 66% 3, HF adopts mass percent concentration to be 49%HF, CH 3c00H adopts mass percent concentration to be 99.5%CH 3c00H, according to volume ratio 5:3:4, etching time 45-60s.
The invention has the beneficial effects as follows: acetic acid, as buffer solvent, slow down speed of reaction, make silicon and nitration mixture stable reaction, improve the utilization ratio of HF, HNO3.Save production cost.Etching time is short, shortens the production cycle.
Embodiment
Adopt existing equipment, adopt that fast floating row is washed, pure water overflow rinsing, pure water lock, ultrasonic cleaning, N 2cut the cleaning step of water, heated drying.Change HF and HNO 3acidwash solution proportioning and add CH 3c00H, pickling tank temperature parameter is defined as 15 DEG C ~ 35 DEG C.
First stage: analyze acid cleaning process production leadtime data, determine to affect the main cause of production cycle, the quality of production (yellow limit, corrode uneven etc.).
This phase data is as follows: HNO 3: HF initial ratio is 8:1, initial corrosion time 120s
Technological effect is as follows: the silicon material cleaned out after initial liquid feeding has yellow limit, surface corrosion uneven, produces a large amount of tobacco simultaneously, temperature fluctuation is large
The analysis of causes is as follows: mixed acid solution initial reaction is violent, affects cleaning quality.
Subordinate phase: for main cause, formulates corresponding countermeasure.
Analyze cleaning of the same trade in conjunction with self cleaning experience, determine acid tank chemical reagent (HF, HNO 3, CH 3c00H) and trial scale be respectively 5:1:1,5:2:2,5:3:3(ratio of mixture and all adopt volume ratio).
This phase data is as follows: HNO 3starting point concentration is 66%(mass percent), HF starting point concentration is 49%(mass percent), CH 3c00H starting point concentration is 99.5%(mass percent).
Phase III: implementation measure, Checking on effect
Grouping is tested, and effect is as follows:
1, HNO 3: HF proportioning 5:1 etching time 60s, corrode uneven, silicon material edge is oxidized, has yellow limit
2, HNO 3: HF:CH 3c00H proportioning 5:1:1 etching time 60s, depth of corrosion is shallow, non-oxidation
3, HNO 3: HF:CH 3c00H proportioning 5:2:2 etching time 60s, depth of corrosion is more shallow, and corrosion evenly
4, HNO 3: HF:CH 3c00H proportioning 5:2:2 etching time 90s, silicon material becomes clear, and corrodes even, moderate (surface is optimum)
5, HNO 3: HF:CH 3c00H proportioning 5:3:2 etching time 60s, corrosion scale is dark, has yellow limit, has oxidation
6, HNO 3: HF:CH 3c00H proportioning 5:3:3 etching time 60s, corrosion scale is dark, Wu Huangbian
7, HNO 3: HF:CH 3c00H proportioning 5:3:3 etching time 90s, corrosion scale is dark, Wu Huangbian, faint oxidation
8, HNO 3: HF:CH 3c00H proportioning 5:3:4 etching time 50s, corrosion scale is dark, Wu Huangbian, non-oxidation (surface is optimum, cleaning speed is the fastest).
Sum up: in above-mentioned experimentation, according to HF, HNO 3, CH 3c00H tri-kinds of acid clean out best effect according to the proportioning of 5:3:4, and cleaning speed is the fastest.
This patent increases acetic acid raw material on original Process ba-sis, serves katalysis simultaneously, reduces original materials consumption, has saved cost, and product innovation quality and output are improved.

Claims (1)

1. a new type solar energy silicon material acid washing method, adopts Full-automatic acid washing machine, carry out that the fast floating row of burn into is washed successively, pure water overflow rinsing, pure water lock, ultrasonic cleaning, N 2cut the step such as water, heated drying, temperature parameter is 15 DEG C ~ 35 DEG C, it is characterized in that: the pickle solution used in corrosion process acid tank is HF, HNO 3, CH 3c00H tri-kinds of acid mix, wherein HNO 3mass percent concentration is adopted to be the HNO of 66% 3, HF adopts mass percent concentration to be 49%HF, CH 3c00H adopts mass percent concentration to be 99.5%CH 3c00H, according to volume ratio 5:3:4 mixing, etching time 45-60s.
CN201510196136.9A 2015-04-23 2015-04-23 Novel solar silicon material pickling method Pending CN104843711A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510196136.9A CN104843711A (en) 2015-04-23 2015-04-23 Novel solar silicon material pickling method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510196136.9A CN104843711A (en) 2015-04-23 2015-04-23 Novel solar silicon material pickling method

Publications (1)

Publication Number Publication Date
CN104843711A true CN104843711A (en) 2015-08-19

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510196136.9A Pending CN104843711A (en) 2015-04-23 2015-04-23 Novel solar silicon material pickling method

Country Status (1)

Country Link
CN (1) CN104843711A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101531366A (en) * 2009-03-09 2009-09-16 常州有则科技有限公司 Method for cleaning polycrystalline silicon material
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
CN102757050A (en) * 2011-04-27 2012-10-31 日鑫(永安)硅材料有限公司 Acid cleaning purification method of metallic silicon
CN103435042A (en) * 2013-08-24 2013-12-11 内蒙古盾安光伏科技有限公司 Polycrystalline silicon reduction pickling system

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101531366A (en) * 2009-03-09 2009-09-16 常州有则科技有限公司 Method for cleaning polycrystalline silicon material
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
CN102757050A (en) * 2011-04-27 2012-10-31 日鑫(永安)硅材料有限公司 Acid cleaning purification method of metallic silicon
CN103435042A (en) * 2013-08-24 2013-12-11 内蒙古盾安光伏科技有限公司 Polycrystalline silicon reduction pickling system

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Application publication date: 20150819