CN106816487A - Metal inducement catalytic reaction liquid and preparation method thereof and application - Google Patents
Metal inducement catalytic reaction liquid and preparation method thereof and application Download PDFInfo
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- CN106816487A CN106816487A CN201510861891.4A CN201510861891A CN106816487A CN 106816487 A CN106816487 A CN 106816487A CN 201510861891 A CN201510861891 A CN 201510861891A CN 106816487 A CN106816487 A CN 106816487A
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- polysilicon chip
- reaction liquid
- catalytic reaction
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 94
- 239000002184 metal Substances 0.000 title claims abstract description 94
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 63
- 239000012295 chemical reaction liquid Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 44
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002923 metal particle Substances 0.000 claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000008021 deposition Effects 0.000 claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 28
- 239000010703 silicon Substances 0.000 claims abstract description 28
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 18
- 230000002378 acidificating effect Effects 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 101
- 229920005591 polysilicon Polymers 0.000 claims description 98
- 238000005530 etching Methods 0.000 claims description 51
- 238000000034 method Methods 0.000 claims description 43
- 238000005520 cutting process Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 229910021418 black silicon Inorganic materials 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000012423 maintenance Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 7
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 7
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 7
- 229920000053 polysorbate 80 Polymers 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 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 4
- 239000000463 material Substances 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 2
- -1 polyoxyethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 229910052738 indium Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000003825 pressing Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 230000013011 mating Effects 0.000 abstract description 5
- 238000007781 pre-processing Methods 0.000 abstract description 5
- 229910003460 diamond Inorganic materials 0.000 description 18
- 239000010432 diamond Substances 0.000 description 18
- 239000004570 mortar (masonry) Substances 0.000 description 15
- 238000002310 reflectometry Methods 0.000 description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 10
- 229910052737 gold Inorganic materials 0.000 description 10
- 239000010931 gold Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 235000008216 herbs Nutrition 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 210000002268 wool Anatomy 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001039 wet etching Methods 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000012459 cleaning agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001312 dry etching Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000001020 plasma etching Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910001573 adamantine Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent 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
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02363—Special surface textures of the semiconductor body itself, e.g. textured active layers
-
- 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
- H01L31/18—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
- 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
Landscapes
- 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 present invention relates to a kind of metal inducement catalytic reaction liquid and preparation method thereof and application.Metal inducement catalytic reaction liquid is grouped into by the following each group according to volume parts:Acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.Above-mentioned metal inducement catalytic reaction liquid includes acidic cleaner, nonionic surfactant, source metal and deionized water.Wherein, acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.Source metal can provide metallic.And nonionic surfactant plays a part of to lubricate dispersed metal particle.Silicon chip after pretreatment is put into this metal inducement catalytic reaction liquid of present invention offer carries out metal particle deposition, under the mating reaction of the above-mentioned each component of metal inducement catalytic reaction liquid, metallic can be on uniform deposition silicon chip after pre-processing, it is not easy to reunite.
Description
Technical field
The present invention relates to photovoltaic art, more particularly to a kind of metal inducement catalytic reaction liquid and preparation method thereof,
And application.
Background technology
In photovoltaic slice field, traditional mortar dicing method has used cutting liquid and carborundum, has cut
Cheng Hou, a large amount of waste mortars need online or processed offline, and this brings very big pressure to environment.And with light
The development of microtomy is lied prostrate, new diamond wire dicing method does not use mortar, it is only necessary to aqueous more than 90%
Coolant and consolidated diamond line (resin diamond wire), not only cutting speed is fast, and production efficiency is high,
And environmental protection pressure is small, it has also become the main flow direction of new microtomy, and it is applied to the big of silicon chip cutting
In large-scale production.
However, novel adamantine wire cutting is different from the silicon chip pattern obtained by traditional mortar cutting, the two pattern
Respectively as shown in Fig. 1 (a) and Fig. 1 (b), there is a plurality of cutting strain line on the former surface, and surface damage layer is shallower,
This causes traditional sour etching method can not to form effective matte on Buddha's warrior attendant wire cutting polysilicon chip surface, gives
The making herbs into wool operation of battery manufacturer brings very big difficulty.Therefore, researcher develops and various is cut for diamond wire
The etching method of polysilicon chip, including reactive ion etching method (Reactive Ion Etching), femtosecond laser
Method (Femtosecond Laser Method) etc., they belong to dry etching (Dry Etching) system,
Very harsh to the condition requirement of production device and method, manufacturing cost is expensive, and etches limited area, no
Beneficial to heavy industrialization application.And metal inducement method, belong to wet etching (Wet Etching) system,
Its pile effects is good, and manufacturing cost is relatively low, and reaction condition is easily realized, it has also become realize industrialized mass production
The important method of the black silicon matte of polysilicon chip.The black silicon matte that this kind of method is obtained, outward appearance is more black, and aperture is closed
Suitable, reflectivity is low, it is adaptable to the making of road battery afterwards, and can promote the raising of battery efficiency.
However, in metal inducement wet etching system, the general step of metal inducement wet etching is first will
The silicon chip of wire cutting is pre-processed, and then carries out the deposition and etching of metallic.In above process,
The dispersion of metallic is a very crucial step.If the dispersion of metallic can not be controlled well,
Then metallic can be very easy to reunite in etching process, as shown in Figure 2.And the reunion of metallic
The consumption of metallic can be accelerated, and cause the uniformity of silicon chip erosion to decline, it is unfavorable that matte is produced
Influence.
The content of the invention
Based on this, it is necessary to easily reunite for metallic in traditional metal inducement wet etching system
Problem, there is provided a kind of to make metallic be not easy the metal inducement catalytic reaction liquid reunited.
A kind of metal inducement catalytic reaction liquid, is grouped into by the following each group according to volume parts:
The acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.
Above-mentioned metal inducement catalytic reaction liquid includes acidic cleaner, nonionic surfactant, source metal
And deionized water.Wherein, acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.Source metal energy
Metallic is enough provided.And nonionic surfactant plays a part of to lubricate dispersed metal particle.To locate in advance
Silicon chip after reason be put into the present invention offer this metal inducement catalytic reaction liquid in carry out metallic sink
Product, under the mating reaction of the above-mentioned each component of metal inducement catalytic reaction liquid, metallic can uniformly sink
On product silicon chip after pre-processing, it is not easy to reunite.
Wherein in one embodiment, it is grouped into by the following each group according to volume parts:
Wherein in one embodiment, the volume ratio of the hydrofluoric acid and the hydrogen peroxide is 3:1~1:10.
Wherein in one embodiment, the nonionic surfactant is selected from ethanol, ethylene glycol, poly- second two
In alcohol, Tween-60, Tween-80, OPEO -10 and NPE at least one
Kind.
Wherein in one embodiment, the source metal is selected from gold chloride, chloroplatinic acid, silver nitrate and copper nitrate
In one kind.
Wherein in one embodiment, the electrical conductivity of the deionized water is less than 0.5 μ S/cm.
A kind of preparation method of metal inducement catalytic reaction liquid is also provided, is comprised the following steps:
By in source metal addition deionized water, the aqueous solution of source metal is obtained after mixing;
Acidic cleaner and nonionic surfactant are mixed, 5 DEG C~15 DEG C are cooled to, is added dropwise over afterwards
The aqueous solution of the source metal, obtains metal inducement catalytic reaction liquid after mixing;
The acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.
The preparation method of above-mentioned metal inducement catalytic reaction liquid prepares metal inducement catalytic reaction liquid, wherein
Including acidic cleaner, nonionic surfactant, source metal and deionized water.Wherein, acid cleaning
Agent is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.Source metal can provide metallic.And non-ionic surface
Activating agent plays a part of to lubricate dispersed metal particle.Silicon chip after pretreatment is put into present invention offer
Metal particle deposition is carried out in this metal inducement catalytic reaction liquid, in the above-mentioned of metal inducement catalytic reaction liquid
Under the mating reaction of each component, metallic can be on uniform deposition silicon chip after pre-processing, it is not easy to
Reunite.
Additionally, also providing a kind of black silicon etching method of Buddha's warrior attendant wire cutting polysilicon chip, comprise the following steps:
Polysilicon chip after Buddha's warrior attendant wire cutting is pre-processed to remove damage layer, is obtained pretreated many
Crystal silicon chip;
In the metal inducement catalytic reaction liquid that the pretreated polysilicon chip is put into described in claim 1,
Maintain to be taken out after 15s~90s, obtain the polysilicon chip after metal particle deposition;
Polysilicon chip after the metal particle deposition is put into etching solution and is performed etching, after being etched
Polysilicon chip;
The metallic of the polysilicon chip remained on surface after the etching is removed, is cleaned afterwards and is dried,
Obtain the polysilicon chip after black silicon etching.
The black silicon etching method of above-mentioned Buddha's warrior attendant wire cutting polysilicon chip, first puts pretreated polysilicon chip
Enter and carry out metal particle deposition in metal inducement catalytic reaction liquid, as a result of metal inducement catalytic reaction liquid,
Metallic can be evenly dispersed in silicon chip surface.Reaction, energy are performed etching after deposited metal particle again
Enough separate the etching solutions such as metal inducement catalytic reaction liquid and hydrogen peroxide, hydrofluoric acid, nitric acid, it is to avoid play
The metallic agglomeration that strong reaction zone comes, reduces the waste of noble metal, and it is uneven to avoid etching
The generation of phenomenon.Final polysilicon chip surface can obtain preferable nanometer suede, and this kind of matte can be reduced effectively
The reflectivity on polysilicon chip surface, promotes the raising of battery efficiency.Additionally, the method is simple to operate, cost
It is relatively low, and metallic is uniformly dispersed, it is adaptable to the making herbs into wool of large-area polycrystalline silicon chip.
Wherein in one embodiment, the pretreated polysilicon chip is put into described in claim 1
In metal inducement catalytic reaction liquid, maintain to be taken out after 15s~90s, obtain the polysilicon after metal particle deposition
The operation of piece is:
Support is provided, for supporting the pretreated polysilicon chip, the material of the support is polytetrafluoro
Ethene;
The pretreated polysilicon chip is put on the bracket, by the pretreated polysilicon chip
It is put into together with the support in the metal inducement catalytic reaction liquid described in claim 1, after the pretreatment
Polysilicon chip surface where plane perpendicular to the plane where the metal inducement catalytic reaction liquid;
Maintain to be taken out after 15s~90s, obtain the polysilicon chip after metal particle deposition.
Wherein in one embodiment, the polysilicon chip after the metal particle deposition is put into etching solution
In the operation for performing etching, it is 5 DEG C~15 DEG C to maintain etching temperature, and maintenance etch period is 2min~15min,
The etching solution is included according to the following each component of volume parts:
The nonionic surfactant be selected from ethanol, ethylene glycol, polyethylene glycol, Tween-60, Tween-80,
At least one in OPEO -10 and NPE.
Brief description of the drawings
Fig. 1 (a) is the SEM figures of the silicon chip pattern that Buddha's warrior attendant wire cutting is obtained;
Fig. 1 (b) is the SEM figures of the silicon chip pattern that traditional mortar cutting is obtained;
Fig. 2 is the SEM figures that gold particle is reunited in silicon chip surface;
Fig. 3 is the preparation method of the metal inducement catalytic reaction liquid of an implementation method;
Fig. 4 is the black silicon etching method of the Buddha's warrior attendant wire cutting polysilicon chip of an implementation method;
Fig. 5 is the deposition process of the metallic on polysilicon chip surface of an implementation method;
Fig. 6 is that the diamond wire of an implementation method cuts polysilicon chip and mortar is cut polysilicon chip and pre-processed respectively
The reflectance map for measuring afterwards;
Fig. 7 is the schematic device of the metal inducement catalytic reaction of an implementation method;
Fig. 8 is the gold grain of an implementation method in the dispersed SEM shape appearance figures in polysilicon chip surface;
Fig. 9 is two grades of SEM shape appearance figures of black silicon matte of an implementation method;
Figure 10 is that the diamond wire of an implementation method cuts polysilicon chip and mortar cuts polysilicon chip and carries out black silicon quarter respectively
The reflectance map measured after etching method treatment.
Specific embodiment
It is right below in conjunction with the accompanying drawings to enable the above objects, features and advantages of the present invention more obvious understandable
Specific embodiment of the invention is described in detail.Elaborate in the following description many details with
It is easy to fully understand the present invention.But the present invention can come real to be much different from other manner described here
Apply, those skilled in the art can do similar improvement, therefore this hair in the case of without prejudice to intension of the present invention
It is bright not limited by following public specific embodiment.
Unless otherwise defined, all of technologies and scientific terms used here by the article with belong to technology of the invention
The implication that the technical staff in field is generally understood that is identical.The art for being used in the description of the invention herein
Language is intended merely to describe the purpose of specific embodiment, it is not intended that in the limitation present invention.It is used herein
Term " and/or " include the arbitrary and all of combination of one or more related Listed Items.
The metal inducement catalytic reaction liquid of one implementation method, is grouped into by the following each group according to volume parts:
Acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.
In one preferably implementation method, metal inducement catalytic reaction liquid is by according to the following each of volume parts
Component is constituted:
In one preferably implementation method, the volume ratio of hydrofluoric acid and hydrogen peroxide is 3:1~1:10.
Nonionic surfactant can selected from ethanol, ethylene glycol, polyethylene glycol, Tween-60, Tween-80,
At least one in OPEO -10 and NPE.Nonionic surfactant energy
Enough make the metallic restored from source metal be not easy reunite, and it is dispersed in the solution.
Source metal is selected from the one kind in gold chloride, chloroplatinic acid, silver nitrate and copper nitrate.Source metal is used to provide
Metallic, generally soluble metallic salt, the different source metal of different metal particle correspondence.
The electrical conductivity of deionized water is less than 0.5 μ S/cm.The metal inducement catalytic reaction liquid of present embodiment is follow-up
Solar silicon wafers surface is directly acted on, because the foreign ion in above-mentioned deionized water is less, can be avoided
Excessive foreign ion remains in the surface of solar silicon wafers and reduces the cleanliness factor of silicon chip surface, so as to influence
It is subsequently used.
In sum, above-mentioned metal inducement catalytic reaction liquid includes acidic cleaner, non-ionic surface active
Agent, source metal and deionized water.Wherein, acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.
Source metal can provide metallic.And nonionic surfactant plays a part of to lubricate dispersed metal particle.
Silicon chip after pretreatment is put into this metal inducement catalytic reaction liquid of present invention offer carries out clipped wire
Son deposition, under the mating reaction of the above-mentioned each component of metal inducement catalytic reaction liquid, metallic can be equal
On even deposition silicon chip after pre-processing, it is not easy to reunite.
The preparation method of the metal inducement catalytic reaction liquid of one implementation method, as shown in figure 3, including following step
Suddenly:
S10, by source metal add deionized water in, the aqueous solution of source metal is obtained after mixing.
Source metal is selected from the one kind in gold chloride, chloroplatinic acid, silver nitrate and copper nitrate.
S20, acidic cleaner and nonionic surfactant are mixed, be cooled to 5 DEG C~15 DEG C, afterwards dropwise
The aqueous solution of the source metal in step S10 is added, metal inducement catalytic reaction liquid is obtained after mixing;It is acid
Cleaning agent is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.
The volume ratio of hydrofluoric acid and hydrogen peroxide is 3:1~1:10.
Nonionic surfactant is selected from ethanol, ethylene glycol, polyethylene glycol, Tween-60, Tween-80, octyl group
At least one in phenol polyethenoxy ether -10 and NPE.
The preparation method of above-mentioned metal inducement catalytic reaction liquid prepares metal inducement catalytic reaction liquid, wherein
Including acidic cleaner, nonionic surfactant, source metal and deionized water.Wherein, acid cleaning
Agent is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.Source metal can provide metallic.And non-ionic surface
Activating agent plays a part of to lubricate dispersed metal particle.Silicon chip after pretreatment is put into present invention offer
Metal particle deposition is carried out in this metal inducement catalytic reaction liquid, in the above-mentioned of metal inducement catalytic reaction liquid
Under the mating reaction of each component, metallic can be on uniform deposition silicon chip after pre-processing, it is not easy to
Reunite.
The black silicon etching method of the Buddha's warrior attendant wire cutting polysilicon chip of one implementation method, as shown in figure 4, including such as
Lower step:
S100, the polysilicon chip after Buddha's warrior attendant wire cutting is pre-processed to remove damage layer, pre-processed
Polysilicon chip afterwards.
The step of above-mentioned removing damages layer is to be capable of achieving using the conventional acid etching method in solar energy industry, i.e.,
Polysilicon after Buddha's warrior attendant wire cutting is put into HF (49%) and HNO3(65%) it is 1 according to volume ratio:3
In mixed solution, 5 DEG C~10 DEG C of maintenance reaction temperature can obtain pre- place after reaction time 1min~3min
Polysilicon chip after reason.
S200, the metal inducement that pretreated polysilicon chip in step S100 is put into above-mentioned implementation method is urged
Change in reaction solution, maintain to be taken out after 15s~90s, obtain the polysilicon chip after metal particle deposition.
As shown in figure 5, the metal inducement catalysis that pretreated polysilicon chip is put into above-mentioned implementation method is anti-
Answer in liquid, maintain to be taken out after 15s~90s, the operation for obtaining the polysilicon chip after metal particle deposition is:
S210, offer support, for supporting pretreated polysilicon chip, the material of support is polytetrafluoroethyl-ne
Alkene.
Support is used to support pretreated polysilicon chip, its contact area with pretreated polysilicon chip
It is more few better, it is to avoid the deposition of influence metallic.
S220, pretreated polysilicon chip is placed on the support of step S210, by pretreated polycrystalline
Silicon chip is put into the metal inducement catalytic reaction liquid of above-mentioned implementation method together with support, pretreated polycrystalline
Plane where the surface of silicon chip is perpendicular to the plane where metal inducement catalytic reaction liquid.
By the plane where the surface of pretreated polysilicon chip is perpendicular to metal inducement catalytic reaction liquid institute
Plane, then pretreated polysilicon chip be put into vertically in metal inducement catalytic reaction liquid.Business is needed herein
Polysilicon chip must be kept vertically, and prevent it from inclining.Metallic can be so avoided to be deposited because of Action of Gravity Field
Onto inclined polysilicon chip, and there is metallic and disperse uneven phenomenon.
Taken out after S230, maintenance 15s~90s, obtain the polysilicon chip after metal particle deposition.
Now, the dispersed metallic in the surface of polysilicon chip.In one preferably embodiment, gold
The size for belonging to particle is nanoscale, is conducive to subsequently carrying out making herbs into wool.
And the polysilicon chip after metal particle deposition need not be cleaned and dried, next step can be directly carried out.
S300, the polysilicon chip after metal particle deposition in step S200 be put into etching solution perform etching,
Polysilicon chip after being etched.
Polysilicon chip after metal particle deposition is put into the operation performed etching in etching solution, maintains to carve
Erosion temperature is 5 DEG C~15 DEG C, and maintenance etch period is 2min~15min.Etching solution includes following volume parts
Each component:
Nonionic surfactant is selected from ethanol, ethylene glycol, polyethylene glycol, Tween-60, Tween-80, octyl group
At least one in phenol polyethenoxy ether -10 and NPE.Can be in magnetic agitation or bubbling shape
Above-mentioned etching process is carried out under state, is beneficial to the uniformity of etching.
The metallic of the polysilicon chip remained on surface after being etched in S400, removing step S300, is carried out afterwards
Clean and dry, obtain the polysilicon chip after black silicon etching.
In one preferably embodiment, the behaviour of the metallic of the polysilicon chip remained on surface after etching is removed
In work:Metallic is gold particle, and the polysilicon chip after etching is entered with the mixed solution of iodine using KI
Row is cleaned to remove the gold particle of the polysilicon chip remained on surface after etching, and maintenance reaction temperature is 20 DEG C
~30 DEG C, the maintenance reaction time is 1min~3min;
In the mixed solution of KI and iodine, the mass fraction of KI is 19%, and the mass fraction of iodine is
4.76%.
Certainly, if metallic is other particles, according to the corresponding cleaning solution of different metal particle selection
Polysilicon chip after etching is cleaned.
The black silicon etching method of above-mentioned Buddha's warrior attendant wire cutting polysilicon chip, first puts pretreated polysilicon chip
Enter and carry out metal particle deposition in metal inducement catalytic reaction liquid, as a result of metal inducement catalytic reaction liquid,
Metallic can be evenly dispersed in silicon chip surface.Reaction, energy are performed etching after deposited metal particle again
Enough separate the etching solutions such as metal inducement catalytic reaction liquid and hydrogen peroxide, hydrofluoric acid, nitric acid, it is to avoid play
The metallic agglomeration that strong reaction zone comes, reduces the waste of noble metal, and it is uneven to avoid etching
The generation of phenomenon.Final polysilicon chip surface can obtain preferable nanometer suede, and this kind of matte can be reduced effectively
The reflectivity on polysilicon chip surface, promotes the raising of battery efficiency.Additionally, the method is simple to operate, cost
It is relatively low, and metallic is uniformly dispersed, it is adaptable to the making herbs into wool of large-area polycrystalline silicon chip.
It is below specific embodiment (by taking golden nanometer particle as an example):
Polysilicon after Buddha's warrior attendant wire cutting is put into HF (49%) and HNO3(65%) it is according to volume ratio
1:In 3 mixed solution, 5 DEG C~10 DEG C of maintenance reaction temperature, after being pre-processed after reaction time 2min
Polysilicon chip.
Test above-mentioned pretreated polysilicon chip and cut the polysilicon chip after the low-kappa number of polysilicon chip with mortar
Reflectivity, as a result as shown in Figure 6.Polysilicon after Buddha's warrior attendant wire cutting polysilicon chip is pre-processed
Piece is referred to as " diamond wire piece ", and mortar is cut the polysilicon chip referred to as " sand after the low-kappa number of polysilicon chip
Lodicule ".A represents the reflectivity of " diamond wire piece " in figure, and B represents the reflectivity of " mortar piece " in figure.
From fig. 6, it can be seen that the reflectivity of " diamond wire piece " shows cutting side more than the reflectivity of " mortar piece "
Method generates certain influence to the reflectivity of polysilicon chip, and is carried out for Buddha's warrior attendant wire cutting polysilicon chip pre-
Polysilicon chip after treatment, is processed by traditional sour making herbs into wool and is extremely difficult to the low effect of reflectivity.
By in gold chloride addition deionized water, the aqueous solution of gold chloride is obtained after mixing.By hydrofluoric acid, double
Oxygen water and ethanol are mixed, and are cooled to 15 DEG C, under magnetic agitation state, are added dropwise over a certain amount of gold chloride
The aqueous solution, continues to stir, and metal inducement catalytic reaction liquid is obtained after mixing.Metal inducement catalytic reaction liquid
In, the volume fraction of hydrofluoric acid, hydrogen peroxide and ethanol isoreactivity agent is respectively 1%, 0.5% and 0.5%.
" diamond wire piece " is placed on the reaction support of PVDF materials vertically, then the two is put into together
In stating metal inducement catalytic reaction liquid.As shown in fig. 7, reaction unit 100 is including reaction vessels 110 and instead
Support 120 is answered, " diamond wire piece " 200 is placed on reaction support 120 vertically.After reaction 90s, rapidly will
" diamond wire piece " and reaction support propose liquid level together, obtain the post-depositional polysilicon chip of gold particle.To upper
Stating the post-depositional polysilicon chip of gold particle carries out SEM tests, obtains Fig. 8.As can be seen from Figure 8, this
When the uniformly dispersing gold nano little particle of polysilicon chip sample surfaces.
The above-mentioned silicon chip sample for being dispersed through uniform gold nano grain is put into hydrofluoric acid, hydrogen peroxide and second
In the etching solution of alcohol isoreactivity agent.The volume of hydrofluoric acid, hydrogen peroxide and ethanol isoreactivity agent in etching solution
Fraction is respectively 25%, 15% and 15%.Under magnetic agitation or bubbling state, controlling reaction temperature is 10 DEG C
~15 DEG C, the reaction time is 15min, the polysilicon chip after being etched.
By the polysilicon chip after above-mentioned etching in KI and I2Mixed solution in cleaned, it is therefore an objective to remove residual
Stay in the gold grain of silicon chip surface.Wherein, I24.76% and 19% are respectively with the mass fraction of KI.Control
Reaction temperature is 20 DEG C~30 DEG C, and the reaction time is 3min, now obtains the black silicon sample of one-level.
The above-mentioned silicon chip sample for cleaning up is put into carries out alkali cleaning treatment in KOH solution, control reaction temperature
It is 50 DEG C~70 DEG C to spend, and the reaction time is 25s.
Finally, the sample that will be obtained is cleaned up with pure water, obtains being applied to two grades of black silicon suedes of solar cell
Face.SEM tests are carried out to above-mentioned two grades black silicon mattes, pattern is as shown in Figure 9.
Test now " diamond wire piece " and be applied to the reflectivity of " the mortar piece " of solar cell, as a result such as
Shown in Figure 10.C represents the reflectivity of " diamond wire piece " in figure, and D represents the reflection of " mortar piece " in figure
Rate.Figure 10 and Fig. 6 before is compared and be can be seen that first, " diamond wire piece " and " mortar piece "
The reflectivity of the two is below only carrying out pretreated sample, secondly, by a series of above-mentioned treatment after,
The reflectivity of " diamond wire piece " is far below the reflectivity of " mortar piece ", therefore, " diamond wire piece " is more favourable
In commercial Application, be conducive to improving the efficiency of correspondence solar cell.
After two grades of black silicon matte pieces are carried out into conventional batteries preparation method, diamond wire multi-wafer obtains the effect of battery
Rate significantly improves about 0.1%~0.5% than the efficiency of the battery of gained after classical acid making herbs into wool.
Each technical characteristic of embodiment described above can be combined arbitrarily, not right to make description succinct
The all possible combination of each technical characteristic in above-described embodiment is all described, as long as however, these skills
The combination of art feature does not exist contradiction, is all considered to be the scope of this specification record.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed,
But can not therefore be construed as limiting the scope of the patent.It should be pointed out that for this area
For those of ordinary skill, without departing from the inventive concept of the premise, some deformations can also be made and changed
Enter, these belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with appended power
Profit requires to be defined.
Claims (10)
1. a kind of metal inducement catalytic reaction liquid, it is characterised in that by the following each component according to volume parts
Composition:
The acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.
2. metal inducement catalytic reaction liquid according to claim 1, it is characterised in that by according to volume
The following each group of number is grouped into:
3. metal inducement catalytic reaction liquid according to claim 1, it is characterised in that the hydrofluoric acid
It is 3 with the volume ratio of the hydrogen peroxide:1~1:10.
4. metal inducement catalytic reaction liquid according to claim 1, it is characterised in that the nonionic
Surfactant is selected from ethanol, ethylene glycol, polyethylene glycol, Tween-60, Tween-80, octyl phenol polyoxyethylene
At least one in ether -10 and NPE.
5. metal inducement catalytic reaction liquid according to claim 1, it is characterised in that the source metal
Selected from the one kind in gold chloride, chloroplatinic acid, silver nitrate or copper nitrate.
6. metal inducement catalytic reaction liquid according to claim 1, it is characterised in that the deionization
The electrical conductivity of water is less than 0.5 μ S/cm.
7. a kind of preparation method of metal inducement catalytic reaction liquid, it is characterised in that comprise the following steps:
By in source metal addition deionized water, the aqueous solution of source metal is obtained after mixing;
Acidic cleaner and nonionic surfactant are mixed, 5 DEG C~15 DEG C are cooled to, is added dropwise over afterwards
The aqueous solution of the source metal, obtains metal inducement catalytic reaction liquid after mixing;
The acidic cleaner is selected from the mixed solution of hydrofluoric acid and hydrogen peroxide.
8. a kind of black silicon etching method of Buddha's warrior attendant wire cutting polysilicon chip, it is characterised in that comprise the following steps:
Polysilicon chip after Buddha's warrior attendant wire cutting is pre-processed to remove damage layer, is obtained pretreated many
Crystal silicon chip;
In the metal inducement catalytic reaction liquid that the pretreated polysilicon chip is put into described in claim 1,
Maintain to be taken out after 15s~90s, obtain the polysilicon chip after metal particle deposition;
Polysilicon chip after the metal particle deposition is put into etching solution and is performed etching, after being etched
Polysilicon chip;
The metallic of the polysilicon chip remained on surface after the etching is removed, is cleaned afterwards and is dried,
Obtain the polysilicon chip after black silicon etching.
9. the black silicon etching method of Buddha's warrior attendant wire cutting polysilicon chip according to claim 8, its feature exists
In, in the metal inducement catalytic reaction liquid that the pretreated polysilicon chip is put into described in claim 1,
Maintain to be taken out after 15s~90s, the operation for obtaining the polysilicon chip after metal particle deposition is:
Support is provided, for supporting the pretreated polysilicon chip, the material of the support is polytetrafluoro
Ethene;
The pretreated polysilicon chip is put on the bracket, by the pretreated polysilicon chip
It is put into together with the support in the metal inducement catalytic reaction liquid described in claim 1, after the pretreatment
Polysilicon chip surface where plane perpendicular to the plane where the metal inducement catalytic reaction liquid;
Maintain to be taken out after 15s~90s, obtain the polysilicon chip after metal particle deposition.
10. the black silicon etching method of Buddha's warrior attendant wire cutting polysilicon chip according to claim 8, its feature
It is that the polysilicon chip after the metal particle deposition is put into the operation performed etching in etching solution,
It is 5 DEG C~15 DEG C to maintain etching temperature, and maintenance etch period is 2min~15min, and the etching solution includes pressing
According to the following each component of volume parts:
The nonionic surfactant be selected from ethanol, ethylene glycol, polyethylene glycol, Tween-60, Tween-80,
At least one in OPEO -10 and NPE.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107265398A (en) * | 2017-06-15 | 2017-10-20 | 西南交通大学 | The silicon that is etched based on mechanical scratching and metal catalytic is micro-/micro-nano structure preparation method |
CN108133968A (en) * | 2017-12-27 | 2018-06-08 | 南京理工大学 | Utilize the method for pine structural porous copper auxiliary etch taper array silicon face |
CN114203855A (en) * | 2020-09-18 | 2022-03-18 | 苏州阿特斯阳光电力科技有限公司 | Silicon wafer composite suede manufacturing method and silicon wafer manufactured by same |
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CN104962998A (en) * | 2015-07-08 | 2015-10-07 | 中国科学院宁波材料技术与工程研究所 | Diamond wire cutting-based silicon wafer texturing pretreatment method and silicon wafer texturing method |
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CN104576830A (en) * | 2014-12-30 | 2015-04-29 | 江西赛维Ldk太阳能高科技有限公司 | Texturing pretreatment liquid and texturing pretreatment method for diamond wire cutting polycrystalline silicon sheet, texturing pretreatment silicon sheet and application of texturing pretreatment silicon sheet |
CN104962998A (en) * | 2015-07-08 | 2015-10-07 | 中国科学院宁波材料技术与工程研究所 | Diamond wire cutting-based silicon wafer texturing pretreatment method and silicon wafer texturing method |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107265398A (en) * | 2017-06-15 | 2017-10-20 | 西南交通大学 | The silicon that is etched based on mechanical scratching and metal catalytic is micro-/micro-nano structure preparation method |
CN108133968A (en) * | 2017-12-27 | 2018-06-08 | 南京理工大学 | Utilize the method for pine structural porous copper auxiliary etch taper array silicon face |
CN114203855A (en) * | 2020-09-18 | 2022-03-18 | 苏州阿特斯阳光电力科技有限公司 | Silicon wafer composite suede manufacturing method and silicon wafer manufactured by same |
CN114551614A (en) * | 2020-11-24 | 2022-05-27 | 苏州阿特斯阳光电力科技有限公司 | Silicon wafer composite suede manufacturing method and silicon wafer manufactured by same |
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