CN102644084A - Pre-cleaning agent used before napping monocrystalline silicon piece and application method - Google Patents
Pre-cleaning agent used before napping monocrystalline silicon piece and application method Download PDFInfo
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- CN102644084A CN102644084A CN2012100981624A CN201210098162A CN102644084A CN 102644084 A CN102644084 A CN 102644084A CN 2012100981624 A CN2012100981624 A CN 2012100981624A CN 201210098162 A CN201210098162 A CN 201210098162A CN 102644084 A CN102644084 A CN 102644084A
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Abstract
The invention relates to a pre-cleaning agent used before napping a monocrystalline silicon piece and an application method. The existing main problem is that cleaning fluids in the market at present contain phosphorus substances, and the eutrophication of water quality can be caused if the phosphorus substances are discharged to the environment, and the phosphorus substances are not favorable of the development of efforts at environmental protection. The pre-cleaning agent is characterized by comprising the following components: alkylphenol ethoxylates, inorganic base and salt of the inorganic base, sodium citrate, paratoluenesulfonic acid sodium salt, cosolvent and the balance of water, wherein the deionized water is used as the water preferably. The pre-cleaning agent used before napping the monocrystalline silicon piece has the advantages that the occurrence probability of contaminations, such as fingerprints and spots on the surface of the silicon piece, can be reduced, a napping effect is obviously enhanced, the yield of the silicon piece is further increased, and the production efficiency of enterprises is increased. Moreover, a catalyst used by the pre-cleaning agent is nontoxic, non-corrosive and non-irritant, has no burning and explosion hazards and is not harmful to human bodies and the environment. Moreover, the catalyst is simple in preparation and application process, equipment is cheap and the repeatability is high.
Description
Technical field
The present invention relates to a kind of fine-hair maring using monocrystalline silicon slice preceding pre-washing agent and method of use of being used for.
Background technology
It is one important procedure of preparation solar battery sheet that silicon chip cleans, and this is because the impurity of surface contamination can have a strong impact on performance, the yield rate of battery sheet.The particle of silicon chip surface, metal contamination, organism contamination, natural oxide film etc. can have a strong impact on the efficient and the yield rate of battery sheet.The problem that scavenging solution in the market mainly exists is to contain Phosphorus material, like tripoly phosphate sodium STPP, sodium phosphate etc.These materials are unfavorable for carrying out of efforts at environmental protection if be disposed to the eutrophication that can cause water quality in the environment.If adopt traditional RCA scavenging solution or ydrogen peroxide 50 cleaning system, also have a lot of shortcomings.Some reagent has severe corrosive, harmful to human safety; Ydrogen peroxide 50 very easily decomposes, and processing parameter should not be controlled; The cleaning operation step is many, consumes a large amount of chemical reagent and pure water, has promoted production cost; There is irritating smell in some reagent, has increased the maintenance cost of clean room.At present; The problem that scavenging solution mainly exists be after cleaning the silicon chip blackout, have that phenomenons such as piebald, color and luster be inconsistent, the major cause that produces these phenomenons are that silicon chip film source ginseng is time uneven, factors such as the reagent type in the scavenging solution, content proportioning, temperature control cause.Therefore,, solve the problems referred to above, will have great importance if can mix the silicon chip cleaning liquid of a kind of " fool " formula.
Summary of the invention
The present invention is directed to the defective that prior art exists, a kind of fine-hair maring using monocrystalline silicon slice preceding pre-washing agent and method of use of being used for is provided, can reach excellent making herbs into wool effect, effectively reduce the probability of finger-marks, the generation of hickie sheet.
For this reason; The present invention takes following technical scheme; A kind of pre-washing agent that is used for before the silicon single crystal making herbs into wool; It is characterized in that comprising following component: the water of TX10, mineral alkali and its esters, Trisodium Citrate, paratoluenesulfonic acid sodium salt, solubility promoter and surplus, described water is preferably deionized water.
Described TX10 is a kind of in polyoxyethylene octylphenol ether, the polyoxyethylene nonylphenol or two kinds; Mineral alkali is a sodium hydroxide; Its esters is a kind of in yellow soda ash or the water glass or two kinds, and described solubility promoter is a kind of or its mixture in diethylene glycol dimethyl ether, the diethyl ether.
A preferred embodiment of the present invention, wherein the weight ratio of TX10 and water is 0.5-2.5%, preferred mass is than being 1-2%; The mass ratio of paratoluenesulfonic acid sodium salt and water is 0.5-2%, and preferred mass is than being 0.8-1.5%; The weight ratio of mineral alkali and water is 0.1-1%, and preferred mass is than being 0.2-0.8%, and the mass ratio of its esters and water is 0.1-0.6%, and preferred mass is than being 0.2-0.5%; The mass ratio of Trisodium Citrate and water is 0.5-1.5%, and preferred mass is than being 0.5-1%; The volume ratio of solubility promoter Diethylene Glycol ethers and water is 1-8%, and preferred volume ratio is 1.5-6%.
The present invention is used for monocrystalline silicon surface, and to clean the preparation method of pre-washing agent of usefulness following:
(1) is that the sodium hydroxide of 0.1-1% and the sodium salt of 0.1-0.6% are dissolved in the deionized water with weight percentage, obtains alkali solution;
(2) be that the TX10 of 0.5-2.5%, the paratoluenesulfonic acid sodium salt of 0.5-2%, the Trisodium Citrate of 0.5-1.5% are dissolved in the deionized water with weight percentage; Alkali solution in wherein slowly adding step (1), volumn concentration are solubility promoter and the remaining deionized water of 1-8% again, make 1L pre-washing agent.
As preferably, above-mentioned sodium hydroxide, sodium salt, TX10, paratoluenesulfonic acid sodium salt, Trisodium Citrate, solubility promoter shared weight percentage in the pre-washing agent is respectively 0.2-0.8%, 0.2-0.5%, 1-2%, 0.8-1.5%, 0.5-1%, 1.5-6%.
The present invention also provides the method for use of the preceding pre-washing agent of a kind of silicon single crystal making herbs into wool; The pre-washing agent that configures is added in the de-ionized tank; According to volume ratio is dilution in 1: 50, silicon single crystal is immersed in the scavenging solution after the dilution cleans then, during cleaning; Temperature is 50-60 ℃, and the ultrasonic cleaning time is 180-300s.
After adopting monocrystalline silicon piece after this clean-out system cleans to carry out silicon chip surface making herbs into wool, the pyramid size that forms at silicon chip surface is less than 5 μ m, the whole complexion of silicon chip pool evenly, cashmere output rate is high, contaminations such as no finger-marks piebald, integrated reflectivity is lower than 12%.Before solar cell is carried out making herbs into wool with monocrystalline silicon piece, use clean-out system of the present invention to carry out pre-washing in advance,
The invention has the advantages that: after adopting this clean-out system and method for use; With do not compare through what clean-out system cleaned, can reduce silicon chip surface finger-marks, piebald etc. and stain the probability that occurs, the making herbs into wool effect obviously improves; The silicon chip yield rate further rises, and improves the production efficiency of enterprise.In addition, catalyzer nontoxicity of the present invention, non-corrosiveness, nonirritant does not have burning and explosion hazard, and human body and environment are not had harm; And the configuration of catalyzer and use technology are simple, cheap device, good reproducibility.
Description of drawings
Fig. 1 is the ESEM plat that does not pass through the silicon chip surface matte of prewashed making herbs into wool.
Fig. 2 is the ESEM plat through the silicon chip surface matte of making herbs into wool after the pre-washing.
Fig. 3 is the reflection spectrum through the silicon chip surface matte of making herbs into wool after the pre-washing.
Embodiment
Embodiment 1
Take following process step: 1) preparation alkali solution: with the 40ml deionized water is solvent, and 0.4g sodium hydroxide, 0.3g water glass are dissolved in the deionized water; 2) be solvent with the 40ml deionized water, 0.6g Trisodium Citrate, 1g paratoluenesulfonic acid sodium salt and 1.6g polyoxyethylene octylphenol ether are dissolved in the deionized water; 3) diethylene glycol dimethyl ether and the remaining 17ml deionized water with alkali solution, 3ml slowly joins step 2) in the solution, make 100ml pre-washing agent; 4) 100ml pre-washing agent being added in the de-ionized tank, is dilution in 1: 50 according to volume ratio, silicon single crystal is immersed in the scavenging solution after the dilution cleans then, and temperature is 55 ℃, and scavenging period is 250s.Solar silicon wafers after cleaning is carried out making herbs into wool according to the technology of the general making herbs into wool of photovoltaic industry, obtain the making herbs into wool silicon chip, contrast matte effect.
Fig. 2 has provided the ESEM plat through the silicon chip surface matte of making herbs into wool after the pre-washing, compares with the matte figure without prewashed making herbs into wool among Fig. 1, and the pyramid size of the formation after silicon chip cleans is more even, is approximately 1-5 μ m, and cashmere output rate is higher.Fig. 3 has provided the reflection spectrum of the silicon chip surface matte that obtains through making herbs into wool after the pre-washing, from figure, can see that the reflectivity of the silicon chip surface matte that the present invention obtains is lower, and integrated reflectivity is lower than 12%.
Embodiment 2
Take following process step: 1) preparation alkali solution: with the 40ml deionized water is solvent, and 0.5g sodium hydroxide, 0.4g water glass are dissolved in the deionized water; 2) be solvent with the 40ml deionized water, 0.7g Trisodium Citrate, 1.1g paratoluenesulfonic acid sodium salt, 1g polyoxyethylene octylphenol ether and 0.5g polyoxyethylene nonylphenol are dissolved in the deionized water; 3) diethylene glycol dimethyl ether and the remaining 16ml deionized water with alkali solution, 4ml slowly joins step 2) in the solution, make 100ml pre-washing agent; 4) 100ml pre-washing agent being added in the de-ionized tank, is dilution in 1: 50 according to volume ratio, silicon single crystal is immersed in the scavenging solution after the dilution cleans then, and temperature is 50 ℃, and scavenging period is 300s.
Embodiment 3
Take following process step: 1) preparation alkali solution: with the 40ml deionized water is solvent, and 0.4g sodium hydroxide, 0.3g yellow soda ash are dissolved in the deionized water; 2) be solvent with the 40ml deionized water, 0.8g Trisodium Citrate, 1.2g paratoluenesulfonic acid sodium salt and 1.8g polyoxyethylene octylphenol ether are dissolved in the deionized water; 3) diethylene glycol dimethyl ether and the remaining 15ml deionized water with alkali solution, 5ml slowly joins step 2) in the solution, make 100ml pre-washing agent; 4) 100ml pre-washing agent being added in the de-ionized tank, is dilution in 1: 50 according to volume ratio, silicon single crystal is immersed in the scavenging solution after the dilution cleans then, and temperature is 60 ℃, and scavenging period is 180s.
Claims (6)
1. one kind is used for the preceding pre-washing agent of fine-hair maring using monocrystalline silicon slice, and it is characterized in that comprising following component: the water of TX10, mineral alkali and its esters, Trisodium Citrate, paratoluenesulfonic acid sodium salt, solubility promoter and surplus, described water is preferably deionized water.
2. the pre-washing agent that is used for before the fine-hair maring using monocrystalline silicon slice according to claim 1; It is characterized in that described TX10 is a kind of in polyoxyethylene octylphenol ether, the polyoxyethylene nonylphenol or two kinds; Mineral alkali is a sodium hydroxide; Its esters is a kind of in yellow soda ash or the water glass or two kinds, and described solubility promoter is a kind of or its mixture in diethylene glycol dimethyl ether, the diethyl ether.
3. the pre-washing agent that is used for before the fine-hair maring using monocrystalline silicon slice according to claim 1 and 2, the weight ratio that it is characterized in that described TX10 and water is 0.5-2.5%, preferred mass is than being 1-2%; The mass ratio of paratoluenesulfonic acid sodium salt and water is 0.5-2%, and preferred mass is than being 0.8-1.5%; The weight ratio of mineral alkali and water is 0.1-1%, and preferred mass is than being 0.2-0.8%, and the mass ratio of its esters and water is 0.1-0.6%, and preferred mass is than being 0.2-0.5%; The mass ratio of Trisodium Citrate and water is 0.5-1.5%, and preferred mass is than being 0.5-1%; The volume ratio of solubility promoter Diethylene Glycol ethers and water is 1-8%, and preferred volume ratio is 1.5-6%.
4. compound method that is used for the pre-washing agent before the silicon single crystal making herbs into wool is characterized in that comprising following preparation process:
(1) is that the sodium hydroxide of 0.1-1% and the sodium salt of 0.1-0.6% are dissolved in the deionized water with weight percentage, obtains alkali solution;
(2) be that the TX10 of 0.5-2.5%, the paratoluenesulfonic acid sodium salt of 0.5-2%, the Trisodium Citrate of 0.5-1.5% are dissolved in the deionized water with weight percentage; Alkali solution in wherein slowly adding step (1), volumn concentration are solubility promoter and the remaining deionized water of 1-8% again, make 1L pre-washing agent.
5. the compound method that is used for the preceding pre-washing agent of silicon single crystal making herbs into wool according to claim 4 is characterized in that described sodium hydroxide, sodium salt, TX10, paratoluenesulfonic acid sodium salt, Trisodium Citrate, solubility promoter shared weight percentage in the pre-washing agent is respectively 0.2-0.8%, 0.2-0.5%, 1-2%, 0.8-1.5%, 0.5-1%, 1.5-6%.
6. the method for use of pre-washing agent before the silicon single crystal making herbs into wool; It is characterized in that the pre-washing agent of configuration in claim 4 or 5 is joined earlier in the ion tank; According to volume ratio is dilution in 1: 50, silicon single crystal is immersed in the pre-washing agent cleans again, during cleaning; Temperature is 50-60 ℃, and scavenging period is 180-300s.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102888656A (en) * | 2012-09-28 | 2013-01-23 | 绍兴拓邦电子科技有限公司 | High-boiling point monocrystalline silicon wafer surface texturing additive and using method thereof |
CN106521636A (en) * | 2016-12-30 | 2017-03-22 | 德清丽晶能源科技有限公司 | Single crystal wafer texturing additive |
CN106835288A (en) * | 2016-12-30 | 2017-06-13 | 德清丽晶能源科技有限公司 | A kind of etching method of monocrystalline silicon piece |
CN108690747A (en) * | 2018-06-25 | 2018-10-23 | 安徽全兆光学科技有限公司 | A kind of photovoltaic chip detergent |
CN113980747A (en) * | 2021-11-10 | 2022-01-28 | 重庆臻宝实业有限公司 | Cleaning agent for semiconductor material surface degreasing treatment |
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CN101892132A (en) * | 2010-07-23 | 2010-11-24 | 北京工业大学 | Solar silicon slice cleaning agent and method for preparing same |
CN102304444A (en) * | 2011-08-01 | 2012-01-04 | 合肥华清金属表面处理有限责任公司 | Environmental-protection water-base cleaning agent for solar-grade silicon wafers |
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2012
- 2012-04-01 CN CN2012100981624A patent/CN102644084A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101892132A (en) * | 2010-07-23 | 2010-11-24 | 北京工业大学 | Solar silicon slice cleaning agent and method for preparing same |
CN102304444A (en) * | 2011-08-01 | 2012-01-04 | 合肥华清金属表面处理有限责任公司 | Environmental-protection water-base cleaning agent for solar-grade silicon wafers |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102888656A (en) * | 2012-09-28 | 2013-01-23 | 绍兴拓邦电子科技有限公司 | High-boiling point monocrystalline silicon wafer surface texturing additive and using method thereof |
CN102888656B (en) * | 2012-09-28 | 2015-04-08 | 绍兴拓邦电子科技有限公司 | High-boiling point monocrystalline silicon wafer surface texturing additive and using method thereof |
CN106521636A (en) * | 2016-12-30 | 2017-03-22 | 德清丽晶能源科技有限公司 | Single crystal wafer texturing additive |
CN106835288A (en) * | 2016-12-30 | 2017-06-13 | 德清丽晶能源科技有限公司 | A kind of etching method of monocrystalline silicon piece |
CN108690747A (en) * | 2018-06-25 | 2018-10-23 | 安徽全兆光学科技有限公司 | A kind of photovoltaic chip detergent |
CN113980747A (en) * | 2021-11-10 | 2022-01-28 | 重庆臻宝实业有限公司 | Cleaning agent for semiconductor material surface degreasing treatment |
CN113980747B (en) * | 2021-11-10 | 2023-08-25 | 重庆臻宝科技股份有限公司 | Cleaning agent for degreasing treatment of semiconductor material surface |
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Application publication date: 20120822 |