CN115216301B - Texturing solution for monocrystalline silicon and texturing method - Google Patents
Texturing solution for monocrystalline silicon and texturing method Download PDFInfo
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- CN115216301B CN115216301B CN202210725214.XA CN202210725214A CN115216301B CN 115216301 B CN115216301 B CN 115216301B CN 202210725214 A CN202210725214 A CN 202210725214A CN 115216301 B CN115216301 B CN 115216301B
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 131
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 50
- 239000002904 solvent Substances 0.000 claims abstract description 46
- 230000005496 eutectics Effects 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000654 additive Substances 0.000 claims abstract description 28
- 239000000126 substance Substances 0.000 claims abstract description 17
- 210000002268 wool Anatomy 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000013530 defoamer Substances 0.000 claims description 25
- 230000000996 additive effect Effects 0.000 claims description 22
- -1 (2-hydroxyethyl) acetyl trimethylammonium chloride Chemical compound 0.000 claims description 17
- 229920002873 Polyethylenimine Polymers 0.000 claims description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 10
- 229920000570 polyether Polymers 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- KIZQNNOULOCVDM-UHFFFAOYSA-M 2-hydroxyethyl(trimethyl)azanium;hydroxide Chemical compound [OH-].C[N+](C)(C)CCO KIZQNNOULOCVDM-UHFFFAOYSA-M 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- VYWQTJWGWLKBQA-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;chloride Chemical compound Cl.NC(N)=O VYWQTJWGWLKBQA-UHFFFAOYSA-N 0.000 claims description 6
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims description 6
- 229960001231 choline Drugs 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- UMESNHVJZFCGBV-UHFFFAOYSA-N 2-methyl-4-[(2-methylphenyl)methylidene]-1,3-oxazol-5-one Chemical compound O=C1OC(C)=NC1=CC1=CC=CC=C1C UMESNHVJZFCGBV-UHFFFAOYSA-N 0.000 claims description 5
- 239000000872 buffer Substances 0.000 claims description 5
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 5
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical group C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- 229920000180 alkyd Polymers 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000002952 polymeric resin Substances 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 235000011088 sodium lactate Nutrition 0.000 claims description 4
- 239000001540 sodium lactate Substances 0.000 claims description 4
- 229940005581 sodium lactate Drugs 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- PIIRYSWVJSPXMW-UHFFFAOYSA-N 1-octyl-4-(4-octylphenoxy)benzene Chemical compound C1=CC(CCCCCCCC)=CC=C1OC1=CC=C(CCCCCCCC)C=C1 PIIRYSWVJSPXMW-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000013504 Triton X-100 Substances 0.000 claims description 2
- 229920004890 Triton X-100 Polymers 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 229920003169 water-soluble polymer Polymers 0.000 claims description 2
- 239000004973 liquid crystal related substance Substances 0.000 claims 2
- 150000007529 inorganic bases Chemical class 0.000 claims 1
- 150000007530 organic bases Chemical class 0.000 claims 1
- 235000012431 wafers Nutrition 0.000 abstract description 56
- 238000002310 reflectometry Methods 0.000 abstract description 14
- 238000004140 cleaning Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 36
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 15
- 230000008569 process Effects 0.000 description 11
- 230000007797 corrosion Effects 0.000 description 10
- 238000005260 corrosion Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000006260 foam Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 125000000879 imine group Chemical group 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- 241001122767 Theaceae Species 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
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- 238000013112 stability test Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/02—Etching, surface-brightening or pickling compositions containing an alkali metal hydroxide
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02363—Special surface textures of the semiconductor body itself, e.g. textured active layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic System
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a texturing solution and a texturing method for monocrystalline silicon, and belongs to the technical field of monocrystalline silicon texturing solutions. The wool making liquid consists of the following components in percentage by mass: 1-3% of alkaline substances, 0.3-2.5% of texturing additives, 5-30% of eutectic solvents and the balance of water. The texturing solution can be used for texturing monocrystalline silicon wafers of any size. The invention also discloses a texturing method for monocrystalline silicon, which comprises the steps of firstly placing monocrystalline silicon into self-made pretreatment liquid for cleaning, then placing into the texturing liquid for texturing, wherein the texturing temperature is 50-85 ℃, and the texturing time is 80-250s. The invention solves the problems of long texturing time, nonuniform texturing surface, short service life of the texturing solution, and has the advantages of good stability of the texturing solution, low reflectivity of the monocrystalline silicon wafer after texturing and the like.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon texturing solution, and relates to a texturing solution for monocrystalline silicon and a texturing method.
Background
Currently, in the photovoltaic field, monocrystalline silicon solar cells are receiving a great deal of attention because of their high conversion efficiency. In the production process of the monocrystalline silicon solar cell, in order to reduce the reflection of light, increase the absorption of sunlight and improve the photoelectric conversion efficiency of the monocrystalline silicon solar cell, the surface of the monocrystalline silicon needs to be textured, i.e. a suede structure is formed on the surface of the monocrystalline silicon by adopting a method, so that the incident light is reflected on the suede of the monocrystalline silicon for multiple times,the optical path is lengthened, thereby increasing the absorption of light. The common texturing method for the monocrystalline silicon surface comprises the following steps: wet alkali etching, dry etching, laser or mechanical engraving and the like, wherein the wet alkali etching is widely used due to the advantages of low cost, high efficiency, convenient operation and the like. In wet lye etching technology, the principle of reaction of monocrystalline silicon with lye (lye is usually aqueous solution of KOH or NaOH) is: si+2OH - +H 2 O＝SiO 3 2- +2H 2 And ∈c, based on the corrosion rate difference of alkali liquor on each crystal face of monocrystalline silicon, specifically: the (100) surface of the monocrystalline silicon wafer is easier to be corroded by alkali liquor than the (111) surface or the (110) surface of the monocrystalline silicon wafer, and the (111) surface of the monocrystalline silicon wafer has an inclination angle of about 54 degrees relative to the (100) surface of the monocrystalline silicon wafer, so that after the alkali liquor etching is finished, a texture structure similar to a pyramid shape formed by the (111) surface and the equivalent surface of the (111) surface is finally formed on the surface of the monocrystalline silicon wafer, and compared with a planar structure, the texture structure can effectively enhance the absorption of the silicon wafer to incident light and improve the photo-generated current density.
Various factors influence the size and density of the pyramid structure on the surface of the monocrystalline silicon, such as the concentration of alkali liquor, the composition of the texturing solution, the types and contents of components of the texturing additive, the texturing temperature and the like. The mass ratio of the texturing additive to the alkali liquor in the invention patent CN201610738890.5 is 0.2-5:100, but when the concentration of the alkali liquor is too high, the corrosion to the monocrystalline silicon wafer is too strong, the formed textured surface is poor, the effect similar to polishing is generated, and even the phenomenon of collapse of the textured structure of the monocrystalline silicon wafer can occur. Therefore, it is necessary to add additives to the texturing agent to adjust the OH in the texturing agent - The etching rate of the monocrystalline silicon surface, i.e. the size and density of the pyramids are adjusted from the level of the texturing additive.
The monocrystalline silicon piece prepared by the texturing agent in the prior art has the problems of small and uncontrollable textured size, low texturing rate, high reflectivity, large alkali liquor consumption in the texturing solvent, long texturing time, high texturing temperature and the like. The single crystal silicon texturing process generally uses a KOH (or NaOH) aqueous solution with the mass concentration of 10-25% and isopropanol as texturing solution, the texturing temperature is 75-90 ℃, and the texturing time is 15-30min. Isopropyl alcohol is used for reducing solution surface tension and regulating corrosion reactionGenerated H 2 The rapid separation function, however, the monocrystalline silicon texturing process has the defects of long reaction time, regular pyramid textured structure formed on the surface of the monocrystalline silicon, greatly reduced production efficiency, high reflectivity of the obtained monocrystalline silicon textured structure, easy volatilization of isopropanol in the texturing liquid, large consumption, environmental protection and the like. Therefore, development of alcohol-free texturing additives tends to be carried out, but the defects are that the texturing time is long and the consumption of alkali liquor is large, for example, patent CN201210330618.5 discloses an additive of monocrystalline silicon wafer alkaline environment-friendly alcohol-free texturing liquid, which comprises 0.05-1wt.% of protein, 0.01-1wt.% of detergent, 0.001-0.003wt.% of one or combination of vitamins, donkey-hide gelatin and tea polyphenol and the balance of water, and although compared with the additive, the additive is not added, the texturing temperature is reduced, volatile isopropanol is not used, the texturing time is shortened, the texturing effect is improved, but the texturing time is longer (700-1500 s), and the problems of relatively higher alkali consumption and poor stability of the texturing liquid caused by excessive corrosion and weight reduction are also caused.
Therefore, it is necessary to provide a texturing solution and a texturing method for monocrystalline silicon, which are used for solving the problems of low texturing rate, long texturing time and non-uniform texturing of monocrystalline silicon.
Disclosure of Invention
In order to solve the problems in the prior art, one of the purposes of the invention is to innovatively provide a texturing solution for monocrystalline silicon, the texturing solution is used for texturing on the surface of monocrystalline silicon, the texturing time is short, the reflectivity of the textured surface is low (11%), the textured surface is uniform, and the problem of poor stability of the texturing solution can be solved.
The aim of the invention is achieved by the following technical scheme:
the wool making liquid for monocrystalline silicon consists of the following components in percentage by mass:
1-3% of alkaline substances, 0.3-2.5% of texturing additives, 5-30% of eutectic solvents and the balance of deionized water.
Preferably, the mass percentage of the eutectic solvent in the texturing solution is 15-28%, and the preparation method of the eutectic solvent comprises the following steps:
drying (2-hydroxyethyl) trimethyl ammonium hydroxide and urea in a vacuum drying oven at 60 ℃ for 12h respectively according to the mass ratio of n (2-hydroxyethyl) trimethylammonium hydroxide :n Urea Mixing and stirring the materials in a ratio of (1:2), sealing, and heating the materials in an oil bath at the temperature of 70-80 ℃ until colorless transparent liquid is obtained, thus obtaining the choline chloride-urea eutectic solvent;
the other conditions are kept unchanged, the raw material types are only changed, and other substances which can replace (2-hydroxyethyl) -trimethyl ammonium chloride can be n-octyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride or (2-hydroxyethyl) acetyl trimethyl ammonium chloride, and the substances are sequentially mixed with urea to prepare n-octyl trimethyl ammonium chloride-urea eutectic solvent (B), dodecyl trimethyl ammonium chloride-urea eutectic solvent (C) and (2-hydroxyethyl) acetyl trimethyl ammonium chloride-urea eutectic solvent (D); the reagent purities were 99wt.%, all purchased from national pharmaceutical group chemical reagent production company.
It should be noted that the eutectic solvent refers to a binary or ternary eutectic mixture formed by combining a hydrogen bond donor and a hydrogen bond acceptor through hydrogen bond interaction, and has the advantages of low melting point, low vapor pressure, low cost, biodegradability, high stability and the like. Although the eutectic solvent is widely applied, the eutectic solvent is still the first example in the invention for monocrystalline silicon slice texturing, the eutectic solvent prepared by the invention has low steam pressure and is not easy to volatilize, the stability of the texturing liquid can be kept without continuous replenishment in the texturing process, and compared with the volatile isopropanol, the alkali liquid consumption can be greatly reduced; the eutectic solvent has a medium-length hydrocarbon chain structure and polar functional groups such as hydroxyl, acyl, ester, amino and the like, and can reduce the surface tension of the texturing liquid by at least about 30 percent (compared with the surface tension of water of 72 mN/m) under the condition of no surfactant addition, thereby overcoming the defect that the use of various surfactants in the prior art increases the cleaning difficulty in the post-texturing treatment step, reducing the surface tension and the interaction between the polar functional groups in the eutectic solvent and Si-H bonds on the surface of monocrystalline silicon, facilitating the adsorption of the texturing liquid on the surface of monocrystalline silicon, and preparing more uniform textured surfaces.
Preferably, the alkaline substance comprises inorganic alkali and organic alkali, wherein the inorganic alkali is sodium hydroxide or potassium hydroxide, and the inorganic alkali accounts for 1-2% of the mass of the texturing solution;
the organic alkali is polyethyleneimine, and the mass percentage of the organic alkali in the texturing solution is 0.5-1%.
Compared with inorganic alkali, the organic alkali substance has low corrosiveness to the monocrystalline silicon piece, and the polyethyleneimine exists in the form of polymeric cations in water, can chelate heavy metal ions, and can remove pollution of heavy metal ions possibly mixed in the texturing process to the monocrystalline silicon piece.
Preferably, the components of the texturing additive are as follows by mass percent: 0.1 to 0.5 percent of water-soluble polymer resin, 0.1 to 1 percent of defoamer and 0.01 to 0.1 percent of buffer;
the water-soluble high polymer resin is water-soluble alkyd resin or water-soluble acrylic resin, the defoamer is polyether defoamer or organosilicon defoamer, and the buffer is sodium lactate or sodium bicarbonate.
The organic silicon defoamer comprises an organic silicon defoamer FAG-470, an organic silicon defoamer BYK-065, an organic silicon defoamer BYK-066N or a polysiloxane defoamer YCK-615, wherein the effect of the defoamer is to reduce foam in the mixing and stirring process when the wool making liquid is prepared, and the defoamer can be contacted with monocrystalline silicon more uniformly so as to obtain a more uniform suede structure;
and the hydrolysis reaction of the buffer agent in the water is reversible, and can be dynamically adjusted according to the concentration change of hydroxide ions in the texturing liquid, so that the corrosion rate of the hydroxide ions to the monocrystalline silicon wafer in the texturing process is adjusted, and uniform textured surfaces are obtained.
Preferably, the rest of the texturing solution is water, and the water is deionized water.
Another object of the present invention is to provide a method for texturing monocrystalline silicon, wherein the monocrystalline silicon is textured by using the texturing solution, and the method comprises the following specific steps:
(1) Dissolving alkaline substances in water to prepare alkali liquor with certain mass concentration for standby, and then uniformly mixing the texturing additive, the eutectic solvent and the water with the alkaline substances in the alkali liquor according to the mass ratio;
(2) Placing the monocrystalline silicon wafer into self-made pretreatment liquid for soaking treatment, and then performing ultrasonic treatment and cleaning for later use;
(3) Immersing the pretreated monocrystalline silicon piece into the texturing solution prepared in the step (1) for surface texturing, and sequentially washing the textured monocrystalline silicon piece with water and absolute ethyl alcohol for three times to obtain the textured monocrystalline silicon piece.
Preferably, in the step (2), the pretreatment liquid comprises the following components in percentage by mass: 1-5% of sodium silicate, 0.5-2% of triton X-100 (polyethylene glycol monooctylphenyl ether), 0.5-2% of OP-101-3% of sodium tripolyphosphate, 1-3% of polyether defoamer GP-3301 and the balance of water.
And the pretreatment temperature is 50-60 ℃, the ultrasonic power is 60-100W, the ultrasonic time is 5-10min, and the cleaning is carried out by absolute ethyl alcohol.
Preferably, the texturing temperature in the step (3) is 50-85 ℃, and the texturing time is 80-250s.
Further preferably, the pretreatment temperature is 50 ℃, the texturing temperature is 55-80 ℃, the texturing time is 100-200s, and the textured monocrystalline silicon wafer is obtained by washing the monocrystalline silicon wafer with water and absolute ethyl alcohol for three times in sequence.
In addition, the mechanism of the monocrystalline silicon texturing reaction is as follows:
1. hydroxide ion OH - Diffusing to the surface of the silicon wafer; 2. adsorption of OH by silicon wafer - And other substances; 3. oxidation of silicon occurs; 4. desorbing the product from the surface of the silicon wafer; 5. the product diffuses into the solution, hydroxyl in the high-concentration alkali liquor directly acts on the surface of the monocrystalline silicon wafer, and as the etching speed is too high, a uniform suede structure cannot be obtained, if the product on the surface of the silicon wafer after etching is not timely dropped off, the etching sites on the surface of the monocrystalline silicon wafer are covered by the product, and the suede structure can be also causedNon-uniformity.
Based on the above, the invention discloses the wool making liquid and the wool making method for monocrystalline silicon, which have the following advantages compared with the prior art:
(1) The eutectic solvent disclosed by the invention can slowly release OH under alkaline heating condition - The etching (corrosion) rate is regulated, and monocrystalline silicon slice etching can be carried out even under the condition of small alkali liquor consumption, so that the cost is greatly saved; and the monocrystalline silicon slice is textured by combining inorganic alkali and organic alkali, the organic alkali has low corrosion to the monocrystalline silicon slice, and the texture liquid can gently texture the monocrystalline silicon, so that the texture surface prepared is more uniform, and the reflectivity is lower than 11%.
(2) Compared with the volatile isopropanol, the eutectic solvent disclosed by the invention has the advantages that the vapor pressure is low, the volatile isopropanol is not easy to volatilize, the stability of the texturing solution can be kept without being continuously supplemented in the texturing process, the alkali solution consumption can be greatly reduced, and the problem of short service life of the texturing solution is effectively solved; the eutectic solvent has a medium-length hydrocarbon chain structure and rich polar functional groups such as hydroxyl, acyl, ester, amino and the like, and can reduce the surface tension of the texturing liquid under the condition of not adding a surfactant, so that the problems that various surfactants are used in the prior art to increase the cleaning difficulty in the post-texturing treatment step are solved, the surface tension is reduced, and the polar functional groups in the eutectic solvent interact with Si-H bonds on the surface of monocrystalline silicon, so that the texturing liquid is convenient to adsorb on the surface of monocrystalline silicon wafers, and more uniform textured surfaces are prepared.
(3) The polyethyleneimine exists in water in the form of polymeric cations, can chelate heavy metal ions, eliminates pollution of heavy metal ions possibly mixed in the texturing process to monocrystalline silicon wafers, can adsorb active imine groups in the polyethyleneimine on the surfaces of the monocrystalline silicon, regulates uniform corrosion of hydroxyl ions to the monocrystalline silicon wafers during texturing, and has a long-chain structure which can promote desorption of products on the surfaces of the monocrystalline silicon wafers.
(4) The single crystal silicon of the invention has short texturing time, and the texturing process can be completed within 100-200s, thereby effectively solving the problem of long texturing time (15-30 min) of the single crystal silicon.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention discloses a texturing solution and a texturing method for monocrystalline silicon, which are used for solving the problems of low texturing rate, long texturing time, nonuniform texturing surface and short service life of the texturing solution of monocrystalline silicon.
To further illustrate the superior effect of the present application over the prior art, the inventors performed the following tests:
the reflectivity testing method comprises the following steps: the reflectivity test was performed on the textured sheets obtained in examples 1 to 4 and comparative example 1 above, the reflectivity test apparatus used an NXT Helios-rc reflectivity test apparatus, and the reflectivity obtained by the front and back side tests of the silicon wafer were averaged as average reflectivity.
The stability test method comprises the following steps: the single crystal silicon wool making liquid samples in examples 1-4 were placed at 25+ -1deg.C, and the presence or absence of delamination and the presence or absence of significant precipitates were observed.
Foam performance test of the texturing additive: the foam performance of the texturing additive is tested by adopting a vibration method, 15mL of the texturing agent in the examples and the comparative examples is placed in a measuring cylinder with a plug, the vibration is stopped after 40s, the measuring cylinder with the plug is placed on an experiment table, the foam height is recorded and timing is started, and the foam height is recorded at the same time until the foam completely disappears. The smaller the foam volume, the more uniform the texture-making additive can be in contact with the monocrystalline silicon, thereby obtaining uniform textured monocrystalline silicon.
The morphology testing method comprises the following steps: and observing the morphology of the prepared textured monocrystalline silicon sample by adopting a TM 3000 scanning electron microscope. The textured monocrystalline silicon wafers prepared in examples 1-4 were observed to be textured uniformly.
Surface tension test method: monocrystalline silicon wafers were subjected to the texturing process according to examples 1-4 and comparative example 1 using a K100 fully automatic surface tensiometer (KRUSS, germany), the surface tension of the texturing solution was measured at different setting times (by sampling at different times), the test temperature was controlled at 25.+ -. 1 ℃, all samples were cooled and set for 30min before testing, the measurement was repeated three times, and the average value was recorded in units of mN/m.
The invention is further illustrated, but is not limited, by the following examples.
Example 1
Preparation of the eutectic solvent: drying (2-hydroxyethyl) trimethyl ammonium hydroxide and urea in a vacuum drying oven at 60 ℃ for 12h respectively according to the mass ratio of n (2-hydroxyethyl) trimethylammonium hydroxide :n Urea Mixing and stirring =1:2, sealing, and then heating in an oil bath at 75 ℃ until a colorless transparent liquid, i.e. choline chloride-urea eutectic solvent, is obtained.
The texture-making additive is prepared from water-soluble alkyd resin: polyether defoamer GP-330: sodium lactate=0.5%: 0.8%:0.07% of the total weight of the composition.
The single crystal silicon is textured as follows:
(1) Preparing a wool making liquid: dissolving sodium hydroxide and polyethylenimine in water to prepare alkali liquor, and mixing alkaline substances in the alkali liquor with the texturing additive, the eutectic solvent and water according to the mass percentage of 3.0 percent: 2.5%:26%: mixing evenly at a mass ratio of sodium hydroxide to polyethyleneimine of 2:1 in alkali liquor;
(2) After soaking monocrystalline silicon wafers in self-made pretreatment liquid, carrying out ultrasonic treatment and cleaning, wherein the pretreatment temperature is 55 ℃, the ultrasonic power is 100W, the ultrasonic time is 10min, and the monocrystalline silicon wafers are cleaned by absolute ethyl alcohol, and the pretreatment liquid comprises the following components in percentage by mass: 5% of sodium silicate, 5% of triton X-1001.5%, 101.5% of OP-101, 2% of sodium tripolyphosphate, 2% of polyether defoamer GP-3303% and the balance of water;
(3) Immersing the pretreated monocrystalline silicon wafer into the texturing solution prepared in the step (1) for surface texturing, wherein the texturing temperature is 75 ℃, the texturing time is 95s, and the textured monocrystalline silicon wafer is obtained by washing the monocrystalline silicon wafer with water and washing the monocrystalline silicon wafer with absolute ethyl alcohol three times in sequence.
Example 2
Preparation of the eutectic solvent: drying n-octyl trimethyl ammonium chloride and urea in vacuum drying oven at 60deg.C for 12 hr to obtain n-type solution N-octyl trimethyl ammonium chloride :n Urea Mixing and stirring =1:2, sealing, and then heating in an oil bath at 80 ℃ until a colorless transparent liquid, i.e. choline chloride-urea eutectic solvent, is obtained.
The texture-making additive is prepared from water-soluble acrylic resin: silicone defoamer FAG-470: sodium lactate=0.4%: 0.9%:0.05% of the total weight of the composition.
The single crystal silicon is textured as follows:
(1) Preparing a wool making liquid: dissolving sodium hydroxide and polyethylenimine in water to prepare alkali liquor, and mixing alkaline substances in the alkali liquor with the texturing additive, the eutectic solvent and water according to the mass percentage of 2.5 percent: 2%:28%:67.5% of the alkali solution is uniformly mixed, wherein the mass ratio of sodium hydroxide to polyethyleneimine in the alkali solution is 1.5:1.0;
(2) After soaking monocrystalline silicon wafers in self-made pretreatment liquid, carrying out ultrasonic treatment and cleaning, wherein the pretreatment temperature is 50 ℃, the ultrasonic power is 100W, the ultrasonic time is 8min, and the monocrystalline silicon wafers are cleaned by absolute ethyl alcohol, and the pretreatment liquid comprises the following components in percentage by mass: 4% of sodium silicate, 4% of triton X-1002%, 103% of OP-103%, 0.5% of sodium tripolyphosphate, 2% of polyether defoamer GP-3302% and the balance of water;
(3) Immersing the pretreated monocrystalline silicon wafer into the texturing solution prepared in the step (1) for surface texturing, wherein the texturing temperature is 70 ℃, the texturing time is 116s, and the textured monocrystalline silicon wafer is obtained by washing the monocrystalline silicon wafer with water and washing the monocrystalline silicon wafer with absolute ethyl alcohol three times in sequence.
Example 3
Preparation of the eutectic solvent: drying dodecyl trimethyl ammonium chloride and urea in vacuum drying oven at 60deg.C for 12 hr to obtain n Dodecyl trimethyl ammonium chloride :n Urea Mixing and stirring =1:2, sealing, and then heating in an oil bath at 72 ℃ until a colorless transparent liquid, i.e. choline chloride-urea eutectic solvent, is obtained.
The texture-making additive is prepared from water-soluble acrylic resin: polyether defoamer PPG-1000: sodium bicarbonate = 0.4%:0.7%:0.1% of the total weight of the composition.
The single crystal silicon is textured as follows:
(1) Preparing a wool making liquid: dissolving sodium hydroxide and polyethylenimine in water to prepare alkali liquor, and mixing alkaline substances in the alkali liquor with the texturing additive, the eutectic solvent and water according to the mass percentage of 2.0 percent: 2.5%:24%: mixing evenly with 71.5%, wherein the mass ratio of sodium hydroxide to polyethyleneimine in the alkali liquor is 1.2:0.8;
(2) After soaking monocrystalline silicon wafers in self-made pretreatment liquid, carrying out ultrasonic treatment and cleaning, wherein the pretreatment temperature is 50 ℃, the ultrasonic power is 60W, the ultrasonic time is 10min, and the monocrystalline silicon wafers are cleaned by absolute ethyl alcohol, and the pretreatment liquid comprises the following components in percentage by mass: 3% of sodium silicate, 3% of triton X-1002%, 1% of OP-101%, 1% of sodium tripolyphosphate, 2% of polyether defoamer GP-3302% and the balance of water;
(3) Immersing the pretreated monocrystalline silicon wafer into the texturing solution prepared in the step (1) for surface texturing, wherein the texturing temperature is 65 ℃, and the texturing time is 150s, so that the textured monocrystalline silicon wafer is obtained.
Example 4
Preparation of the eutectic solvent: drying (2-hydroxyethyl) acetyl trimethyl ammonium chloride and urea in vacuum drying oven at 60deg.C for 12 hr to obtain n (2-hydroxyethyl) acetyl trimethyl ammonium chloride :n Urea Mixing and stirring =1:2, sealing, and then heating in an oil bath at 70 ℃ until a colorless transparent liquid, i.e. choline chloride-urea eutectic solvent, is obtained.
The texture-making additive is prepared from water-soluble alkyd resin: polysiloxane defoamer YCK-615: sodium bicarbonate = 0.5%:0.4%:0.06% of the total weight of the composition.
The single crystal silicon is textured as follows:
(1) Preparing a wool making liquid: dissolving sodium hydroxide and polyethylenimine in water to prepare alkali liquor, and mixing alkaline substances in the alkali liquor, the wool making additive, the eutectic solvent and water according to the mass percentage of 1.5 percent: 2%:22%:74.5% of the alkali solution is uniformly mixed, wherein the mass ratio of sodium hydroxide to polyethyleneimine in the alkali solution is 1.0:0.5;
(2) After soaking monocrystalline silicon wafers in self-made pretreatment liquid, carrying out ultrasonic treatment and cleaning, wherein the pretreatment temperature is 55 ℃, the ultrasonic power is 100W, the ultrasonic time is 5min, and the monocrystalline silicon wafers are cleaned by absolute ethyl alcohol, and the pretreatment liquid comprises the following components in percentage by mass: 1% of sodium silicate, 1.5% of triton X-1001.5%, 101.5% of OP-101, 2% of sodium tripolyphosphate, 2% of polyether defoamer GP-3303% and the balance of water;
(3) Immersing the pretreated monocrystalline silicon wafer into the texturing solution prepared in the step (1) for surface texturing, wherein the texturing temperature is 55 ℃, the texturing time is 180s, and the textured monocrystalline silicon wafer is obtained by washing the monocrystalline silicon wafer with water and washing the monocrystalline silicon wafer with absolute ethyl alcohol three times in sequence.
In addition, in order to further explain the novelty of the technical scheme claimed in the application of the invention compared with the prior art, the inventor makes the following comparative experiments, and tests the prepared wool making liquid and the monocrystalline silicon wool face after wool making by using the wool making liquid, the specific contents are as follows:
comparative example 1
The difference from example 1 is that no eutectic solvent was added, and the other monocrystalline silicon pieces subjected to the texturing under the conditions kept unchanged in example 1 were subjected to water washing and absolute ethyl alcohol washing three times in sequence to obtain textured monocrystalline silicon pieces.
Table 1 comparison of the properties of examples 1-4 and comparative example 1
As can be seen from table 1, the comparison between example 1 and comparative example 1 shows that the single crystal silicon texture obtained by adding the eutectic solvent has lower reflectivity, lower surface tension, better stability of the texture-making liquid, better uniformity of the single crystal silicon texture obtained in example 1, and more uniform size and density of texture pyramids observed under an electron microscope, because the addition of the eutectic solvent reduces the surface tension of the texture-making liquid and the interaction between the polar functional groups in the eutectic solvent and Si-H bonds on the surface of the single crystal silicon, the texture-making liquid is easier to adsorb on the surface of the single crystal silicon wafer, so that a more uniform texture is obtained, the stability of the texture-making liquid in comparative example 1 is slightly poor, delamination occurs after 45 days, and sediment is generated, which indicates that van der waals interactions between various functional groups in the eutectic solvent and other additives may play a role in stabilizing.
Compared with the single crystal silicon suede prepared in the examples 1, 3 and 4, the reflectivity of the suede is slightly lower, when the initial volume of 13mL is reduced to 2.0mL and the volume of 5s foam is reduced to 0mL in 3s of the air bubble of the suede additive, the increase of the addition amount of the eutectic solvent can well reduce the surface tension of the suede solution, the surface tension of the suede solution is favorable for removing foam, the surface tension can be contacted with the surface of the single crystal silicon more uniformly, the suede solution in the examples 1 to 4 is stable, and no obvious layering phenomenon and no obvious precipitate are observed after 50 days at 25+/-1 ℃;
in addition, in the embodiment 2, the addition amount of the organic alkali polyethylenimine is more, and the organic alkali has low corrosion to the monocrystalline silicon wafer, so that the obtained texturing liquid can gently texture monocrystalline silicon, the texture obtained by the preparation is more uniform, and the corresponding reflectivity is lower; the organic alkali polyethylenimine exists in water in the form of polymeric cations, heavy metal ions can be chelated, pollution of heavy metal ions possibly mixed in the texturing process to monocrystalline silicon wafers is eliminated, active imine groups in the polyethylenimine can be adsorbed on the surfaces of the monocrystalline silicon wafers, uniform corrosion of hydroxyl ions to the monocrystalline silicon wafers during texturing is regulated, and desorption of products on the surfaces of the monocrystalline silicon wafers can be promoted by a long-chain structure of the polyethylenimine, so that the finally obtained textured surfaces are more uniform.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The wool making liquid for the monocrystalline silicon is characterized by comprising the following components in percentage by mass:
1-3% of alkaline substances, 0.3-2.5% of texturing additives, 5-30% of eutectic solvents and the balance of deionized water;
the preparation method of the eutectic solvent comprises the following steps:
drying (2-hydroxyethyl) trimethyl ammonium hydroxide and urea in a vacuum drying oven at 60 ℃ for 12h respectively according to the mass ratio of n (2-hydroxyethyl) trimethylammonium hydroxide :n Urea Mixing and stirring the materials in a ratio of (1:2), sealing, and heating the materials in an oil bath at the temperature of 70-80 ℃ until colorless transparent liquid is obtained, thus obtaining the choline chloride-urea eutectic solvent;
wherein the (2-hydroxyethyl) trimethylammonium hydroxide can be replaced by n-octyl trimethylammonium chloride, dodecyl trimethylammonium chloride or (2-hydroxyethyl) acetyl trimethylammonium chloride;
correspondingly, the n-octyl trimethyl ammonium chloride is mixed with urea to prepare the n-octyl trimethyl ammonium chloride-urea eutectic solvent;
the dodecyl trimethyl ammonium chloride and urea are mixed to prepare a dodecyl trimethyl ammonium chloride-urea eutectic solvent;
and mixing the (2-hydroxyethyl) acetyl trimethyl ammonium chloride with urea to prepare the (2-hydroxyethyl) acetyl trimethyl ammonium chloride-urea eutectic solvent.
2. The etching solution for monocrystalline silicon according to claim 1, wherein the eutectic solvent accounts for 15-28% of the etching solution by mass.
3. A texturing solution for single crystal silicon according to claim 1, wherein said basic substance comprises an inorganic base and an organic base; wherein, the liquid crystal display device comprises a liquid crystal display device,
the inorganic alkali is sodium hydroxide or potassium hydroxide, and the inorganic alkali accounts for 1-2% of the mass of the texturing liquid;
the organic alkali is polyethyleneimine, and the organic alkali accounts for 0.5-1% of the mass of the wool making liquid.
4. The texturing solution for monocrystalline silicon according to claim 1, wherein the texturing additive comprises the following components in percentage by mass: 0.1 to 0.5 percent of water-soluble polymer resin, 0.1 to 1 percent of defoamer and 0.01 to 0.1 percent of buffer;
the water-soluble high polymer resin is water-soluble alkyd resin or water-soluble acrylic resin, the defoamer is polyether defoamer or organosilicon defoamer, and the buffer is sodium lactate or sodium bicarbonate.
5. A method for texturing monocrystalline silicon, characterized in that the monocrystalline silicon wafer is textured by the texturing solution according to claim 1, and the method comprises the following steps:
(1) Dissolving an alkaline substance in water to prepare alkali liquor, and uniformly mixing a texturing additive, a eutectic solvent, water and the alkaline substance according to mass proportion;
(2) Placing the monocrystalline silicon piece into pretreatment liquid for soaking treatment, and then carrying out ultrasonic treatment and cleaning for standby;
(3) Immersing the pretreated monocrystalline silicon piece into the texturing solution prepared in the step (1) for surface texturing, and sequentially washing the textured monocrystalline silicon piece with water and absolute ethyl alcohol for three times to obtain the textured monocrystalline silicon piece.
6. The method for producing silicon single crystal according to claim 5, wherein in the step (2), the pretreatment liquid comprises the following components in percentage by mass: 1-5% of sodium silicate, 0.5-2% of triton X-100 polyethylene glycol monooctyl phenyl ether, 1-3% of OP-10, 0.5-2% of sodium tripolyphosphate, 1-3% of polyether defoamer GP and the balance of water.
7. The method of claim 5 or 6, wherein the pretreatment temperature in the step (2) is 50-60 ℃, the ultrasonic power is 60-100W, the ultrasonic time is 5-10min, and the silicon is cleaned with absolute ethanol.
8. The method of claim 5, wherein the temperature of the single crystal silicon is 50-85 ℃ and the time of the single crystal silicon is 80-250s.
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| CN114182356A (en) * | 2021-12-23 | 2022-03-15 | 江苏捷捷半导体新材料有限公司 | Low-reflectivity monocrystalline silicon wafer texturing additive, preparation method and application thereof |
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| CN107287597A (en) * | 2016-03-30 | 2017-10-24 | 杭州聚力氢能科技有限公司 | Wool-making agent of monocrystalline silicon surface processing and preparation method thereof and application method |
| CN114182356A (en) * | 2021-12-23 | 2022-03-15 | 江苏捷捷半导体新材料有限公司 | Low-reflectivity monocrystalline silicon wafer texturing additive, preparation method and application thereof |
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