CN103904157A - Method for making texture surface of silicon wafer - Google Patents
Method for making texture surface of silicon wafer Download PDFInfo
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- CN103904157A CN103904157A CN201310746508.1A CN201310746508A CN103904157A CN 103904157 A CN103904157 A CN 103904157A CN 201310746508 A CN201310746508 A CN 201310746508A CN 103904157 A CN103904157 A CN 103904157A
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- wool
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 87
- 239000010703 silicon Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 78
- 238000004140 cleaning Methods 0.000 claims abstract description 20
- 238000003631 wet chemical etching Methods 0.000 claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 88
- 210000002268 wool Anatomy 0.000 claims description 83
- 235000008216 herbs Nutrition 0.000 claims description 73
- 238000005260 corrosion Methods 0.000 claims description 43
- 230000007797 corrosion Effects 0.000 claims description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 32
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 31
- 238000009792 diffusion process Methods 0.000 claims description 31
- 238000005530 etching Methods 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 26
- 229910017604 nitric acid Inorganic materials 0.000 claims description 26
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 25
- 229910052796 boron Inorganic materials 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 24
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 24
- 229910052698 phosphorus Inorganic materials 0.000 claims description 24
- 239000011574 phosphorus Substances 0.000 claims description 24
- 239000002253 acid Substances 0.000 claims description 20
- 150000007529 inorganic bases Chemical class 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- 239000002019 doping agent Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 230000001681 protective effect Effects 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical group ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- ILAHWRKJUDSMFH-UHFFFAOYSA-N boron tribromide Chemical compound BrB(Br)Br ILAHWRKJUDSMFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000004816 latex Substances 0.000 claims description 6
- 229920000126 latex Polymers 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 210000004209 hair Anatomy 0.000 claims description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000003570 air Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000010422 painting Methods 0.000 claims description 3
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 claims description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims description 2
- PHSPJQZRQAJPPF-UHFFFAOYSA-N N-alpha-Methylhistamine Chemical compound CNCCC1=CN=CN1 PHSPJQZRQAJPPF-UHFFFAOYSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 2
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000005297 pyrex Substances 0.000 claims description 2
- 230000002000 scavenging effect Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical group ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 2
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010981 drying operation Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 17
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000002310 reflectometry Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 19
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 10
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 10
- 229920005591 polysilicon Polymers 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 7
- 229910001882 dioxygen Inorganic materials 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 238000005247 gettering Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000007704 wet chemistry method Methods 0.000 description 2
- 241000361919 Metaphire sieboldi Species 0.000 description 1
- 238000003854 Surface Print Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000010307 cell transformation Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen potassium oxide Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
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- 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 Table
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/547—Monocrystalline silicon PV cells
-
- 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
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Weting (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention relates to a method for making the texture surface of a silicon wafer. The method includes the steps of firstly, pre-cleaning the silicon wafer; secondly, conducting doping on the surface of the silicon wafer; thirdly, making the texture surface through a wet chemical etching method; fourthly, cleaning and drying the texture surface. Compared with the prior art, the method has the advantages that the manufactured texture surface is small and even in structure and low in reflectivity, and the method is easy to operate, suitable for mass production and high in cell conversion efficiency and has wide application prospects in the field of solar cells.
Description
Technical field
The invention belongs to crystal silicon solar batteries field, especially relate to a kind of silicon wafer fine hair making method.
Background technology
Process for etching and diffusion technology are the important steps that affects solar cell photoelectric conversion efficiency, are also technique comparatively ripe in solar cell preparation flow.
Process for etching has mechanical carving groove method, mask corrosion honeycomb suede structure technology, electrochemical erosion method, reactive ion etching technology etc.In current battery process is produced, generally adopt the making herbs into wool of wet chemistry solution corrosion method, wherein monocrystalline silicon piece adopts caustic corrosion liquid making herbs into wool method to form " pyramid " suede structure; Polysilicon chip utilizes acid corrosion liquid making herbs into wool method to form " earthworm " shape matte texture.
In diffusion process, silicon face can form high-concentration dopant layer, becomes near the gettering center of the harmful impurity of some silicon faces, in subsequent technique, Symmicton is removed, and reduces complex centre, reaches and improves minority carrier life time, raising solar cell transformation efficiency object.Mainly phosphorus gettering, aluminium gettering and boron gettering at present.
Summary of the invention
The object of the present invention is to provide the etching method of a kind of silicon chip wet chemical etching technique after diffusion.This method is mainly to utilize the phosphorus atoms of silicon chip surface formation in diffusion process or the state of boron atom change silicon chip surface, form the even distortion of lattice layer of many atom level sizes, these defects of gathering in silicon chip become in wafer bulk and the impurity gettering center on nearly surface, thereby reduce the complex centre in silicon body; Simultaneously these by diffusing into the atom of silicon chip surface, captured by surperficial gettering center former in wafer bulk and impurity, the defect of silicon chip surface etc. on the nearly surface of silicon chip just become active corrosion " activation " point of subsequent chemistry corrosion making herbs into wool, the corrosion reaction activation energy of these points is lower, become the Seed Layer of silicon chip surface chemical corrosion method making herbs into wool, make silicon chip surface reaction rate faster than general chemistry corrosion making herbs into wool, also make the corrosion rate of whole silicon chip surface even.The matte of preparation is tiny and even in this way, reflectivity is low, be applicable to monocrystalline silicon, polysilicon, quasi-monocrystalline silicon, the battery conversion efficiency of preparation is high, be the fusion of common diffusion technology and general chemistry corrosion process for etching, cost is lower, and the process time shortens, adapt to demand of industrial production, development prospect is wide.
Technical scheme of the present invention provides a kind of silicon wafer fine hair making method: by silicon chip prerinse, then carry out surface doping at diffusion furnace; Further gained silicon chip is carried out to the making herbs into wool of wet chemical etching technique method; The remaining making herbs into wool corrosive liquid in cleaning silicon chip surface, finally cleans and dries afterwards, gets final product to obtain suede structure silicon chip.
The method providing according to technique scheme, comprises following steps altogether: 1) by silicon chip prerinse; 2) step 1) gained silicon chip is carried out to surface doping; 3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool; 4) by step 3) gained Wafer Cleaning drying.
In some embodiments, cleaning fluid described in step 1) is acid etching solution or alkaline corrosion liquid, and prerinse temperature is 3-85 DEG C, and the prerinse time is 1-40 minute.In some embodiments, acid etching solution is the mixed solution of nitric acid, hydrofluoric acid and water, and wherein the mass fraction of nitric acid is 5-65%, and the mass fraction of hydrofluoric acid is 2-45%; Alkaline corrosion liquid is the aqueous solution of inorganic base, and wherein the mass fraction of inorganic base is 0.5-30%; Described inorganic base is selected from ammoniacal liquor, lithium hydroxide, NaOH or potassium hydroxide.
In some embodiments, step 2) described in the surface doping agent of surface doping be selected from the surface doping agent of phosphorus source or the surface doping agent of boron source.In some embodiments, the surface doping agent of phosphorus source is selected from phosphorus oxychloride, phosphorus trichloride, phosphorus tribromide, phosphoric acid, trimethyl phosphate, phosphorus pentoxide, phosphorus devitrified glass, phosphorosilicate glass or phosphorus containing silicon dioxide latex source; The surface doping agent of boron source is selected from boron chloride, Boron tribromide, boric acid, trimethylborate, triproylborate, titanium dioxide two boron, boron nitride, boron devitrified glass, boracic silicon dioxide latex source or Pyrex.In some embodiments, step 2) in doping way be liquid state diffusion source, planar dopant host, box diffusion, solid diffusion, the diffusion of painting source, stopped pipe diffusion, gaseous state diffusion or precipitation diffusion.In some embodiments, step 2) described in the heat treatment temperature of adulterating be 800-1050 DEG C, doping heat treatment time is 5-120 minute; Doping protective atmosphere is selected from argon gas, nitrogen, oxygen or air; Silicon chip surface doping depth is 0.1-15 μ m.
In some embodiments, the corrosive liquid of the making herbs into wool of wet chemical etching technique described in step 3) is acid etching solution or alkaline corrosion liquid, and corrosion number of times is 1-4 time.In some embodiments, the corrosive liquid of wet chemical etching technique making herbs into wool is acid etching solution, is the mixed solution of hydrofluoric acid, corrosion reagent and water, and wherein the mass fraction of hydrofluoric acid is 2%-45%; Corrosion making herbs into wool temperature is 0-30 DEG C, and the corrosion making herbs into wool time is 1-20 minute; Corrosion reagent is selected from nitric acid, acetic acid, phosphoric acid, sulfuric acid or chromic acid.In some embodiments, the corrosive liquid of wet chemical etching technique making herbs into wool is alkaline corrosion liquid, is the mixed solution of inorganic base, isopropyl alcohol, sodium metasilicate, making herbs into wool additive and water, and wherein the mass fraction of inorganic base is 0.5-15%; Corrosion making herbs into wool temperature is 20-85 DEG C, and the corrosion making herbs into wool time is 5-40 minute; Inorganic base is selected from ammoniacal liquor, lithium hydroxide, NaOH or potassium hydroxide.In some embodiments, silicon wafer wool making etching extent described in step 3) of the present invention is 0.005-0.2mg/cm
2.
In some embodiments, in step 4), the cleaning solution of silicon chip is acidic aqueous solution or alkaline aqueous solution, and cleaning temperature is 15-30 DEG C, and scavenging period is 1-25 minute.Acidic aqueous solution is the mixed solution of hydrochloric acid, hydrofluoric acid and water, wherein hydrochloric acid mass fraction 2-10%, hydrofluoric acid mass fraction 2-10%; Alkaline aqueous solution is the aqueous solution of inorganic base, and wherein the mass fraction of inorganic base is 0.5-15%; Described inorganic base is selected from ammoniacal liquor, lithium hydroxide, NaOH or potassium hydroxide.
Etching method of the present invention, is applicable to P type or N-type solar energy-level silicon wafer.Wet chemical etching technique process for etching after diffusion, near silicon chip surface, impurity is absorbed, and reduces complex centre, contribute to improve minority carrier life time, improve Si wafer quality, reduce reflectivity, increase PN junction effective area, suede structure is more reasonable, and then reaches the object that improves battery conversion efficiency.The method has merged current common diffusion technology and wet chemistry process for etching, has that cost is low, simple to operate, making herbs into wool is repeated and the advantage such as good uniformity, is applicable to producing production requirement on line, has higher commercial value.
Unless clearly state in contrast, otherwise all scopes that the present invention quotes comprised end value.For example, " the corrosion making herbs into wool time is 1-20 minute " represents that the time T scope of corrosion making herbs into wool is 1min≤T≤20min.
The term "or" that the present invention uses represents alternative, if suitable, they can be combined, and that is to say, term "or" comprises each listed independent alternative and their combination.For example, " inorganic base is selected from ammoniacal liquor, lithium hydroxide, NaOH or potassium hydroxide " represents that inorganic base can be the one of ammoniacal liquor, lithium hydroxide, NaOH, potassium hydroxide, can be also its more than one combination.
Compared with existing making herbs into wool technology, the etching method tool that technical scheme of the present invention provides has the following advantages:
1, the diffusion Symmicton that in doping heat treatment process, silicon chip surface forms, can absorb impurity in the nearly surface of silicon chip and body, reduces complex centre, contributes to improve minority carrier life time and battery conversion efficiency;
2, after doping treatment silicon chip surface form densely covered chemical corrosion " activation " and point, as the Seed Layer of chemical corrosion making herbs into wool, suede structure is tiny and even, pile depth and width are moderate;
3, due to the existence of surface doping layer, form atom distortion layer, in follow-up chemical corrosion making herbs into wool process, corrosion rate is very fast, shortens the process time;
4, be applicable to solar level P type or n type single crystal silicon sheet, polysilicon chip, quasi-monocrystalline silicon, particularly for the higher low quality silicon chip of impurity content, applied widely;
5, diffusion technology and general chemistry corrosion process for etching require simply, and matte effect is reproducible, is applicable to large-scale industrialization and produces.
Brief description of the drawings
Fig. 1 is the polysilicon chip surface scan Electronic Speculum figure after the embodiment of the present invention 1 making herbs into wool.
Fig. 2 is the polysilicon chip surface scan Electronic Speculum figure after the embodiment of the present invention 2 making herbs into wool.
Fig. 3 is the monocrystalline silicon sheet surface scanning electron microscope (SEM) photograph after the embodiment of the present invention 3 making herbs into wool.
Fig. 4 is the polycrystalline field surface scanning electron microscope (SEM) photograph of the quasi-monocrystalline silicon after the embodiment of the present invention 4 making herbs into wool.
Embodiment
The following stated be the preferred embodiment of the present invention, what the present invention protected is not limited to following preferred implementation.It should be pointed out that on the basis of conceiving in these innovation and creation for a person skilled in the art, some distortion and the improvement made, all belong to protection scope of the present invention.
1) be that 0.5-3 Ω cm, thickness are 180 μ m, are of a size of 156 × 156 P type polysilicon chip prerinse by resistivity, solution is made up of nitric acid, hydrofluoric acid, deionized water, nitric acid mass fraction 44%, hydrofluoric acid mass fraction 4.9%, prerinse temperature is 8 DEG C, and the prerinse time is 5 minutes.
2) step 1) gained silicon chip is carried out to phosphorus doping: adopt liquid state diffusion source method; phosphorus source is phosphorus oxychloride; 850 DEG C of doping temperature; protective gas is high pure nitrogen and high purity oxygen gas; flow is respectively 1.5L/min; taking phosphorus source nitrogen flow is 0.5L/min, and doping time is 20 minutes, and recording silicon chip surface doping depth is 2 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: making herbs into wool corrosive liquid is made up of hydrofluoric acid, nitric acid and deionized water, nitric acid mass fraction 44%, hydrofluoric acid mass fraction 4.9%, making herbs into wool temperature is 6 DEG C, 2 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.01mg/cm
2.
4) by step 3) gained Wafer Cleaning drying: the sodium hydroxide solution rinsing that is first 1.5% with mass fraction, temperature is 20 DEG C, rinsing time is 10 minutes; Use acid solution rinsing, hydrochloric acid mass fraction is 5.6% again, and hydrofluoric acid mass fraction is 5.4%, and temperature is 20 DEG C, and rinsing time is 10 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 19.6%, and its stereoscan photograph as shown in Figure 1.
Embodiment 2
1) by resistivity be 0.5-3 Ω cm, thickness is 180 μ m, is of a size of 156 × 156 P type polysilicon chip prerinse, and solution is made up of nitric acid, hydrofluoric acid, deionized water, nitric acid mass fraction 27%, hydrofluoric acid mass fraction 3%, prerinse temperature is 10 DEG C, the prerinse time is 10 minutes.
2) step 1) gained silicon chip is carried out to boron doping: adopt liquid state diffusion source method; boron source is Boron tribromide; 920 DEG C of doping temperature; protective gas is high pure nitrogen and high purity oxygen gas; flow is respectively 1L/min; taking boron source nitrogen flow is 1L/min, and doping time is 30 minutes, and recording silicon chip surface doping depth is 5 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: making herbs into wool corrosive liquid is made up of hydrofluoric acid, phosphoric acid and deionized water, phosphoric acid quality mark 44%, hydrofluoric acid mass fraction 5%, making herbs into wool temperature is 8 DEG C, 2.5 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.03mg/cm
2.
4) by step 3) gained Wafer Cleaning drying: the sodium hydroxide solution that is first 3% with mass fraction corrosion, temperature is 30 DEG C, etching time is 5 minutes; Use acid solution rinsing, hydrochloric acid mass fraction is 3.8% again, and hydrofluoric acid mass fraction is 5%, and temperature is 25 DEG C, and rinsing time is 25 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 19%, and its stereoscan photograph as shown in Figure 2.
Embodiment 3
1) resistivity is about to 3 Ω cm, thickness is 200 μ m, is of a size of 156 × 156 n type single crystal silicon sheet prerinse, and sodium hydroxide solution mass fraction used is 20%, and prerinse temperature is 80 DEG C, and the prerinse time is 15 minutes.
2) step 1) gained silicon chip is carried out to phosphorus doping: adopt silk screen print method and adopt liquid state diffusion source method; phosphorus source is phosphorus slurry and phosphorus oxychloride; silicon chip surface printing phosphorus is starched the heat treatment of adulterating after 200 DEG C of oven dry; 880 DEG C of doping temperature; protective gas is high pure nitrogen and high purity oxygen gas, and flow is respectively 0.5L/min, and taking phosphorus source nitrogen flow is 0.5L/min; doping time is 35 minutes, and recording silicon chip surface doping depth is 6.6 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: making herbs into wool corrosive liquid consists of NaOH mass fraction 2.5%, isopropyl alcohol volume fraction is 10%, sodium metasilicate mass fraction is 5%, time to create monocrystalline making herbs into wool additive S929-B volume fraction be 5%, 83 DEG C of making herbs into wool temperature, 25 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.1mg/cm2.
4) by step 3) gained Wafer Cleaning drying: use acid solution rinsing, hydrochloric acid mass fraction is 10%, and hydrofluoric acid mass fraction is 10%, and temperature is 30 DEG C, and rinsing time is 15 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 9.3%, and its stereoscan photograph as shown in Figure 3.
1) resistivity is about to 1-3 Ω cm, thickness is 180 μ m, is of a size of 156 × 156, (100) chip area accounts for the P type quasi-monocrystalline silicon prerinse of whole silicon area >=60%, solution is made up of nitric acid, hydrofluoric acid, deionized water, nitric acid mass fraction 10%, hydrofluoric acid mass fraction 40%, prerinse temperature is 15 DEG C, the prerinse time is 6 minutes.
2) step 1) gained silicon chip is carried out to boron doping: adopt liquid state diffusion source method, boron source is trimethylborate, 900 DEG C of doping temperature; Protective gas is high pure nitrogen and high purity oxygen gas, and flow is respectively 1L/min, 0.2L/min, and taking boron source argon stream amount is 1L/min, and doping time is 10 minutes, and recording silicon chip surface doping depth is 0.5 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: alkaline corrosion liquid making herbs into wool after first acid etching solution making herbs into wool, acid etching solution is made up of hydrofluoric acid, nitric acid and water, nitric acid mass fraction 40%, hydrofluoric acid mass fraction 4.5%, making herbs into wool temperature is 5 DEG C, 1 minute making herbs into wool time; Alkaline corrosion liquid hydrogen potassium oxide mass fraction 2%, isopropyl alcohol volume fraction is 5%, sodium metasilicate mass fraction is 5%, time to create monocrystalline making herbs into wool additive S929-B volume fraction be 5%, 80 DEG C of making herbs into wool temperature, 20 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.04mg/cm2.
4) by step 3) gained Wafer Cleaning drying: use acid solution rinsing, hydrochloric acid mass fraction is 7%, and hydrofluoric acid mass fraction is 8.8%, and temperature is 15 DEG C, and rinsing time is 15 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 9.8%, and its polycrystalline region stereoscan photograph as shown in Figure 4.
Embodiment 5
1) by resistivity be 0.5-3 Ω cm, thickness be 180 μ m (± 5 μ m), be of a size of 156 × 156 N-type polysilicon chip prerinse, solution is made up of nitric acid, hydrofluoric acid, deionized water, nitric acid mass fraction 5%, hydrofluoric acid mass fraction 10%, prerinse temperature is 3 DEG C, and the prerinse time is 20 minutes.
2) step 1) gained silicon chip is carried out to boron doping: adopt diffusion method admittedly, boron source is boron nitride, 1050 DEG C of doping temperature; protective gas is high pure nitrogen and oxygen; flow is respectively 2L/min, 0.1L/min, and doping time is 120 minutes, and recording silicon chip surface doping depth is 15 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: making herbs into wool corrosive liquid is made up of hydrofluoric acid, acetic acid, nitric acid and deionized water, acetic acid quality mark 5%, nitric acid mass fraction 3%, hydrofluoric acid mass fraction 40%, making herbs into wool temperature is 10 DEG C, 15 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.18mg/cm2.
4) by step 3) gained Wafer Cleaning and dry: the potassium hydroxide that is first 15% with mass fraction and 5% ammoniacal liquor mixed solution rinsing, temperature is 25 DEG C, rinsing time is 2 minutes; Use acid solution rinsing, hydrochloric acid mass fraction is 10% again, and hydrofluoric acid mass fraction is 10%, and temperature is 25 DEG C, and rinsing time is 25 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 19.8%.
Embodiment 6
1) resistivity is about to 3 Ω cm, thickness be 200 μ m (± 5 μ m), be of a size of 156 × 156 p type single crystal silicon sheet prerinse, sodium hydroxide solution mass fraction used is 10%, prerinse temperature is 85 DEG C, the prerinse time is 10 minutes.
2) step 1) gained silicon chip is carried out to boron doping: adopt planar dopant host method, boron source is boron devitrified glass, 950 DEG C of doping temperature; protective gas is the air after dust removal by filtration; flow is 2L/min, and doping time is 60 minutes, and recording silicon chip surface doping depth is 10 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: making herbs into wool corrosive liquid consists of potassium hydroxide mass fraction 10%, isopropyl alcohol volume fraction is 5%, sodium metasilicate mass fraction is 3%, time to create monocrystalline making herbs into wool additive S929-B volume fraction be 5%, 75 DEG C of making herbs into wool temperature, 15 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.12mg/cm2.
4) by step 3) gained Wafer Cleaning drying: use acid solution rinsing, hydrochloric acid mass fraction is 2%, and hydrofluoric acid mass fraction is 2%, and temperature is 30 DEG C, and rinsing time is 5 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 10%.
Embodiment 7
1) by resistivity be 2 Ω cm, thickness be 180 μ m (± 5 μ m), be of a size of 156 × 156 P type polysilicon chip prerinse, solution is made up of nitric acid, hydrofluoric acid, deionized water, nitric acid mass fraction 20%, hydrofluoric acid mass fraction 20%, prerinse temperature is 25 DEG C, and the prerinse time is 3 minutes.
2) step 1) gained silicon chip is carried out to boron doping after first phosphorus doping: adopt liquid state diffusion source method, phosphorus source is phosphorus oxychloride, 850 DEG C of phosphorus doping temperature, protective gas is high pure nitrogen and high purity oxygen gas, flow is respectively 1.5L/min, and taking phosphorus source nitrogen flow is 0.5L/min, and doping time is 10 minutes; Boron source is Boron tribromide, 950 DEG C of boron doping hot temperature degree, and protective gas is high pure nitrogen and high purity oxygen gas, and flow is respectively 2L/min, and taking boron source nitrogen flow is 0.5L/min, and doping time is 10 minutes, recording silicon chip surface doping depth is 4 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: making herbs into wool corrosive liquid is made up of hydrofluoric acid, phosphoric acid, sulfuric acid and deionized water, sulfuric acid mass fraction 5%, phosphoric acid quality mark is 5%, hydrofluoric acid mass fraction 10%, making herbs into wool temperature is 15 DEG C, 5 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.12mg/cm
2.
4) by step 3) gained Wafer Cleaning drying: the potassium hydroxide solution rinsing that is first 5% with mass fraction, temperature is 25 DEG C, rinsing time is 3 minutes; Use acid solution rinsing, hydrochloric acid mass fraction is 6% again, and hydrofluoric acid mass fraction is 6%, and temperature is 25 DEG C, and rinsing time is 10 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 20%.
Embodiment 8
1) by resistivity be 1 Ω cm, thickness be 180 μ m (± 5 μ m), be of a size of 156 × 156 P type polysilicon chip prerinse, solution is made up of nitric acid, hydrofluoric acid, deionized water, nitric acid mass fraction 40%, hydrofluoric acid mass fraction 10%, prerinse temperature is 6 DEG C, and the prerinse time is 8 minutes.
2) step 1) gained silicon chip is carried out to phosphorus doping: adopt painting source diffuse source method; phosphorus source is phosphorus containing silicon dioxide latex source; silicon chip surface coating latex source; the heat treatment of adulterating after dry under natural conditions; 890 DEG C of doping temperature, protective gas is high-purity argon gas and high purity oxygen gas, flow is respectively 1.5L/min; doping time is 40 minutes, and recording silicon chip surface doping depth is 7 μ m.
3) by step 2) gained silicon chip carries out wet chemical etching technique making herbs into wool: making herbs into wool corrosive liquid is made up of hydrofluoric acid, nitric acid and deionized water, nitric acid mass fraction 10%, hydrofluoric acid mass fraction 44%, making herbs into wool temperature is 6 DEG C, 2.5 minutes making herbs into wool time, recording silicon wafer wool making front and back etching extent is 0.15mg/cm
2.
4) by step 3) gained Wafer Cleaning drying: the sodium hydroxide solution rinsing that is first 7% with mass fraction, temperature is 20 DEG C, rinsing time is 5 minutes; Use acid solution rinsing, hydrochloric acid mass fraction is 5.6% again, and hydrofluoric acid mass fraction is 5.4%, and temperature is that 20 DEG C of rinsing times are 10 minutes; Finally by drying after washed with de-ionized water.
Its average reflectance in 350-1100nm wave-length coverage of gained silicon test is 21%.
Claims (16)
1. a silicon wafer fine hair making method, is characterized in that: by silicon chip prerinse, then carry out surface doping at diffusion furnace; Further gained silicon chip is carried out to the making herbs into wool of wet chemical etching technique method; The remaining making herbs into wool corrosive liquid in cleaning silicon chip surface, finally cleans and dries afterwards, gets final product to obtain suede structure silicon chip.
2. method according to claim 1, is characterized in that, described prewashed cleaning fluid is acid etching solution or alkaline corrosion liquid, and prerinse temperature is 3-85 DEG C, and the prerinse time is 1-40 minute.
3. method according to claim 2, is characterized in that, described acid etching solution is the mixed solution of nitric acid, hydrofluoric acid and water, and wherein the mass fraction of nitric acid is 5-65%, and the mass fraction of hydrofluoric acid is 2-45%; Described alkaline corrosion liquid is the aqueous solution of inorganic base, and wherein the mass fraction of inorganic base is 0.5-30%.
4. method according to claim 3, is characterized in that, described inorganic base is selected from ammoniacal liquor, lithium hydroxide, NaOH or potassium hydroxide.
5. method according to claim 1, is characterized in that, the surface doping agent of described surface doping is selected from the surface doping agent of phosphorus source or the surface doping agent of boron source.
6. method according to claim 6, it is characterized in that, the surface doping agent of described phosphorus source is selected from phosphorus oxychloride, phosphorus trichloride, phosphorus tribromide, phosphoric acid, trimethyl phosphate, phosphorus pentoxide, phosphorus devitrified glass, phosphorosilicate glass or phosphorus containing silicon dioxide latex source; The surface doping agent of boron source is selected from boron chloride, Boron tribromide, boric acid, trimethylborate, triproylborate, titanium dioxide two boron, boron nitride, boron devitrified glass, boracic silicon dioxide latex source or Pyrex.
7. method according to claim 1, is characterized in that, the doping way of described surface doping is liquid state diffusion source, planar dopant host, box diffusion, solid diffusion, the diffusion of painting source, stopped pipe diffusion, gaseous state diffusion or precipitation diffusion.
8. method according to claim 1, is characterized in that, the doping temperature of described surface doping is 800-1050 DEG C, and the heat treatment time of doping is 5-120 minute; The protective atmosphere of doping is selected from argon gas, nitrogen, oxygen or air; Silicon chip surface doping depth is 0.1-15 μ m.
9. method according to claim 1, is characterized in that, the corrosive liquid of described wet chemical etching technique making herbs into wool is acid etching solution or alkaline corrosion liquid, and corrosion number of times is 1-4 time.
10. method according to claim 9, is characterized in that, described acid etching solution is the mixed solution of hydrofluoric acid, corrosion reagent and water, and wherein the mass fraction of hydrofluoric acid is 2%-45%, and corrosion making herbs into wool temperature is 0-30 DEG C, and the corrosion making herbs into wool time is 1-20 minute.
11. methods according to claim 10, is characterized in that, described corrosion reagent is selected from nitric acid, acetic acid, phosphoric acid, sulfuric acid or chromic acid.
12. methods according to claim 9, is characterized in that, described alkaline corrosion liquid is the mixed solution of inorganic base, isopropyl alcohol, sodium metasilicate, making herbs into wool additive and water, and wherein the mass fraction of inorganic base is 0.5-15%; Corrosion making herbs into wool temperature is 20-85 DEG C, and the corrosion making herbs into wool time is 5-40 minute.
13. methods according to claim 12, is characterized in that, described inorganic base is selected from ammoniacal liquor, lithium hydroxide, NaOH or potassium hydroxide.
14. methods according to claim 1, is characterized in that, the etching extent of silicon wafer wool making is 0.005-0.2mg/cm
2.
15. methods according to claim 1, is characterized in that, described cleaning spin-drying operation cleaning solution used is acidic aqueous solution or alkaline aqueous solution, and cleaning temperature is 15-30 DEG C, and scavenging period is 1-25 minute.
16. methods according to claim 15, is characterized in that, described acid solution is the mixed solution of hydrochloric acid, hydrofluoric acid and water, wherein hydrochloric acid mass fraction 2-10%, hydrofluoric acid mass fraction 2-10%; Described alkaline aqueous solution is the aqueous solution of inorganic base, and wherein the mass fraction of inorganic base is 0.5-15%, and inorganic base is selected from ammoniacal liquor, lithium hydroxide, NaOH or potassium hydroxide.
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| CN104480532A (en) * | 2014-12-30 | 2015-04-01 | 江西赛维Ldk太阳能高科技有限公司 | Texturing preprocessing method of diamond wire cut polycrystalline silicon chip, textured preprocessed silicon chip and application thereof |
| CN106299019A (en) * | 2016-08-05 | 2017-01-04 | 山西潞安太阳能科技有限责任公司 | A kind of polysilicon chip back side purifying process |
| CN109309142A (en) * | 2017-07-26 | 2019-02-05 | 天津环鑫科技发展有限公司 | Liquid source diffusion process before silicon wafer glass passivation |
| CN110257072A (en) * | 2019-06-13 | 2019-09-20 | 常州时创能源科技有限公司 | Silicon wafer one texture-etching side and etching edge additive and its application |
| CN111092137A (en) * | 2019-12-26 | 2020-05-01 | 晋能清洁能源科技股份公司 | Texturing liquid for texturing polycrystalline silicon wafer and texturing method using same |
| CN114883454A (en) * | 2022-06-08 | 2022-08-09 | 湖南红太阳新能源科技有限公司 | Phosphorus diffusion gettering and cleaning method suitable for N-type silicon wafer |
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| CN104480532A (en) * | 2014-12-30 | 2015-04-01 | 江西赛维Ldk太阳能高科技有限公司 | Texturing preprocessing method of diamond wire cut polycrystalline silicon chip, textured preprocessed silicon chip and application thereof |
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| CN109309142A (en) * | 2017-07-26 | 2019-02-05 | 天津环鑫科技发展有限公司 | Liquid source diffusion process before silicon wafer glass passivation |
| CN109309142B (en) * | 2017-07-26 | 2021-09-07 | 天津环鑫科技发展有限公司 | Liquid source diffusion process before silicon wafer glass passivation |
| CN110257072A (en) * | 2019-06-13 | 2019-09-20 | 常州时创能源科技有限公司 | Silicon wafer one texture-etching side and etching edge additive and its application |
| CN111092137A (en) * | 2019-12-26 | 2020-05-01 | 晋能清洁能源科技股份公司 | Texturing liquid for texturing polycrystalline silicon wafer and texturing method using same |
| CN114883454A (en) * | 2022-06-08 | 2022-08-09 | 湖南红太阳新能源科技有限公司 | Phosphorus diffusion gettering and cleaning method suitable for N-type silicon wafer |
| CN114883454B (en) * | 2022-06-08 | 2024-04-30 | 湖南红太阳新能源科技有限公司 | Phosphorus diffusion gettering and cleaning method suitable for N-type silicon wafer |
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