CN109192818A - A kind of method that evening chemical corrosion prepares polycrystalline silicon suede - Google Patents
A kind of method that evening chemical corrosion prepares polycrystalline silicon suede Download PDFInfo
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- CN109192818A CN109192818A CN201811046783.1A CN201811046783A CN109192818A CN 109192818 A CN109192818 A CN 109192818A CN 201811046783 A CN201811046783 A CN 201811046783A CN 109192818 A CN109192818 A CN 109192818A
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- polycrystalline silicon
- corrosion
- film
- silicon suede
- polysilicon chip
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 71
- 230000007797 corrosion Effects 0.000 title claims abstract description 56
- 238000005260 corrosion Methods 0.000 title claims abstract description 56
- 239000000126 substance Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229920005591 polysilicon Polymers 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000005662 Paraffin oil Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- 239000011347 resin Substances 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- 239000004809 Teflon Substances 0.000 claims description 14
- 229920006362 Teflon® Polymers 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 8
- 238000005056 compaction Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 150000002170 ethers Chemical class 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 8
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 229920006361 Polyflon Polymers 0.000 abstract description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 3
- 239000011737 fluorine Substances 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000001579 optical reflectometry Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 210000004027 cell Anatomy 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 238000003303 reheating Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 235000014653 Carica parviflora Nutrition 0.000 description 3
- 241000243321 Cnidaria Species 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 210000004483 pasc Anatomy 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000012546 transfer Methods 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 System
- H01L31/182—Special manufacturing methods for polycrystalline Si, e.g. Si ribbon, poly Si ingots, thin films of polycrystalline Si
-
- 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
- Y02E10/546—Polycrystalline 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
Abstract
The present invention relates to a kind of methods that evening chemical corrosion prepares polycrystalline silicon suede, belong to solar energy materials preparation technical field.High speed dispersion obtains mixture after the present invention first mixes polyflon and fluorine-containing surfactant and paraffin oil, continue green compact after mixture is compacted with compacting machine again, blank stretching-machine biaxial tension is formed a film, obtained film coated will be stretched in polysilicon chip surface, acidizing corrosion is carried out to the polysilicon chip of film coated under high pressure with chemistry acid corrosion liquid again, take off film after the completion up to the uniform polycrystalline silicon suede in surface, polycrystalline silicon suede surface corrosion produced by the present invention is uniform, it is low to sun light reflectivity, utilization rate is high, photoelectric conversion performance is good, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of methods that evening chemical corrosion prepares polycrystalline silicon suede, belong to solar energy materials technology of preparing
Field.
Background technique
Crystal-silicon solar cell (including monocrystalline silicon battery and polycrystal silicon cell) is due to its mature production technology and excellent
Photoelectric conversion performance, firmly in occupation of the leading position of international photovoltaic market, in the process of research polycrystalline silicon solar cell
In, people have found some key technologies for influencing battery efficiency, including rapid thermal treatment, basis material impurity are absorbed, surface
Passivation and body passivation and surface-texturing etc., only have surface-texturing not to be well solved in this several technologies, and
Other several technologies all comparative maturities, all large-scale application in industrialized production.In the production technology of solar cell,
Surface-texturing plays an important role in terms of reducing reflection, one is reaching drop and collecting surface reflection again
The effect of low surface reflection loss；Light is trapped in inside battery the second is being reflected by internally reflective.
The existing flannelette for preparing crystal silicon solar energy battery, the most common are chemical acid corrosion methods, with acid corrosion legal system
Standby polycrystalline silicon suede out is pure chemistry reaction, chemical acid corrosion polycrystalline there is also apparent defect, mainly acid corrosion method
Pasc reaction is exothermic reaction, and reaction is not easy to control, and the reaction time is longer, reacts more not easy to control,
The not high polycrystalline silicon suede surface resulted in of reaction stability is uneven, influences reflectivity.
Therefore, invent that a kind of stable reaction is controllable, the preparation method of the uniform polycrystalline silicon suede material of surface corrosion has
Positive meaning.
Summary of the invention
Present invention mainly solves the technical issues of, during preparing polycrystalline silicon suede for current chemical corrosion method, change
Acid corrosion reaction stability and poor controllability are learned, the polycrystalline silicon suede surface resulted in is uneven, and influencing polycrystalline silicon suede makes
With the defect of performance, a kind of method that evening chemical corrosion prepares polycrystalline silicon suede is provided.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of method that evening chemical corrosion prepares polycrystalline silicon suede, it is characterised in that specific preparation step are as follows:
(1) high speed point is packed into after mixing teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5 and paraffin oil
It dissipates in machine, then dehydrated alcohol is added into high speed disperser, be dispersed with stirring, obtain disperse materials；
(2) above-mentioned disperse materials are put into vacuum oven, vacuum drying treatment obtains mixture, by mixture compacting machine pressure
Real 1~2min obtains compacting blank；
(3) by above-mentioned compacting blank in being put into three-roller calendar, 10~15min is first preheated at 80~90 DEG C, is reheated and is risen
For temperature to 110~120 DEG C, heat preservation compacting obtains sheet material, then by sheet material with stretching-machine biaxial tension at film, controlling stretching ratio is
5 times, 5~10min is stood at 180~190 DEG C after film is stretched to 5 multiplying powers；
(4) to above-mentioned standing after at once by film tiling be wrapped in polysilicon chip surface, obtain pretreatment polysilicon chip, will
The hydrofluoric acid and mass fraction of mass fraction 49% are that 65% nitric acid solution and deionized water mix, it is stirred at room temperature 25~
30min obtains chemical acid corrosion liquid；
(5) above-mentioned pretreatment polysilicon chip is lain in into polytetrafluoroethyllining lining stainless steel cauldron bottom, then into reaction kettle
Above-mentioned chemical acid corrosion liquid is added until submergence pretreatment polysilicon chip, is forced into 2.0~2.2MPa to reaction kettle after sealing, acid
Polysilicon chip is taken out after changing corrosion, is removed after the film on surface up to polycrystalline silicon suede.
Teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5's and paraffin oil as described in step (1)
Mass ratio is 10:1:1, and the additional amount of dehydrated alcohol is equal with teflon resin powder quality, and the revolving speed being dispersed with stirring is
1000~1200r/min, the time being dispersed with stirring are 30~40min.
The temperature of vacuum drying treatment described in step (2) is 70~80 DEG C, time 20 of vacuum drying treatment~
30min, the compaction velocity of compacting machine are 70~80mm/min, and the compaction pressure of compacting machine is 3~4MPa.
Sheet material described in step (3) with a thickness of 0.3~0.5mm.
The hydrofluoric acid and mass fraction of mass fraction 49% described in step (4) are 65% nitric acid solution and deionized water
Mass ratio 2:3:3.
The temperature of acidizing corrosion described in step (5) is 60~70 DEG C, and the time of acidizing corrosion is 8~10min.
The beneficial effects of the present invention are:
(1) high speed dispersion obtains after the present invention first mixes polyflon and fluorine-containing surfactant and paraffin oil
Mixture, then continue green compact after mixture is compacted with compacting machine, blank stretching-machine biaxial tension is formed a film, stretching is obtained
Film coated the polysilicon chip of film coated is carried out under high pressure in polysilicon chip surface, then with chemical acid corrosion liquid
Acidizing corrosion takes off film after the completion up to the uniform polycrystalline silicon suede in surface, and the present invention is raw material, benefit using polyflon
There is unique phase structure with polyflon particle, by zonal growth structure it is closely knit be folded into spherical particle, it is this
Banded structure is easy to be pulled out from graininess, and therefore, polyflon is under extrusion, calendering, drawing process, band-like knot
Structure is pulled out from branch particle, forms the particle fiber parallel with draw direction, and the resin being not stretched gets together to be formed
Knot, with the increase of stretching ratio, there is node and fibrous structure in polytetrafluoroethylene film, and microcellular structure is also gradually obvious,
The microcellular structure of film is gradually uniform, and when stretching ratio reaches 5 times, the microcellular structure uniformity of polytetrafluoroethylene film is most
Height finally obtains the film of class lattice coral structure, is coated on polysilicon chip surface for this film is smooth, then with chemical acid corrosion liquid leaching
Bubble corrosion, since the generation of polytetrafluoroethylene film micropore during stretching is so that the fluorine-containing surfactant of doping is again sudden and violent
Dew reduces the wettability at micropore, and under high pressure effect chemical acid corrosion liquid is entered from the micropore of class lattice coral film
Infiltration corrodes polysilicon surface, and since polytetrafluoroethylene (PTFE) acid resistance itself is splendid, chemical acid corrosion liquid can only be from thin
Corrosion is infiltrated in membrane micropore, and cannot be then corroded at film node, is realized using the class uniform pore structure of lattice coral film
The uniformity of polysilicon surface corrosion, finally obtains the uniform polycrystalline silicon suede of surface corrosion, reduces polycrystalline silicon suede to too
The reflection of sunlight improves its service performance, has broad application prospects.
Specific embodiment
It is in mass ratio 10:1:1 by teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5 and paraffin
It is fitted into high speed disperser after oil mixing, then the anhydrous second of the quality such as teflon resin powder is added into high speed disperser
Alcohol is dispersed with stirring 30~40min with the revolving speed of 1000~1200r/min, obtains disperse materials；Disperse materials are put into vacuum oven
In, 70~80 DEG C are heated to, 20~30min of vacuum drying treatment obtains mixture, by mixture compacting machine to be compacted
It is compacted 1~2min under conditions of rate is 70~80mm/min, compaction pressure is 3~4MPa and obtains compacting blank；Base will be suppressed
Material first preheats 10~15min in being put into three-roller calendar at 80~90 DEG C, and reheating is warming up to 110~120 DEG C, heat preservation
Compacting obtains with a thickness of the sheet material of 0.3~0.5mm thickness, then by sheet material with stretching-machine biaxial tension at film, control stretching ratio
It is 5 times, stands 5~10min at 180~190 DEG C after film is stretched to 5 multiplying powers；Film is put down at once after wait stand
Paving is wrapped in polysilicon chip surface, obtains pretreatment polysilicon chip, 2:3:3 in mass ratio by the hydrofluoric acid of mass fraction 49% and
Mass fraction is that 65% nitric acid solution and deionized water mix, and 25~30min is stirred at room temperature, obtains chemical acid corrosion liquid；
Pretreatment polysilicon chip is lain in into polytetrafluoroethyllining lining stainless steel cauldron bottom, then above-mentioned chemistry is added into reaction kettle
Acid corrosion liquid is forced into 2.0~2.2MPa to reaction kettle after sealing until submergence pretreatment polysilicon chip, and temperature be 60~
Polysilicon chip is taken out after 8~10min of acidizing corrosion at 70 DEG C, is removed after the film on surface up to polycrystalline silicon suede.
It is in mass ratio 10:1:1 by teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5 and paraffin
It is fitted into high speed disperser after oil mixing, then the anhydrous second of the quality such as teflon resin powder is added into high speed disperser
Alcohol is dispersed with stirring 30min with the revolving speed of 1000r/min, obtains disperse materials；Disperse materials are put into vacuum oven, heating rises
For temperature to 70 DEG C, vacuum drying treatment 20min obtains mixture, with compaction velocity is 70mm/min by mixture compacting machine, pressure
Compacting 1min obtains compacting blank under conditions of real pressure is 3MPa；By compacting blank in being put into three-roller calendar, first 80
10min is preheated at DEG C, reheating is warming up to 110 DEG C, and heat preservation compacting obtains with a thickness of the sheet material of 0.3mm thickness, then sheet material is drawn
Machine biaxial tension is stretched into film, and controlling stretching ratio is 5 times, stands 5min at 180 DEG C after film is stretched to 5 multiplying powers；To
Film tiling is wrapped in polysilicon chip surface at once after standing, obtains pretreatment polysilicon chip, 2:3:3 in mass ratio will
The hydrofluoric acid and mass fraction of mass fraction 49% are that 65% nitric acid solution and deionized water mix, and 25min is stirred at room temperature,
Obtain chemical acid corrosion liquid；Pretreatment polysilicon chip is lain in into polytetrafluoroethyllining lining stainless steel cauldron bottom, then to anti-
It answers and above-mentioned chemical acid corrosion liquid is added in kettle until submerging pretreatment polysilicon chip, 2.0MPa is forced into reaction kettle after sealing,
And polysilicon chip is taken out after acidizing corrosion 8min in temperature being 60 DEG C, it removes after the film on surface up to polycrystalline silicon suede.
It is in mass ratio 10:1:1 by teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5 and paraffin
It is fitted into high speed disperser after oil mixing, then the anhydrous second of the quality such as teflon resin powder is added into high speed disperser
Alcohol is dispersed with stirring 35min with the revolving speed of 1100r/min, obtains disperse materials；Disperse materials are put into vacuum oven, heating rises
For temperature to 75 DEG C, vacuum drying treatment 25min obtains mixture, with compaction velocity is 75mm/min by mixture compacting machine, pressure
Compacting 2min obtains compacting blank under conditions of real pressure is 3MPa；By compacting blank in being put into three-roller calendar, first 85
13min is preheated at DEG C, reheating is warming up to 115 DEG C, and heat preservation compacting obtains with a thickness of the sheet material of 0.4mm thickness, then sheet material is drawn
Machine biaxial tension is stretched into film, and controlling stretching ratio is 5 times, stands 8min at 185 DEG C after film is stretched to 5 multiplying powers；To
Film tiling is wrapped in polysilicon chip surface at once after standing, obtains pretreatment polysilicon chip, 2:3:3 in mass ratio will
The hydrofluoric acid and mass fraction of mass fraction 49% are that 65% nitric acid solution and deionized water mix, and 28min is stirred at room temperature,
Obtain chemical acid corrosion liquid；Pretreatment polysilicon chip is lain in into polytetrafluoroethyllining lining stainless steel cauldron bottom, then to anti-
It answers and above-mentioned chemical acid corrosion liquid is added in kettle until submerging pretreatment polysilicon chip, 2.1MPa is forced into reaction kettle after sealing,
And polysilicon chip is taken out after acidizing corrosion 9min in temperature being 65 DEG C, it removes after the film on surface up to polycrystalline silicon suede.
It is in mass ratio 10:1:1 by teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5 and paraffin
It is fitted into high speed disperser after oil mixing, then the anhydrous second of the quality such as teflon resin powder is added into high speed disperser
Alcohol is dispersed with stirring 40min with the revolving speed of 1200r/min, obtains disperse materials；Disperse materials are put into vacuum oven, heating rises
For temperature to 80 DEG C, vacuum drying treatment 30min obtains mixture, with compaction velocity is 80mm/min by mixture compacting machine, pressure
Compacting 2min obtains compacting blank under conditions of real pressure is 4MPa；By compacting blank in being put into three-roller calendar, first 90
15min is preheated at DEG C, reheating is warming up to 120 DEG C, and heat preservation compacting obtains with a thickness of the sheet material of 0.5mm thickness, then sheet material is drawn
Machine biaxial tension is stretched into film, and controlling stretching ratio is 5 times, stands 10min at 190 DEG C after film is stretched to 5 multiplying powers；To
Film tiling is wrapped in polysilicon chip surface at once after standing, obtains pretreatment polysilicon chip, 2:3:3 in mass ratio will
The hydrofluoric acid and mass fraction of mass fraction 49% are that 65% nitric acid solution and deionized water mix, and 30min is stirred at room temperature,
Obtain chemical acid corrosion liquid；Pretreatment polysilicon chip is lain in into polytetrafluoroethyllining lining stainless steel cauldron bottom, then to anti-
It answers and above-mentioned chemical acid corrosion liquid is added in kettle until submerging pretreatment polysilicon chip, 2.2MPa is forced into reaction kettle after sealing,
And polysilicon chip is taken out after acidizing corrosion 10min in temperature being 70 DEG C, it removes after the film on surface up to polycrystalline silicon suede.
Reference examples are using polycrystalline silicon suede prepared by general chemistry acid corrosion method as reference examples
Performance detection, testing result such as table 1 are carried out to the polycrystalline silicon suede in polycrystalline silicon suede produced by the present invention and reference examples
It is shown:
1 performance test results of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Corrosion depth (μm) | 3.10 | 3.02 | 2.98 | 4.58 |
| Sun light reflectivity (%) | 10.35 | 10.21 | 10.05 | 26.32 |
| Charge transfer resistance (Ω) | 720 | 715 | 708 | 950 |
Polycrystalline silicon suede surface corrosion produced by the present invention is uniform it can be seen from detection data in upper table, reflects sunlight
Rate is low, and utilization rate is high, and photoelectric conversion performance is good, has broad application prospects.
Claims (6)
1. a kind of method that evening chemical corrosion prepares polycrystalline silicon suede, it is characterised in that specific preparation step are as follows:
(1) high speed point is packed into after mixing teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5 and paraffin oil
It dissipates in machine, then dehydrated alcohol is added into high speed disperser, be dispersed with stirring, obtain disperse materials；
(2) above-mentioned disperse materials are put into vacuum oven, vacuum drying treatment obtains mixture, by mixture compacting machine pressure
Real 1~2min obtains compacting blank；
(3) by above-mentioned compacting blank in being put into three-roller calendar, 10~15min is first preheated at 80~90 DEG C, is reheated and is risen
For temperature to 110~120 DEG C, heat preservation compacting obtains sheet material, then by sheet material with stretching-machine biaxial tension at film, controlling stretching ratio is
5 times, 5~10min is stood at 180~190 DEG C after film is stretched to 5 multiplying powers；
(4) to above-mentioned standing after at once by film tiling be wrapped in polysilicon chip surface, obtain pretreatment polysilicon chip, will
The hydrofluoric acid and mass fraction of mass fraction 49% are that 65% nitric acid solution and deionized water mix, it is stirred at room temperature 25~
30min obtains chemical acid corrosion liquid；
(5) above-mentioned pretreatment polysilicon chip is lain in into polytetrafluoroethyllining lining stainless steel cauldron bottom, then into reaction kettle
Above-mentioned chemical acid corrosion liquid is added until submergence pretreatment polysilicon chip, is forced into 2.0~2.2MPa to reaction kettle after sealing, acid
Polysilicon chip is taken out after changing corrosion, is removed after the film on surface up to polycrystalline silicon suede.
2. the method that a kind of evening chemical corrosion according to claim 1 prepares polycrystalline silicon suede, it is characterised in that: step
(1) mass ratio of teflon resin powder and perfluoroalkyl ethers carboxylic acid potassium salt FC-5 and paraffin oil described in is 10:
The additional amount of 1:1, dehydrated alcohol are equal with teflon resin powder quality, and the revolving speed being dispersed with stirring is 1000~1200r/
Min, the time being dispersed with stirring are 30~40min.
3. the method that a kind of evening chemical corrosion according to claim 1 prepares polycrystalline silicon suede, it is characterised in that: step
(2) temperature of the vacuum drying treatment described in is 70~80 DEG C, 20~30min of time of vacuum drying treatment, compacting machine
Compaction velocity is 70~80mm/min, and the compaction pressure of compacting machine is 3~4MPa.
4. the method that a kind of evening chemical corrosion according to claim 1 prepares polycrystalline silicon suede, it is characterised in that: step
(3) sheet material described in a thickness of 0.3~0.5mm.
5. the method that a kind of evening chemical corrosion according to claim 1 prepares polycrystalline silicon suede, it is characterised in that: step
(4) hydrofluoric acid and mass fraction of the mass fraction 49% described in are the mass ratio 2:3 of 65% nitric acid solution and deionized water:
3。
6. the method that a kind of evening chemical corrosion according to claim 1 prepares polycrystalline silicon suede, it is characterised in that: step
(5) temperature of the acidizing corrosion described in is 60~70 DEG C, and the time of acidizing corrosion is 8~10min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811046783.1A CN109192818A (en) | 2018-09-08 | 2018-09-08 | A kind of method that evening chemical corrosion prepares polycrystalline silicon suede |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811046783.1A CN109192818A (en) | 2018-09-08 | 2018-09-08 | A kind of method that evening chemical corrosion prepares polycrystalline silicon suede |
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| CN201811046783.1A Pending CN109192818A (en) | 2018-09-08 | 2018-09-08 | A kind of method that evening chemical corrosion prepares polycrystalline silicon suede |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100117108A1 (en) * | 2006-09-28 | 2010-05-13 | X-Fab Semiconductor Foundries Ag | Uses of self-organized needle-type nanostructures |
| CN104785130A (en) * | 2015-04-23 | 2015-07-22 | 湖州绿净环保科技有限公司 | Hydrophilic biaxially-oriented polytetrafluoroethylene microporous membrane |
| CN104802429A (en) * | 2015-04-23 | 2015-07-29 | 湖州绿净环保科技有限公司 | Method for improving porosity rate of two-way stretching polytetrafluoroethylene micropore thin film |
| CN107342336A (en) * | 2017-06-28 | 2017-11-10 | 常州欣彬纺织品有限公司 | A kind of preparation method of isotypy polycrystalline silicon suede |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100117108A1 (en) * | 2006-09-28 | 2010-05-13 | X-Fab Semiconductor Foundries Ag | Uses of self-organized needle-type nanostructures |
| CN104785130A (en) * | 2015-04-23 | 2015-07-22 | 湖州绿净环保科技有限公司 | Hydrophilic biaxially-oriented polytetrafluoroethylene microporous membrane |
| CN104802429A (en) * | 2015-04-23 | 2015-07-29 | 湖州绿净环保科技有限公司 | Method for improving porosity rate of two-way stretching polytetrafluoroethylene micropore thin film |
| CN107342336A (en) * | 2017-06-28 | 2017-11-10 | 常州欣彬纺织品有限公司 | A kind of preparation method of isotypy polycrystalline silicon suede |
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Application publication date: 20190111 |