CN109599458A - Crystal silicon chip surface pyramid flannelette preparation method - Google Patents
Crystal silicon chip surface pyramid flannelette preparation method Download PDFInfo
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- CN109599458A CN109599458A CN201811293773.8A CN201811293773A CN109599458A CN 109599458 A CN109599458 A CN 109599458A CN 201811293773 A CN201811293773 A CN 201811293773A CN 109599458 A CN109599458 A CN 109599458A
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- copper
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- chloride
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 139
- 239000010703 silicon Substances 0.000 title claims abstract description 139
- 239000013078 crystal Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 70
- 239000008367 deionised water Substances 0.000 claims description 61
- 229910021641 deionized water Inorganic materials 0.000 claims description 61
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 47
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 31
- 239000011259 mixed solution Substances 0.000 claims description 31
- 238000004140 cleaning Methods 0.000 claims description 30
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 26
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 25
- 241000209094 Oryza Species 0.000 claims description 23
- 235000007164 Oryza sativa Nutrition 0.000 claims description 23
- 235000009566 rice Nutrition 0.000 claims description 23
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 16
- 230000007797 corrosion Effects 0.000 claims description 14
- 238000005260 corrosion Methods 0.000 claims description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 9
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 9
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 9
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 9
- 229940099607 manganese chloride Drugs 0.000 claims description 9
- 235000002867 manganese chloride Nutrition 0.000 claims description 9
- 239000011565 manganese chloride Substances 0.000 claims description 9
- 229940071870 hydroiodic acid Drugs 0.000 claims description 7
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 229910052744 lithium Inorganic materials 0.000 claims 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims 1
- 229920005591 polysilicon Polymers 0.000 claims 1
- 229910021419 crystalline silicon Inorganic materials 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 44
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 40
- 229960002050 hydrofluoric acid Drugs 0.000 description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- 229960000935 dehydrated alcohol Drugs 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 20
- 238000002156 mixing Methods 0.000 description 20
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 20
- 238000002604 ultrasonography Methods 0.000 description 20
- 238000007654 immersion Methods 0.000 description 19
- 239000007788 liquid Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 238000002242 deionisation method Methods 0.000 description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000003518 caustics Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- -1 tetramethyl lithium hydroxide Chemical compound 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 241000127225 Enceliopsis nudicaulis Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- LITYQKYYGUGQLY-UHFFFAOYSA-N iron nitric acid Chemical compound [Fe].O[N+]([O-])=O LITYQKYYGUGQLY-UHFFFAOYSA-N 0.000 description 1
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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)
- General Physics & Mathematics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Computer Hardware Design (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of crystal silicon chip surface pyramid flannelette preparation methods, belong to field of new materials.The present invention can prepare large area micro-nano metrical scale pyramid array suede structure in surface of crystalline silicon, and prepared micro-nano positive pyramid density is big, surface is smooth, can dramatically increase absorption of the silicon chip surface to light.The present invention prepares pyramid flannelette simple process and low cost, can be used for the application such as solar battery on a large scale.
Description
Technical field
The present invention relates to a kind of crystal silicon chip surface pyramid flannelette preparation methods, belong to new material technology field.
Background technique
Silicon is only second to the second element abundant of oxygen as content on the earth's crust, is widely used in microelectronics, two pole of crystal
The fields such as pipe, space travel, optical fiber, solar battery.And in solar cells, optical loss is to influence its photoelectricity to turn
As soon as changing the key factor of efficiency, therefore the light reflection research for reducing silicon chip surface is of crucial importance.In commercial monocrystalline silicon battery
Largely the method for caustic corrosion is used to prepare pyramid array in silicon chip surface to achieve the effect that antireflective at present.When sunlight enters
When being mapped to pyramid surface, the sunray of reflection can be further radiated in adjacent positive pyramid structure, be carried out secondary
Incident and reflection, thus reduces the reflection of sunlight and increases silicon to the absorption of sunlight and improve the effect of solar battery
Rate.The research surface of nearly half a century, the preparation method of pyramid array are only limitted to alkaline solution such as lithium hydroxide, hydroxide
Manganese, tetramethyl lithium hydroxide etc. [referring to: Chinese patent CN201310562781.9] or tetramethyl lithium hydroxide corrosive liquid [ginseng
See: Chinese patent ZL200410017032.9], and positive pyramid out can not be corroded in silicon face using acid hydrofluoric acid solution
Array.1973, U.S. Zwicker et al. discovery lithium fluoride and copper nitrate etchant solution can corrode out golden word in silicon face
Tower structure [referring to: W.K.Zwicker, S.K.Kurtz, Anisotropic etching of silicon using
Electrochemical displacement reactions, Semiconductor Silicon, Eds.:Huff, H.R.&
Burgess,R.R.,Electrochemical Society,Pennington,315-326,1973].2006, Tsinghua University
Researcher uses copper particle as corrosion catalyst, corrodes pyramid-like in silicon face using hydrofluoric acid and nitric acid iron mixed solution
Porous structure [referring to: Kuiqing Peng, Juejun Hu, Yunjie Yan, Yin Wu, Hui Fang, Ying Xu,
ShuitTong Lee,and Jing Zhu,Adv.Funct.Mater.16,387–394,2006].2015, Chinese Academy of Sciences's physics
Institute researcher using the hydrofluoric acid solution containing copper ion source and oxidant silicon face corrode out pyramid structure [referring to:
Chinese patent CN105405755A].But the above method is easy to deposit a large amount of copper nano particles in silicon face in corrosion process,
Due to porous containing strong oxidizers, the pyramid flannelettes corroded such as hydrogen peroxide.
Summary of the invention
The purpose of the present invention is to provide a kind of novel crystal silicon chip surface pyramid flannelette preparation method, this method benefits
With containing cupric salt (such as copper chloride, copper sulphate and copper nitrate) and soluble halide (lithium chloride, manganese chloride, iron chloride,
Hydrobromic acid and hydroiodic acid etc.) hydrofluoric acid solution corrode crystalline silicon, the positive pyramid of large area micro-nano rice can be prepared in silicon face
Array structure.This method is without strong oxidizers such as hydrogen peroxide, and the micro-nano positive pyramid surface corroded is smooth, defect is few and class
It is similar to pyramid structure obtained by caustic corrosion, therefore is with a wide range of applications in fields such as solar batteries.
A kind of surface of crystalline silicon acidity etching method proposed by the present invention, it is characterised in that: the method is as follows
It carries out:
(1) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), lithium chloride and hydrogen
In the container of fluoric acid mixed solution, large area micro-nano out can be corroded in silicon chip surface by reacting at 20-90 DEG C 10-100 minutes
Silicon wafer after corrosion, is then put into and impregnates the copper for removing surface remaining inside nitric acid or wang aqueous solution by the positive pyramid flannelette of rice
Grain is simultaneously cleaned with deionized water；
(2) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), manganese chloride and hydrogen
In the container of fluoric acid mixed solution, large area micro-nano out can be corroded in silicon chip surface by reacting at 20-90 DEG C 10-100 minutes
Silicon wafer after corrosion, is then put into and impregnates the copper for removing surface remaining inside nitric acid or wang aqueous solution by the positive pyramid flannelette of rice
Grain is simultaneously cleaned with deionized water；
(3) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), iron chloride and hydrogen
In the container of fluoric acid mixed solution, large area micro-nano out can be corroded in silicon chip surface by reacting at 20-90 DEG C 10-100 minutes
Silicon wafer after corrosion, is then put into and impregnates the copper for removing surface remaining inside nitric acid or wang aqueous solution by the positive pyramid flannelette of rice
Grain is simultaneously cleaned with deionized water；
(4) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), hydrobromic acid and hydrogen
In the container of fluoric acid mixed solution, large area micro-nano out can be corroded in silicon chip surface by reacting at 20-90 DEG C 10-100 minutes
Silicon wafer after corrosion, is then put into and impregnates the copper for removing surface remaining inside nitric acid or wang aqueous solution by the positive pyramid flannelette of rice
Grain is simultaneously cleaned with deionized water；
(5) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), hydroiodic acid and hydrogen
In the container of fluoric acid mixed solution, large area micro-nano out can be corroded in silicon chip surface by reacting at 20-90 DEG C 10-100 minutes
Silicon wafer after corrosion, is then put into and impregnates the copper for removing surface remaining inside nitric acid or wang aqueous solution by the positive pyramid flannelette of rice
Grain is simultaneously cleaned with deionized water；
Mantoquita (copper chloride/copper sulphate/copper nitrate) concentration in the step (1) is 0.001-0.1mol/L, lithium chloride
Concentration is 0.5-5mol/L, hydrofluoric acid concentration 1-10.0mol/L.Mantoquita (copper chloride/copper sulphate/nitre in the step (2)
Sour copper) concentration be 0.001-0.1mol/L, manganese chloride concentration be 0.5-4mol/L, hydrofluoric acid concentration 1-10.0mol/L.It is described
Mantoquita (copper chloride/copper sulphate/copper nitrate) concentration in step (3) is 0.001-0.1mol/L, ferric chloride concn 0.05-
0.2mol/L, hydrofluoric acid concentration 1-10.0mol/L.Mantoquita (copper chloride/copper sulphate/copper nitrate) in the step (4) is dense
Degree is 0.001-0.1mol/L, and hydrobromic acid concentration is 0.5-5mol/L, hydrofluoric acid concentration 1-10.0mol/L.The step (5)
In mantoquita (copper chloride/copper sulphate/copper nitrate) concentration be 0.001-0.1mol/L, hydriodic acid concentration 0.5-5mol/L, hydrogen
Fluoric acid concentration is 1-10.0mol/L.
Detailed description of the invention
Fig. 1 is the positive pyramid array scanning electron microscope shape appearance figure that the embodiment of the present invention 1 is prepared in monocrystalline silicon (100) crystal face
Fig. 2 is the positive pyramid array scanning electron microscope shape appearance figure that the embodiment of the present invention 5 is prepared in monocrystalline silicon (100) crystal face
Fig. 3 is the positive pyramid array scanning electron microscope shape appearance figure that the embodiment of the present invention 9 is prepared in monocrystalline silicon (100) crystal face
Fig. 4 is the positive pyramid array scanning electron microscope shape appearance figure that the embodiment of the present invention 13 is prepared in monocrystalline silicon (100) crystal face
Fig. 5 is the positive pyramid array scanning electron microscope shape appearance figure that the embodiment of the present invention 17 is prepared in monocrystalline silicon (100) crystal face
Specific embodiment
The present invention can prepare large area micro-nano metrical scale pyramid structure on crystalline silicon (100) surface.This method system
Standby micro-nano positive pyramid density is big, and the smooth defect in surface is few, can increase absorption of the silicon chip surface to light, therefore too
The fields such as positive energy battery are with a wide range of applications.Below with reference to embodiment, the present invention will be further described:
Embodiment 1
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper chloride, 2mol/L lithium chloride and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 2
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.005mol/L copper chloride, 1.5mol/L lithium chloride and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 80 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 3
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper sulphate, 2mol/L lithium chloride and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 4
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper nitrate, 2mol/L lithium chloride and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 5
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper chloride, 2mol/L manganese chloride and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 6
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.005mol/L copper chloride, 1.5mol/L manganese chloride and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 80 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 7
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper sulphate, 2mol/L manganese chloride and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 8
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper nitrate, 2mol/L manganese chloride and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 9
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.05mol/L copper chloride, 0.3mol/L iron chloride and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 10
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.005mol/L copper chloride, 0.1mol/L iron chloride and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 80 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 11
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.05mol/L copper sulphate, 0.3mol/L iron chloride and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 12
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.05mol/L copper nitrate, 0.3mol/L iron chloride and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 13
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper chloride, 2mol/L hydrobromic acid and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 14
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.005mol/L copper chloride, 1.5mol/L hydrobromic acid and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 80 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 15
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper sulphate, 2mol/L hydrobromic acid and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 16
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper nitrate, 2mol/L hydrobromic acid and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Flannelette, then by resulting silicon wafer be put into chloroazotic acid ultrasound impregnate the grains of 10 minutes removal silicon face remainings and spend from
Sub- water cleaning.
Embodiment 17
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper chloride, 2mol/L hydroiodic acid and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 18
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up, which is put into, fills 0.005mol/L copper chloride, 1.5mol/L hydroiodic acid and the mixing of 5.0mol/L hydrofluoric acid
Large area micro-nano meter Zheng Jin word out can be corroded in silicon chip surface by reacting at 80 DEG C in the polytetrafluoroethylcontainer container of solution 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionization by tower flannelette
Water cleaning.
Embodiment 19
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper sulphate, 2mol/L hydroiodic acid and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Embodiment 20
Successively it is cleaned by ultrasonic monocrystalline silicon piece with acetone, dehydrated alcohol and deionized water first, silicon wafer is then put into volume
Than heating 30 minutes in the mixed solution of hydrogen peroxide and the concentrated sulfuric acid for 1:3, then cleaned up again with deionized water；It will
The monocrystalline silicon piece cleaned up be put into fill 0.05mol/L copper nitrate, 2mol/L hydroiodic acid and 5.0mol/L hydrofluoric acid mixing it is molten
The positive pyramid of large area micro-nano rice out can be corroded in silicon chip surface by reacting at 25 DEG C in the polytetrafluoroethylcontainer container of liquid 30 minutes
Then resulting silicon wafer is put into the particle of 10 minutes removal silicon face remainings of ultrasound immersion in chloroazotic acid and uses deionized water by flannelette
Cleaning.
Claims (8)
1. crystal silicon chip surface pyramid flannelette preparation method, it is characterised in that: the method successively carries out as follows,
(1) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), lithium chloride and hydrofluoric acid
In the container of mixed solution, reacting at 20-90 DEG C can corrode out that large area micro-nano rice is being just for 10-100 minutes in silicon chip surface
Then silicon wafer after corrosion is put into and impregnates the copper particle for removing surface remaining inside nitric acid or wang aqueous solution simultaneously by pyramid flannelette
It is cleaned with deionized water；
(2) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), manganese chloride and hydrofluoric acid
In the container of mixed solution, reacting at 20-90 DEG C can corrode out that large area micro-nano rice is being just for 10-100 minutes in silicon chip surface
Then silicon wafer after corrosion is put into and impregnates the copper particle for removing surface remaining inside nitric acid or wang aqueous solution simultaneously by pyramid flannelette
It is cleaned with deionized water；
(3) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), iron chloride and hydrofluoric acid
In the container of mixed solution, reacting at 20-90 DEG C can corrode out that large area micro-nano rice is being just for 10-100 minutes in silicon chip surface
Then silicon wafer after corrosion is put into and impregnates the copper particle for removing surface remaining inside nitric acid or wang aqueous solution simultaneously by pyramid flannelette
It is cleaned with deionized water；
(4) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), hydrobromic acid and hydrofluoric acid
In the container of mixed solution, reacting at 20-90 DEG C can corrode out that large area micro-nano rice is being just for 10-100 minutes in silicon chip surface
Then silicon wafer after corrosion is put into and impregnates the copper particle for removing surface remaining inside nitric acid or wang aqueous solution simultaneously by pyramid flannelette
It is cleaned with deionized water；
(5) crystal silicon chip of surface cleaning is put into containing mantoquita (copper chloride/copper sulphate/copper nitrate), hydroiodic acid and hydrofluoric acid
In the container of mixed solution, reacting at 20-90 DEG C can corrode out that large area micro-nano rice is being just for 10-100 minutes in silicon chip surface
Then silicon wafer after corrosion is put into and impregnates the copper particle for removing surface remaining inside nitric acid or wang aqueous solution simultaneously by pyramid flannelette
It is cleaned with deionized water.
Mantoquita 2. pyramid flannelette preparation method in crystal silicon chip surface according to claim 1, in the step (2)
(copper chloride/copper sulphate/copper nitrate) concentration is 0.001-0.1mol/L, and chlorination lithium concentration is 0.5-5.0mol/L, and hydrofluoric acid is dense
Degree is 1-10mol/L.
Mantoquita 3. pyramid flannelette preparation method in crystal silicon chip surface according to claim 1, in the step (4)
(copper chloride/copper sulphate/copper nitrate) concentration is 0.001-0.1mol/L, and manganese chloride concentration is 0.5-4.0mol/L, and hydrofluoric acid is dense
Degree is 1-10mol/L.
Mantoquita 4. pyramid flannelette preparation method in crystal silicon chip surface according to claim 1, in the step (1)
(copper chloride/copper sulphate/copper nitrate) concentration is 0.001-0.1mol/L, ferric chloride concn 0.05-2.0mol/L, and hydrofluoric acid is dense
Degree is 1-10mol/L.
Mantoquita 5. pyramid flannelette preparation method in crystal silicon chip surface according to claim 1, in the step (5)
(copper chloride/copper sulphate/copper nitrate) concentration is 0.001-0.1mol/L, and hydrobromic acid concentration is 0.5-5.0mol/L, and hydrofluoric acid is dense
Degree is 1-10mol/L.
Mantoquita 6. pyramid flannelette preparation method in crystal silicon chip surface according to claim 1, in the step (5)
(copper chloride/copper sulphate/copper nitrate) concentration is 0.001-0.1mol/L, hydriodic acid concentration 0.5-5.0mol/L, and hydrofluoric acid is dense
Degree is 1-10mol/L.
7. pyramid flannelette preparation method in crystal silicon chip surface according to claim 1, the silicon wafer is either monocrystalline
Silicon wafer can be polysilicon chip again.
8. pyramid flannelette preparation method in crystal silicon chip surface according to claim 1, the step (1), (2), (3),
(4) and (5) obtained micro-nano pyramid flannelette can be used for the application such as silicon solar cell.
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| CN114808144A (en) * | 2022-04-08 | 2022-07-29 | 北京师范大学珠海校区 | Wet etching crystalline silicon inverted pyramid structure and positive pyramid structure texturing method |
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