CN112852564A - Silicon material cleaning agent and cleaning method - Google Patents
Silicon material cleaning agent and cleaning method Download PDFInfo
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- CN112852564A CN112852564A CN202110023152.3A CN202110023152A CN112852564A CN 112852564 A CN112852564 A CN 112852564A CN 202110023152 A CN202110023152 A CN 202110023152A CN 112852564 A CN112852564 A CN 112852564A
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- 239000002210 silicon-based material Substances 0.000 title claims abstract description 61
- 238000004140 cleaning Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 27
- 238000002791 soaking Methods 0.000 claims abstract description 35
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 24
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000003599 detergent Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 2
- 238000004804 winding Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 4
- 239000002253 acid Substances 0.000 abstract description 15
- 239000000243 solution Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000536 complexating effect Effects 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000010790 dilution Methods 0.000 abstract description 2
- 239000012895 dilution Substances 0.000 abstract description 2
- 238000011086 high cleaning Methods 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/08—Acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
-
- C11D2111/14—
Abstract
The invention discloses a silicon material cleaning agent which comprises the following raw materials in parts by weight: 1-99 parts of hydrofluoric acid, 1-99 parts of hydrochloric acid, 1-99 parts of nitric acid, 1-99 parts of ethanol, 1-99 parts of citric acid and 1-99 parts of water. The silicon material cleaning solution has high cleaning efficiency, can realize large-batch treatment on the silicon material, and does not need large-scale automatic equipment for auxiliary completion; the cleaning effect is good, the complexing effect of the surface of the silicon material is better than the corrosion effect of mixed acid, and organic impurities and complexing surface metals on the surface of the silicon material can be efficiently dissolved; the surface of the silicon material is not corroded in the cleaning process, and the silicon material is not corroded due to the principle of complex reaction, so that the cleaning discharge rate of the silicon material is improved; the cleaning solution cleans silicon materials by adopting a soaking mode, the time is short and is generally 3-4 hours, the soaking process does not need manual operation and equipment operation, and the cleaning by pure water can be completed after soaking; the cleaning process is environment-friendly and pollution-free, the personal harm is reduced in the production process, and the discharge up to the standard can be realized through dilution in the discharge process.
Description
Technical Field
The invention relates to a silicon material cleaning agent and a cleaning method, in particular to the technical field of cleaning agents.
Background
At present, solar silicon raw materials are mainly primary polycrystalline materials and single crystal circulating redrawing materials in the production process, various pollutants are usually found on the surface in production and logistics transportation, the pollutants generally come from metal particles, silicon particles and other metal substances, cutting liquid and the like, and the pollutants can be strongly adsorbed on the surface of the silicon materials, so that the qualification rate and the yield of products are seriously influenced.
The traditional cleaning method is generally a mixed acid cleaning method, hydrofluoric acid and nitric acid are mixed according to a certain proportion, a silicon material is put into a mixed acid solution after stirring, and the mixed acid is used for corroding the surface of the silicon material in a stirring and pickling process, so that the purposes of removing impurities such as precipitation on the surface of the silicon material and attaching metal ions are achieved. In addition, if the mixed liquid is adopted, toxic nitrogen oxide gas can be generated, the problem of environmental pollution in the production of the solar cell is aggravated, particularly, the discharged tail gas forms a yellow smoke phenomenon, and the yellow smoke phenomenon can be combined with moisture in the air to form nitrous acid mist (namely acid rain).
The traditional acid washing method needs to frequently replace and supplement acid liquor, the cost of washing materials is relatively increased, and particularly, the price of hydrofluoric acid is higher. The acid gas is discharged in the acid washing process, higher requirements on the sealing performance of equipment are required, and the labor protection equipment of personnel must be matched for protection, so that the operation cost of acid washing is increased. In addition, the corrosion process of the mixed acid solution has a process of oxidation-reduction-reaction-after-self-catalysis, the reaction speed is slow and fast, the control is not easy, the re-washing rate of the unqualified product after acid washing is high, and the acid cost is increased.
Disclosure of Invention
The invention aims to provide a silicon material cleaning agent.
In order to achieve the purpose, the invention provides the following technical scheme: the silicon material cleaning agent comprises the following raw materials in parts by weight: 1-99 parts of hydrofluoric acid, 1-99 parts of hydrochloric acid, 1-99 parts of nitric acid, 1-99 parts of ethanol, 1-99 parts of citric acid and 1-99 parts of water.
Further preferably, the silicon material cleaning agent comprises the following raw materials in parts by weight: 50 parts of hydrofluoric acid, 50 parts of hydrochloric acid, 50 parts of nitric acid, 50 parts of ethanol, 50 parts of citric acid and 50 parts of water.
A cleaning method of a silicon material cleaning agent comprises the following steps: immersing the silicon material cleaning agent on the surface of the silicon material
More than 5cm, adopting a soaking mode, sealing by covering or using a winding film in the soaking process of a soaking container without heating, standing and storing in a ventilated and cool place, wherein the soaking container is made of a PP plate, polytetrafluoroethylene and other metal-free plastic materials;
the soaking time is 3-5 hours, the specific cleaning time is distinguished according to the type of the product,
observing the surface condition of the product during soaking;
the cleaned silicon material is washed by pure water or ultrasonic wave to remove surface residues
The reagent does not need to use other chemicals such as a detergent, and the surface of the cleaned product does not remain.
Compared with the prior art, the invention has the following beneficial effects: the silicon material cleaning solution has high cleaning efficiency, can realize large-batch treatment on the silicon material, and does not need large-scale automatic equipment for auxiliary completion; the cleaning effect is good, the complexing effect of the surface of the silicon material is better than the corrosion effect of mixed acid, and organic impurities and complexing surface metals on the surface of the silicon material can be efficiently dissolved; the surface of the silicon material is not corroded in the cleaning process, and the silicon material is not corroded due to the principle of complex reaction, so that the cleaning discharge rate of the silicon material is improved; the cleaning process is simple and convenient to operate, the cleaning solution cleans the silicon material in a soaking mode, the time is short and is generally 3-4 hours, the soaking process does not need manual operation and equipment operation, and the cleaning by pure water can be completed after soaking; the cleaning process is environment-friendly and pollution-free, the cleaning solution has weak acid performance, the personal harm is reduced in the production process, and the discharge up to the standard can be realized through dilution in the discharge process.
Drawings
FIG. 1 is a flow chart of a cleaning method of the silicon material cleaning agent of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely in the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The silicon material cleaning agent comprises the following raw materials in parts by weight: 1 part of hydrofluoric acid, 1 part of hydrochloric acid,
1 part of nitric acid, 1 part of ethanol, 1 part of citric acid and 1 part of water; referring to fig. 1, the cleaning method of the silicon material cleaning agent of the embodiment includes: the silicon material cleaning agent is immersed by 5cm on the surface of the silicon material, a soaking mode is adopted, a soaking container needs to be covered and sealed in the soaking process without heating, the soaking container is placed in a ventilated and shady place for standing and storage, a PP plate is selected as the soaking container, the soaking time is 3 hours, the surface condition of a product is observed during soaking, the cleaned silicon material can be washed by pure water or ultrasonic waves, the surface residual reagent can be removed, other chemicals such as a detergent and the like do not need to be used, and no residue exists on the surface after cleaning. The silicon material cleaned by the method has smooth surface, bright section, no foreign matters and no impurity color, and the cleaning yield reaches 97.6%.
Example 2
The silicon material cleaning agent comprises the following raw materials in parts by weight: 99 parts of hydrofluoric acid, 99 parts of hydrochloric acid, 99 parts of nitric acid, 99 parts of ethanol, 99 parts of citric acid and 99 parts of water; the cleaning method of the silicon material cleaning agent comprises the following steps: the silicon material cleaning agent is immersed 6cm on the surface of the silicon material, a soaking mode is adopted, a soaking container needs to be covered and sealed in the soaking process without heating, the soaking container is placed in a ventilated and cool place for standing and storage, the soaking container is made of polytetrafluoroethylene materials, the soaking time is 4 hours, the surface condition of a product is observed during soaking, the cleaned silicon material can be washed by pure water or ultrasonic waves, the surface residual reagent can be removed, other chemicals such as a detergent and the like do not need to be used, and no residue exists on the surface after cleaning. The surface of the cleaned silicon material is smooth, the section of the cleaned silicon material is bright, foreign matters and variegated are avoided, and the cleaning yield reaches 98.7%.
Example 3
The silicon material cleaning agent comprises the following raw materials in parts by weight: 50 parts of hydrofluoric acid, 50 parts of hydrochloric acid, 50 parts of nitric acid, 50 parts of ethanol, 50 parts of citric acid and 50 parts of water; the cleaning method of the silicon material cleaning agent comprises the following steps: the silicon material cleaning agent is immersed by 5.5cm on the surface of the silicon material, a soaking mode is adopted, a soaking container needs to be covered and sealed in the soaking process without heating, the soaking container is placed in a ventilated and shady place for standing and storage, a PP plate is selected as the soaking container, the soaking time is 3.5 hours, the surface condition of a product is observed during soaking, the cleaned silicon material can be washed by pure water or ultrasonic waves, the surface residual reagent can be removed, other chemicals such as a detergent and the like do not need to be used, and no residue exists on the surface after cleaning. The surface of the cleaned silicon material is smooth and bright without foreign matters, the cleaning yield reaches 99.1 percent,
comparative example: mixing hydrofluoric acid and nitric acid according to the mass ratio of 2:1, stirring, then putting the silicon material into a mixed acid solution, and carrying out a stirring and pickling process, wherein the cleaning time is 4 hours, the surface of the cleaned silicon material is smooth, the cross section and the section are bright, but the chromaticity is not uniform enough, and the cleaning yield reaches 90.5%.
Therefore, the cleaning effect of the silicon gel is better in the embodiments 1 to 3, and the cost of the silicon material cleaning agent in the embodiments 1 to 3 is lower than that of the comparative cleaning mode.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A silicon material cleaning agent is characterized in that: the cleaning agent comprises the following raw materials in parts by weight: 1-99 parts of hydrofluoric acid, 1-99 parts of hydrochloric acid, 1-99 parts of nitric acid, 1-99 parts of ethanol, 1-99 parts of citric acid and 1-99 parts of water.
2. The silicon material cleaning agent as claimed in claim 1, wherein: the silicon material cleaning agent comprises the following raw materials in parts by weight: 50 parts of hydrofluoric acid, 50 parts of hydrochloric acid, 50 parts of nitric acid, 50 parts of ethanol, 50 parts of citric acid and 50 parts of water.
3. A cleaning method of a silicon material cleaning agent is characterized by comprising the following steps: the specific method comprises the following steps: immersing the silicon material cleaning agent into the silicon material surface for more than 5cm, adopting an immersion mode, sealing by covering or using a winding film in the immersion process of an immersion container without heating, standing and storing in a ventilated and shady place, wherein the immersion container is made of a PP plate, polytetrafluoroethylene and other metal-free plastic materials;
the soaking time is 3-5 hours, the specific cleaning time is specifically distinguished according to the type of the product, and the surface condition of the product is observed during the soaking period;
the cleaned silicon material can be washed by pure water or ultrasonic waves to remove residual reagents on the surface, other chemicals such as a detergent and the like are not needed, and no residue is left on the surface after cleaning.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110023152.3A CN112852564A (en) | 2021-01-08 | 2021-01-08 | Silicon material cleaning agent and cleaning method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110023152.3A CN112852564A (en) | 2021-01-08 | 2021-01-08 | Silicon material cleaning agent and cleaning method |
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| CN112852564A true CN112852564A (en) | 2021-05-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110023152.3A Pending CN112852564A (en) | 2021-01-08 | 2021-01-08 | Silicon material cleaning agent and cleaning method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653667A (en) * | 2022-03-31 | 2022-06-24 | 乌海市晶易硅材料有限公司 | Cleaning method for removing oxide layer on surface of silicon material |
| CN114653668A (en) * | 2022-03-31 | 2022-06-24 | 乌海市晶易硅材料有限公司 | Method for removing oxide layer on surface of silicon material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104512894A (en) * | 2013-09-27 | 2015-04-15 | 东莞市长安东阳光铝业研发有限公司 | Treatment method of silicon block |
| CN110257176A (en) * | 2019-07-30 | 2019-09-20 | 锦州众尔泰实业有限公司 | A kind of silicon material degumming cleaning agent |
| CN111154565A (en) * | 2019-12-31 | 2020-05-15 | 宁夏中晶半导体材料有限公司 | Silicon material cleaning agent |
-
2021
- 2021-01-08 CN CN202110023152.3A patent/CN112852564A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104512894A (en) * | 2013-09-27 | 2015-04-15 | 东莞市长安东阳光铝业研发有限公司 | Treatment method of silicon block |
| CN110257176A (en) * | 2019-07-30 | 2019-09-20 | 锦州众尔泰实业有限公司 | A kind of silicon material degumming cleaning agent |
| CN111154565A (en) * | 2019-12-31 | 2020-05-15 | 宁夏中晶半导体材料有限公司 | Silicon material cleaning agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653667A (en) * | 2022-03-31 | 2022-06-24 | 乌海市晶易硅材料有限公司 | Cleaning method for removing oxide layer on surface of silicon material |
| CN114653668A (en) * | 2022-03-31 | 2022-06-24 | 乌海市晶易硅材料有限公司 | Method for removing oxide layer on surface of silicon material |
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Application publication date: 20210528 |