CN104393118B - The crystal silicon solar batteries Wet chemical processing method that making herbs into wool is carried out with cleaning substep - Google Patents
The crystal silicon solar batteries Wet chemical processing method that making herbs into wool is carried out with cleaning substep Download PDFInfo
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- CN104393118B CN104393118B CN201410722696.9A CN201410722696A CN104393118B CN 104393118 B CN104393118 B CN 104393118B CN 201410722696 A CN201410722696 A CN 201410722696A CN 104393118 B CN104393118 B CN 104393118B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 199
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 199
- 239000010703 silicon Substances 0.000 title claims abstract description 199
- 238000004140 cleaning Methods 0.000 title claims abstract description 132
- 238000000034 method Methods 0.000 title claims abstract description 63
- 210000002268 wool Anatomy 0.000 title claims abstract description 55
- 235000008216 herbs Nutrition 0.000 title claims abstract description 54
- 239000013078 crystal Substances 0.000 title claims abstract description 25
- 238000012993 chemical processing Methods 0.000 title claims abstract description 9
- 239000012530 fluid Substances 0.000 claims abstract description 100
- 239000007788 liquid Substances 0.000 claims abstract description 54
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 25
- 239000012535 impurity Substances 0.000 claims abstract description 20
- 238000005498 polishing Methods 0.000 claims abstract description 20
- 238000002203 pretreatment Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 8
- 238000005422 blasting Methods 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- 238000012545 processing Methods 0.000 claims description 41
- 239000011259 mixed solution Substances 0.000 claims description 40
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 36
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 239000000126 substance Substances 0.000 claims description 23
- 238000005260 corrosion Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 14
- 230000005661 hydrophobic surface Effects 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 230000007797 corrosion Effects 0.000 claims description 9
- 230000005587 bubbling Effects 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 238000002161 passivation Methods 0.000 claims description 6
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000003667 anti-reflective effect Effects 0.000 abstract description 5
- 230000003749 cleanliness Effects 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 238000005530 etching Methods 0.000 description 6
- 238000002310 reflectometry Methods 0.000 description 6
- 239000000428 dust Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- 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
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
-
- 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
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1868—Passivation
-
- 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
-
- 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)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Photovoltaic Devices (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention discloses a kind of crystal silicon solar batteries Wet chemical processing method making herbs into wool carried out with cleaning substep, the step of the method is as follows: (1) provides a silicon chip after pre-treatment；(2) use the first cleaning fluid that silicon chip is carried out prerinse, to remove silicon chip surface particle impurity and pollution；(3) use polishing etch liquid that silicon chip is processed by shot blasting, erode the mechanical damage layer on surface；(4) use Woolen-making liquid that silicon chip is carried out making herbs into wool process so that it is surface forms suede structure；(5) use the second cleaning fluid that silicon chip is carried out, to remove surface metal ion, and neutralize alkaline impurities, reduce surface chemistry residual；(6) use oxide etch liquid that silicon chip is processed, to remove removing oxide layer, and form hydrophobic drying structure on its surface.After making herbs into wool of the present invention, silicon chip can be with long storage time, and its surface cleanliness and anti-reflective effect have reached higher level, greatly reduce the production time, improve production efficiency.
Description
Technical field
The present invention relates to a kind of crystal silicon solar batteries Wet chemical processing method making herbs into wool carried out with cleaning substep.
Background technology
At present, existing crystal silicon solar batteries Wet chemical processing method is typically pre-processed by silicon chip, polishing, making herbs into wool, RCA
Clean, the technical process such as drying composition, time-consuming be about 2～3h, be link the slowest in cell piece preparation technology, seriously
Limiting production efficiency, after wet-chemical treatment, silicon wafer suede uniformity is poor, and " pyramid " physical dimension is relatively big,
Anti-reflective effect is general, and during making herbs into wool, the residual liquor of silicon chip, the gaily decorated basket etc. is easily brought in cleaning process, causes solution dirty
Dye, cleaning fluid reduces service life, the problems such as cleaning performance is impacted.
Summary of the invention
The technical problem to be solved is the defect overcoming prior art, it is provided that making herbs into wool is entered by one with cleaning substep
The crystal silicon solar batteries Wet chemical processing method of row, after its making herbs into wool, silicon chip can be with long storage time, and its clean surface
Degree and anti-reflective effect have reached higher level, greatly reduce the production time, improve production efficiency.
In order to solve above-mentioned technical problem, the technical scheme is that a kind of crystal silicon making herbs into wool carried out with cleaning substep
Solar cell Wet chemical processing method, the step of the method is as follows:
(1) silicon chip after pre-treatment is provided；Pre-treatment is: is put into by the silicon chip being contained in the gaily decorated basket in pure water and soaks
Profit overflow, rinses 1-10min, removes dust etc..Pure water resistivity is 10-18M Ω；
(2) use the first cleaning fluid that silicon chip is carried out prerinse, to remove silicon chip surface particle impurity and pollution；
(3) use polishing etch liquid that silicon chip is processed by shot blasting, erode the mechanical damage layer on surface；
(4) use Woolen-making liquid that silicon chip is carried out making herbs into wool process so that it is surface forms suede structure；
(5) use the second cleaning fluid that silicon chip is carried out, to remove surface metal ion, and neutralize alkaline impurities,
Reduce surface chemistry residual；
(6) use oxide etch liquid that silicon chip is processed, to remove removing oxide layer, and form hydrophobic being dried on its surface
Structure；
(7) silicon chip surface is carried out oxidation-corrosion treatmentCorrosion Science repeatedly；
(8) use the 3rd cleaning fluid that silicon chip is carried out, to remove surface particles impurity, carry out chemistry neutralization；
(9) the 4th cleaning fluid is finally used silicon chip to be carried out, to remove removing oxide layer and surface metal ion, simultaneously
Form the hydrophobic surface of passivation, complete crystal silicon solar batteries wet-chemical treatment.
The anti-reflective effect of matte is not affected, in described step (6) and step (7) further as its holding time
Further comprise the steps of: and silicon chip is put into drying cupboard deposit.
Further, in described step (2), the described mixing that the first cleaning fluid is NaOH and hydrogen peroxide is molten
Liquid；And wherein, the mass percentage concentration of NaOH is 0.1%～3%, and the mass percentage concentration of hydrogen peroxide is
1%～10%.
Further, described step (2) is particularly as follows: put into the silicon chip after pre-treatment and carry out 1～5min in the first cleaning fluid
Prerinse, temperature controls at 50-80 DEG C；Then it is rinsed processing with pure water.
Further, in described step (3), described polishing etch liquid be mass percentage concentration be 10%～50%
NaOH.
Further, described step (3) is particularly as follows: be placed in silicon chip in polishing etch liquid, and it is 60 DEG C～100 that temperature controls
DEG C, eroding the mechanical damage layer that silicon chip is formed in slicing processes, the reaction time is 1～10min, and silicon chip every corrodes
3～20um；Then it is rinsed processing with pure water.
Further, in described step (4), described Woolen-making liquid is that the mixing of NaOH and flocking additive is molten
Liquid；And wherein, the mass percentage concentration of NaOH is 0.5%～8%, and the mass percentage concentration of flocking additive is
0.5%～5%.
Further, described step (4) is particularly as follows: put into silicon chip in Woolen-making liquid and carry out making herbs into wool, and reaction temperature is 70～90
DEG C, the reaction time is 10～30min；Then it is rinsed processing with pure water.
Further, in described step (5), the second described cleaning fluid is SC2 cleaning fluid, this SC2 cleaning fluid
For HCL, H2O2And H2The mixed solution of O；And wherein, HCL, H2O2、H2The volume ratio of O is 1:(1～3):
(10～15).
Further, described step (5), particularly as follows: silicon chip is placed in the second cleaning fluid process 3～10min, neutralizes
Silicon chip surface residual alkaline matter and metal ion；Then it is rinsed processing with pure water.
Further, in described step (6), described oxide etch liquid be mass percentage concentration be 0.5%～5%
Hydrofluoric acid solution.
Further, in described step (7), at HF and HNO3Mixed solution in silicon chip surface is carried out repeatedly
Oxidation-corrosion treatmentCorrosion Science；And wherein, HF and HNO3Volume ratio be 1:(50～100).
Further, described step (7) is particularly as follows: be placed in HF and HNO by silicon chip3Mixed solution in react 0.5～2
Min, increases bubbling or ultrasonically treated in solution；Then it is rinsed processing with pure water.
Further, in described step (8), the 3rd described cleaning fluid is SC1 mixing cleaning fluid, and this SC1 mixes
Conjunction cleaning fluid is NH4OH、H2O2And H2The mixed solution of O；And wherein, NH4OH、H2O2And H2The body of O
Long-pending ratio is: 1:(0.5～5): (10～15).
Further, described step (8) particularly as follows: put in the 3rd cleaning fluid that temperature is 60～80 DEG C anti-by silicon chip
Answer 1～10min；Then it is rinsed processing with pure water.
Further, in described step (9), the described mixed solution that the 4th cleaning fluid is hydrofluoric acid and hydrochloric acid；
And wherein, the mass percentage concentration of hydrofluoric acid is 0.5%～5%, and the mass percentage concentration of hydrochloric acid is 0.5%～5%.
Further, described step (9), particularly as follows: silicon chip is placed in the 4th cleaning fluid process 1～10min, is removed
Oxide layer and surface metal ion, and silicon chip surface is passivated, form hydrophobic surface；Then it is rinsed with pure water
Process.
After have employed technique scheme, wet chemical technology is divided into two sections and carries out by the present invention, i.e. making herbs into wool section and cleaning section,
Wherein making herbs into wool section uses specific etching method, forms uniform, fine and close small size " pyramid " structure at silicon chip surface
Matte, and can carry out the most in a large number, after making herbs into wool, silicon chip gets final product long storage time through simple process, takes out preservation according to need
Wafer Cleaning, its surface cleanliness, anti-reflective effect can reach higher level, and the wet chemical technology time is reduced to 1.5h
Left and right, improves production efficiency.Additionally, silicon chip forms hydrophobic dry surface, with this hydrophobic surface after making herbs into wool section processes
Enter cleaning section technique, be carried out liquid and clean, it is to avoid hydrophilic silicon chip causes not because of concentration difference in cleaning fluid
Uniformly etching, this wet chemical method, improve production efficiency, simplify technique, and can prevent solution cross pollution, with
The efficiency of hetero-junctions high performance solar batteries sheet prepared by this wet chemical method can reach 20%.
Accompanying drawing explanation
Fig. 1 is the process chart of the making herbs into wool section of the present invention；
Fig. 2 is the process chart of the cleaning section of the present invention；
Fig. 3 is the top view of the mechanical damage layer of the silicon chip surface of the present invention；
Fig. 4 is the silicon wafer suede top view after the making herbs into wool of the present invention；
Fig. 5 is the silicon wafer suede side view after the making herbs into wool of the present invention；
Fig. 6 is the variation diagram of reflectivity before and after silicon wafer wool making.
Detailed description of the invention
It is clearly understood to make present disclosure be easier to, below according to specific embodiment and combine accompanying drawing, to this
Invention is described in further detail.
As shown in Fig. 1～2, a kind of crystal silicon solar batteries Wet chemical processing method that making herbs into wool is carried out with cleaning substep, should
The step of method is as follows:
Embodiment one
The operation of making herbs into wool section is as follows:
(1) silicon chip after pre-treatment is provided；Pre-treatment is: is put into by the silicon chip being contained in the gaily decorated basket in pure water and soaks
Profit overflow, rinses 5min, removes dust etc..Pure water resistivity is 10-18M Ω.
(2) use the first cleaning fluid that silicon chip is carried out prerinse, to remove silicon chip surface particle impurity and pollution；
(3) use polishing etch liquid that silicon chip is processed by shot blasting, erode the mechanical damage layer on surface, mechanical damage
Layer is as shown in Figure 3；
(4) use Woolen-making liquid that silicon chip is carried out making herbs into wool process so that it is surface forms suede structure；
(5) use the second cleaning fluid that silicon chip is carried out, to remove surface metal ion, and neutralize alkaline impurities,
Reduce surface chemistry residual；
(6) use oxide etch liquid that silicon chip is processed, to remove removing oxide layer, and form hydrophobic being dried on its surface
Structure；
Complete the silicon chip of making herbs into wool to put in drying cupboard and deposit, owing to process for etching repeatability is high, can carry out the most in a large number,
Take out silicon chip after making herbs into wool according to need, i.e. can get antiradar reflectivity, the silicon chip of low recombination-rate surface through following cleaning.
Cleaning section concrete operation step is as follows:
(7) silicon chip surface is carried out oxidation-corrosion treatmentCorrosion Science repeatedly；
(8) use the 3rd cleaning fluid that silicon chip is carried out, to remove surface particles impurity, carry out chemistry neutralization；
(9) the 4th cleaning fluid is finally used silicon chip to be carried out, to remove removing oxide layer and surface metal ion, simultaneously
Form the hydrophobic surface of passivation, complete crystal silicon solar batteries wet-chemical treatment.
Wherein, in described step (2), the described mixed solution that the first cleaning fluid is NaOH and hydrogen peroxide；
And wherein, the mass percentage concentration of NaOH is 0.1%, and the mass percentage concentration of hydrogen peroxide is 1%.
Described step (2) particularly as follows: the silicon chip after pre-treatment is put into the first cleaning fluid carries out 3min prerinse,
Temperature controls at 60 DEG C；Then it is rinsed processing 5min with pure water.
In described step (3), described polishing etch liquid be mass percentage concentration be the NaOH of 30%.
Described step (3) is particularly as follows: be placed in silicon chip in polishing etch liquid, and it is 90 DEG C that temperature controls, and erodes silicon
The mechanical damage layer that sheet is formed in slicing processes, the reaction time is 3min, silicon chip every corrosion 10um；Then with pure
Water is rinsed processing 5min.
In described step (4), described Woolen-making liquid is the mixed solution of NaOH and flocking additive；And
Wherein, the mass percentage concentration of NaOH is 5%, and the mass percentage concentration of flocking additive is 3%.
Described step (4) is particularly as follows: put into silicon chip in Woolen-making liquid and carry out making herbs into wool, and reaction temperature is 80 DEG C, reaction
Time is 12min；Then it is rinsed processing 5min with pure water.
In described step (5), the second described cleaning fluid is SC2 cleaning fluid, this SC2 cleaning fluid be HCL,
H2O2And H2The mixed solution of O；And wherein, HCL, H2O2、H2The volume ratio of O is 1:1:10.
Described step (5), particularly as follows: silicon chip is placed in the second cleaning fluid process 5min, neutralizes silicon chip surface residual
Alkaline matter and metal ion；Then it is rinsed processing 5min with pure water.
In described step (6), described oxide etch liquid be mass percentage concentration be the hydrofluoric acid solution of 5%.
In described step (7), at HF and HNO3Mixed solution in silicon chip surface carried out oxidation repeatedly-
Corrosion treatmentCorrosion Science；And wherein, HF and HNO3Volume ratio be 1:50.
Described step (7) is particularly as follows: be placed in HF and HNO by silicon chip3Mixed solution in react 1min, in solution
Increase bubbling or ultrasonically treated；Then it is rinsed processing 5min with pure water.
In described step (8), the 3rd described cleaning fluid is SC1 mixing cleaning fluid, this SC1 mixing cleaning fluid
For NH4OH、H2O2And H2The mixed solution of O；And wherein, NH4OH、H2O2And H2The volume ratio of O is:
1:1:10.
Described step (8) particularly as follows: put into reaction 1min in the 3rd cleaning fluid that temperature is 60～80 DEG C by silicon chip；
Then it is rinsed processing 5min with pure water.
In described step (9), the described mixed solution that the 4th cleaning fluid is hydrofluoric acid and hydrochloric acid；And wherein,
The mass percentage concentration of hydrofluoric acid is 5%, and the mass percentage concentration of hydrochloric acid is 5%.
Described step (9), particularly as follows: silicon chip is placed in the 4th cleaning fluid process 3min, goes to removing oxide layer and surface
Metal ion, and silicon chip surface is passivated, form hydrophobic surface；Then it is rinsed processing 5min with pure water.
Embodiment two
The operation of making herbs into wool section is as follows:
(1) silicon chip after pre-treatment is provided；Pre-treatment is: is put into by the silicon chip being contained in the gaily decorated basket in pure water and soaks
Profit overflow, rinses 8min, removes dust etc..Pure water resistivity is 10-18M Ω.
(2) use the first cleaning fluid that silicon chip is carried out prerinse, to remove silicon chip surface particle impurity and pollution；
(3) use polishing etch liquid that silicon chip is processed by shot blasting, erode the mechanical damage layer on surface, mechanical damage
Layer is as shown in Figure 3；
(4) use Woolen-making liquid that silicon chip is carried out making herbs into wool process so that it is surface forms suede structure；
(5) use the second cleaning fluid that silicon chip is carried out, to remove surface metal ion, and neutralize alkaline impurities,
Reduce surface chemistry residual；
(6) use oxide etch liquid that silicon chip is processed, to remove removing oxide layer, and form hydrophobic being dried on its surface
Structure；
Complete the silicon chip of making herbs into wool to put in drying cupboard and deposit, owing to process for etching repeatability is high, can carry out the most in a large number,
Take out silicon chip after making herbs into wool according to need, i.e. can get antiradar reflectivity, the silicon chip of low recombination-rate surface through following cleaning.
Cleaning section concrete operation step is as follows:
(7) silicon chip surface is carried out oxidation-corrosion treatmentCorrosion Science repeatedly；
(8) use the 3rd cleaning fluid that silicon chip is carried out, to remove surface particles impurity, carry out chemistry neutralization；
(9) the 4th cleaning fluid is finally used silicon chip to be carried out, to remove removing oxide layer and surface metal ion, simultaneously
Form the hydrophobic surface of passivation, complete crystal silicon solar batteries wet-chemical treatment.
Wherein, in described step (2), the described mixed solution that the first cleaning fluid is NaOH and hydrogen peroxide；
And wherein, the mass percentage concentration of NaOH is 2%, and the mass percentage concentration of hydrogen peroxide is 5%.
Described step (2) particularly as follows: the silicon chip after pre-treatment is put into the first cleaning fluid carries out 3min prerinse,
Temperature controls at 60 DEG C；Then it is rinsed processing 5min with pure water.
In described step (3), described polishing etch liquid be mass percentage concentration be the NaOH of 30%.
Described step (3) is particularly as follows: be placed in silicon chip in polishing etch liquid, and it is 80 DEG C that temperature controls, and erodes silicon
The mechanical damage layer that sheet is formed in slicing processes, the reaction time is 5min, silicon chip every corrosion 11um；Then with pure
Water is rinsed processing 5min.
In described step (4), described Woolen-making liquid is the mixed solution of NaOH and flocking additive；And
Wherein, the mass percentage concentration of NaOH is 4%, and the mass percentage concentration of flocking additive is 3%.
Described step (4) is particularly as follows: put into silicon chip in Woolen-making liquid and carry out making herbs into wool, and reaction temperature is 80 DEG C, reaction
Time is 30min；Then it is rinsed processing 5min with pure water.
In described step (5), the second described cleaning fluid is SC2 cleaning fluid, this SC2 cleaning fluid be HCL,
H2O2And H2The mixed solution of O；And wherein, HCL, H2O2、H2The volume ratio of O is 1:2:13.
Described step (5), particularly as follows: silicon chip is placed in the second cleaning fluid process 7min, neutralizes silicon chip surface residual
Alkaline matter and metal ion；Then it is rinsed processing 5min with pure water.
In described step (6), described oxide etch liquid be mass percentage concentration be the hydrofluoric acid solution of 3%.
In described step (7), at HF and HNO3Mixed solution in silicon chip surface carried out oxidation repeatedly-
Corrosion treatmentCorrosion Science；And wherein, HF and HNO3Volume ratio be 1:75.
Described step (7) is particularly as follows: be placed in HF and HNO by silicon chip3Mixed solution in react 1.5min, solution
Middle increase bubbling or ultrasonically treated；Then it is rinsed processing 5min with pure water.
In described step (8), the 3rd described cleaning fluid is SC1 mixing cleaning fluid, this SC1 mixing cleaning fluid
For NH4OH、H2O2And H2The mixed solution of O；And wherein, NH4OH、H2O2And H2The volume ratio of O is:
1:3:10.
Described step (8) particularly as follows: put into reaction 5min in the 3rd cleaning fluid that temperature is 70 DEG C by silicon chip；Then
It is rinsed processing 5min with pure water.
In described step (9), the described mixed solution that the 4th cleaning fluid is hydrofluoric acid and hydrochloric acid；And wherein,
The mass percentage concentration of hydrofluoric acid is 3%, and the mass percentage concentration of hydrochloric acid is 3%.
Described step (9), particularly as follows: silicon chip is placed in the 4th cleaning fluid process 5min, goes to removing oxide layer and surface
Metal ion, and silicon chip surface is passivated, form hydrophobic surface；Then it is rinsed processing 5min with pure water.
Embodiment three
The operation of making herbs into wool section is as follows:
(1) silicon chip after pre-treatment is provided；Pre-treatment is: is put into by the silicon chip being contained in the gaily decorated basket in pure water and soaks
Profit overflow, rinses 1min, removes dust etc..Pure water resistivity is 10-18M Ω.
(2) use the first cleaning fluid that silicon chip is carried out prerinse, to remove silicon chip surface particle impurity and pollution；
(3) use polishing etch liquid that silicon chip is processed by shot blasting, erode the mechanical damage layer on surface, mechanical damage
Layer is as shown in Figure 3；
(4) use Woolen-making liquid that silicon chip is carried out making herbs into wool process so that it is surface forms suede structure；
(5) use the second cleaning fluid that silicon chip is carried out, to remove surface metal ion, and neutralize alkaline impurities,
Reduce surface chemistry residual；
(6) use oxide etch liquid that silicon chip is processed, to remove removing oxide layer, and form hydrophobic being dried on its surface
Structure；
Complete the silicon chip of making herbs into wool to put in drying cupboard and deposit, owing to process for etching repeatability is high, can carry out the most in a large number,
Take out silicon chip after making herbs into wool according to need, i.e. can get antiradar reflectivity, the silicon chip of low recombination-rate surface through following cleaning.
Cleaning section concrete operation step is as follows:
(7) silicon chip surface is carried out oxidation-corrosion treatmentCorrosion Science repeatedly；
(8) use the 3rd cleaning fluid that silicon chip is carried out, to remove surface particles impurity, carry out chemistry neutralization；
(9) the 4th cleaning fluid is finally used silicon chip to be carried out, to remove removing oxide layer and surface metal ion, simultaneously
Form the hydrophobic surface of passivation, complete crystal silicon solar batteries wet-chemical treatment.
Wherein, in described step (2), the described mixed solution that the first cleaning fluid is NaOH and hydrogen peroxide；
And wherein, the mass percentage concentration of NaOH is 1%, and the mass percentage concentration of hydrogen peroxide is 5%.
Described step (2) particularly as follows: the silicon chip after pre-treatment is put into the first cleaning fluid carries out 1min prerinse,
Temperature controls at 50-80 DEG C；Then it is rinsed processing with pure water.
In described step (3), described polishing etch liquid be mass percentage concentration be the NaOH of 10%.
Described step (3) is particularly as follows: be placed in silicon chip in polishing etch liquid, and it is 60 DEG C that temperature controls, and erodes silicon
The mechanical damage layer that sheet is formed in slicing processes, the reaction time is 1min, silicon chip every corrosion 3um；Then with pure
Water is rinsed processing.
In described step (4), described Woolen-making liquid is the mixed solution of NaOH and flocking additive；And
Wherein, the mass percentage concentration of NaOH is 0.5%, and the mass percentage concentration of flocking additive is 0.5%.
Described step (4) is particularly as follows: put into silicon chip in Woolen-making liquid and carry out making herbs into wool, and reaction temperature is 70 DEG C, reaction
Time is 10min；Then it is rinsed processing with pure water.
In described step (5), the second described cleaning fluid is SC2 cleaning fluid, this SC2 cleaning fluid be HCL,
H2O2And H2The mixed solution of O；And wherein, HCL, H2O2、H2The volume ratio of O is 1:2:12.
Described step (5), particularly as follows: silicon chip is placed in the second cleaning fluid process 3min, neutralizes silicon chip surface residual
Alkaline matter and metal ion；Then it is rinsed processing with pure water.
In described step (6), described oxide etch liquid be mass percentage concentration be the hydrofluoric acid solution of 0.5%.
In described step (7), at HF and HNO3Mixed solution in silicon chip surface carried out oxidation repeatedly-
Corrosion treatmentCorrosion Science；And wherein, HF and HNO3Volume ratio be 1:80.
Described step (7) is particularly as follows: be placed in HF and HNO by silicon chip3Mixed solution in react 0.5min, solution
Middle increase bubbling or ultrasonically treated；Then it is rinsed processing with pure water.
In described step (8), the 3rd described cleaning fluid is SC1 mixing cleaning fluid, this SC1 mixing cleaning fluid
For NH4OH、H2O2And H2The mixed solution of O；And wherein, NH4OH、H2O2And H2The volume ratio of O is:
1:0.5:10.
Described step (8) particularly as follows: put into reaction 1min in the 3rd cleaning fluid that temperature is 60～80 DEG C by silicon chip；
Then it is rinsed processing with pure water.
In described step (9), the described mixed solution that the 4th cleaning fluid is hydrofluoric acid and hydrochloric acid；And wherein,
The mass percentage concentration of hydrofluoric acid is 0.5%, and the mass percentage concentration of hydrochloric acid is 0.5%.
Described step (9), particularly as follows: silicon chip is placed in the 4th cleaning fluid process 1min, goes to removing oxide layer and surface
Metal ion, and silicon chip surface is passivated, form hydrophobic surface；Then it is rinsed processing 5min with pure water.
Embodiment four
The operation of making herbs into wool section is as follows:
(1) silicon chip after pre-treatment is provided；Pre-treatment is: is put into by the silicon chip being contained in the gaily decorated basket in pure water and soaks
Profit overflow, rinses 10min, removes dust etc..Pure water resistivity is 10-18M Ω.
(2) use the first cleaning fluid that silicon chip is carried out prerinse, to remove silicon chip surface particle impurity and pollution；
(3) use polishing etch liquid that silicon chip is processed by shot blasting, erode the mechanical damage layer on surface, mechanical damage
Layer is as shown in Figure 3；
(4) use Woolen-making liquid that silicon chip is carried out making herbs into wool process so that it is surface forms suede structure；
(5) use the second cleaning fluid that silicon chip is carried out, to remove surface metal ion, and neutralize alkaline impurities,
Reduce surface chemistry residual；
(6) use oxide etch liquid that silicon chip is processed, to remove removing oxide layer, and form hydrophobic being dried on its surface
Structure；
Complete the silicon chip of making herbs into wool to put in drying cupboard and deposit, owing to process for etching repeatability is high, can carry out the most in a large number,
Take out silicon chip after making herbs into wool according to need, i.e. can get antiradar reflectivity, the silicon chip of low recombination-rate surface through following cleaning.
Cleaning section concrete operation step is as follows:
(7) silicon chip surface is carried out oxidation-corrosion treatmentCorrosion Science repeatedly；
(8) use the 3rd cleaning fluid that silicon chip is carried out, to remove surface particles impurity, carry out chemistry neutralization；
(9) the 4th cleaning fluid is finally used silicon chip to be carried out, to remove removing oxide layer and surface metal ion, simultaneously
Form the hydrophobic surface of passivation, complete crystal silicon solar batteries wet-chemical treatment.
Wherein, in described step (2), the described mixed solution that the first cleaning fluid is NaOH and hydrogen peroxide；
And wherein, the mass percentage concentration of NaOH is 3%, and the mass percentage concentration of hydrogen peroxide is 10%.
Described step (2) particularly as follows: the silicon chip after pre-treatment is put into the first cleaning fluid carries out 5min prerinse,
Temperature controls at 80 DEG C；Then it is rinsed processing with pure water.
In described step (3), described polishing etch liquid be mass percentage concentration be the NaOH of 50%.
Described step (3) is particularly as follows: be placed in silicon chip in polishing etch liquid, and it is 100 DEG C that temperature controls, and erodes
The mechanical damage layer that silicon chip is formed in slicing processes, the reaction time is 10min, silicon chip every corrosion 20um；Then
It is rinsed processing with pure water.
In described step (4), described Woolen-making liquid is the mixed solution of NaOH and flocking additive；And
Wherein, the mass percentage concentration of NaOH is 8%, and the mass percentage concentration of flocking additive is 5%.
Described step (4) is particularly as follows: put into silicon chip in Woolen-making liquid and carry out making herbs into wool, and reaction temperature is 90 DEG C, reaction
Time is 30min；Then it is rinsed processing with pure water.
In described step (5), the second described cleaning fluid is SC2 cleaning fluid, this SC2 cleaning fluid be HCL,
H2O2And H2The mixed solution of O；And wherein, HCL, H2O2、H2The volume ratio of O is 1:3:15.
Described step (5), particularly as follows: silicon chip is placed in the second cleaning fluid process 10min, neutralizes silicon chip surface residual
Stay alkaline matter and metal ion；Then it is rinsed processing with pure water.
In described step (6), described oxide etch liquid be mass percentage concentration be the hydrofluoric acid solution of 5%.
In described step (7), at HF and HNO3Mixed solution in silicon chip surface carried out oxidation repeatedly-
Corrosion treatmentCorrosion Science；And wherein, HF and HNO3Volume ratio be 1:100.
Described step (7) is particularly as follows: be placed in HF and HNO by silicon chip3Mixed solution in react 2min, solution
Middle increase bubbling or ultrasonically treated；Then it is rinsed processing with pure water.
In described step (8), the 3rd described cleaning fluid is SC1 mixing cleaning fluid, this SC1 mixing cleaning fluid
For NH4OH、H2O2And H2The mixed solution of O；And wherein, NH4OH、H2O2And H2The volume ratio of O is:
1:5:15.
Described step (8) particularly as follows: put into reaction 10min in the 3rd cleaning fluid that temperature is 60～80 DEG C by silicon chip；
Then it is rinsed processing with pure water.
In described step (9), the described mixed solution that the 4th cleaning fluid is hydrofluoric acid and hydrochloric acid；And wherein,
The mass percentage concentration of hydrofluoric acid is 5%, and the mass percentage concentration of hydrochloric acid is 5%.
Described step (9), particularly as follows: silicon chip is placed in the 4th cleaning fluid process 10min, removes removing oxide layer and table
Face metal ion, and silicon chip surface is passivated, form hydrophobic surface；Then it is rinsed processing 5min with pure water.
Silicon chip carries out " lifting slowly " operation from pure water and takes out, and can carry out last part technology after drying.
Through test, as shown in Figure 4,5, silicon wafer suede " pyramid " structure processed by above wet chemical technology
Size 1-4um, its recombination-rate surface is less than 10cm/s, as shown in Figure 6, in the reflection of 300-1100nm scope
Rate is about 11%, and the wet chemical technology time is reduced to about 1.5h, thus reduces reflectivity, improves silicon chip table
Face cleanliness factor, meets the requirement of efficient heterojunction solar battery.
Particular embodiments described above, to present invention solves the technical problem that, technical scheme and beneficial effect entered
One step describes in detail, be it should be understood that the specific embodiment that the foregoing is only the present invention, is not limited to
The present invention, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. done, all should wrap
Within being contained in protection scope of the present invention.
Claims (11)
1. the crystal silicon solar batteries Wet chemical processing method that making herbs into wool is carried out with cleaning substep, it is characterised in that should
The step of method is as follows:
(1) silicon chip after pre-treatment is provided；
(2) use the first cleaning fluid that silicon chip is carried out prerinse, to remove silicon chip surface particle impurity and pollution；
(3) use polishing etch liquid that silicon chip is processed by shot blasting, erode the mechanical damage layer on surface；
(4) use Woolen-making liquid that silicon chip is carried out making herbs into wool process so that it is surface forms suede structure；
(5) use the second cleaning fluid that silicon chip is carried out, to remove surface metal ion, and neutralize alkaline impurities,
Reduce surface chemistry residual；
(6) use oxide etch liquid that silicon chip is processed, to remove removing oxide layer, and form hydrophobic being dried on its surface
Structure；
(7) silicon chip surface is carried out oxidation-corrosion treatmentCorrosion Science repeatedly；In described step (7), at HF and HNO3
Mixed solution in silicon chip surface carried out oxidation-corrosion treatmentCorrosion Science repeatedly；And wherein, HF and HNO3Volume ratio
For 1:(50～100)；Described step (7) is particularly as follows: be placed in HF and HNO by silicon chip3Mixed solution in react
0.5～2min, solution increases bubbling or ultrasonically treated；Then it is rinsed processing with pure water；
(8) use the 3rd cleaning fluid that silicon chip is carried out, to remove surface particles impurity, carry out chemistry neutralization；?
In described step (8), the 3rd described cleaning fluid is SC1 mixing cleaning fluid, and this SC1 mixing cleaning fluid is NH4OH、
H2O2And H2The mixed solution of O；And wherein, NH4OH、H2O2And H2The volume ratio of O is: 1:(0.5～5):
(10～15)；Described step (8) is particularly as follows: put into silicon chip in the 3rd cleaning fluid that temperature is 60～80 DEG C and react
1～10min；Then it is rinsed processing with pure water；
(9) the 4th cleaning fluid is finally used silicon chip to be carried out, to remove removing oxide layer and surface metal ion, simultaneously
Form the hydrophobic surface of passivation, complete crystal silicon solar batteries wet-chemical treatment；In described step (9), described
The mixed solution that the 4th cleaning fluid is hydrofluoric acid and hydrochloric acid；And wherein, the mass percentage concentration of hydrofluoric acid is
0.5%～5%, the mass percentage concentration of hydrochloric acid is 0.5%～5%；Described step (9) particularly as follows: be placed in by silicon chip
Four cleaning fluids process 1～10min, removes removing oxide layer and surface metal ion, and silicon chip surface is passivated, formed
Hydrophobic surface；Then it is rinsed processing with pure water.
The crystal silicon solar batteries wet-chemical treatment side that making herbs into wool is carried out with cleaning substep the most according to claim 1
Method, it is characterised in that: described step (6) and step (7) further comprise the steps of: and silicon chip is put into drying cupboard deposits.
At the crystal silicon solar batteries wet-chemical that making herbs into wool and cleaning substep are carried out the most according to claim 1 and 2
Reason method, it is characterised in that: in described step (2), the first described cleaning fluid is NaOH and hydrogen peroxide
Mixed solution；And wherein, the mass percentage concentration of NaOH is 0.1%～3%, the mass percentage concentration of hydrogen peroxide
It is 1%～10%.
The crystal silicon solar batteries wet-chemical treatment side that making herbs into wool is carried out with cleaning substep the most according to claim 3
Method, it is characterised in that: described step (2) is particularly as follows: put into the silicon chip after pre-treatment in the first cleaning fluid and carry out
1～5min prerinse, temperature controls at 50-80 DEG C；Then it is rinsed processing with pure water.
At the crystal silicon solar batteries wet-chemical that making herbs into wool and cleaning substep are carried out the most according to claim 1 and 2
Reason method, it is characterised in that: in described step (3), described polishing etch liquid is that mass percentage concentration is
The NaOH of 10%～50%.
The crystal silicon solar batteries wet-chemical treatment side that making herbs into wool is carried out with cleaning substep the most according to claim 5
Method, it is characterised in that: described step (3) is particularly as follows: be placed in silicon chip in polishing etch liquid, and it is 60 that temperature controls
DEG C～100 DEG C, erode the mechanical damage layer that silicon chip is formed in slicing processes, the reaction time is 1～10min, silicon chip
Every corrosion 3～20um；Then it is rinsed processing with pure water.
At the crystal silicon solar batteries wet-chemical that making herbs into wool and cleaning substep are carried out the most according to claim 1 and 2
Reason method, it is characterised in that: in described step (4), described Woolen-making liquid is NaOH and flocking additive
Mixed solution；And wherein, the mass percentage concentration of NaOH is 0.5%～8%, the percent mass of flocking additive
Concentration is 0.5%～5%.
The crystal silicon solar batteries wet-chemical treatment side that making herbs into wool is carried out with cleaning substep the most according to claim 7
Method, it is characterised in that: described step (4) is particularly as follows: put into silicon chip in Woolen-making liquid and carry out making herbs into wool, reaction temperature
Being 70～90 DEG C, the reaction time is 10～30min；Then it is rinsed processing with pure water.
At the crystal silicon solar batteries wet-chemical that making herbs into wool and cleaning substep are carried out the most according to claim 1 and 2
Reason method, it is characterised in that: in described step (5), the second described cleaning fluid is SC2 cleaning fluid, this SC2
Cleaning fluid is HCL, H2O2And H2The mixed solution of O；And wherein, HCL, H2O2、H2The volume ratio of O is 1:
(1～3): (10～15).
The crystal silicon solar batteries wet-chemical treatment side that making herbs into wool is carried out with cleaning substep the most according to claim 9
Method, it is characterised in that: described step (5) particularly as follows: silicon chip is placed in the second cleaning fluid process 3～10min,
Neutralize silicon chip surface residual alkaline matter and metal ion；Then it is rinsed processing with pure water.
At the 11. crystal silicon solar batteries wet-chemical that making herbs into wool and cleaning substep are carried out according to claim 1 and 2
Reason method, it is characterised in that: in described step (6), described oxide etch liquid is that mass percentage concentration is
The hydrofluoric acid solution of 0.5%～5%.
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| CN106373862A (en) * | 2015-07-24 | 2017-02-01 | 钧石(中国)能源有限公司 | Processing method applicable to wet cleaning of heterojunction cell |
| GR20150100472A (en) * | 2015-10-30 | 2017-07-03 | Πανεπιστημιο Πατρων | Polycrystalline silicon water with configured microstructures on their surfaces for improving solar absorption |
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| CN107706087B (en) * | 2017-08-21 | 2021-04-13 | 环晟光伏(江苏)有限公司 | Silicon wafer cleaning method |
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| CN108231540A (en) * | 2017-12-20 | 2018-06-29 | 横店集团东磁股份有限公司 | A kind of rear cleaning applied to solar cell making herbs into wool |
| CN108384667A (en) * | 2018-02-28 | 2018-08-10 | 浙江晶科能源有限公司 | A kind of silicon chip cleaning liquid and silicon wafer cleaning method |
| CN109148265A (en) * | 2018-08-10 | 2019-01-04 | 横店集团东磁股份有限公司 | A kind of solar energy polycrystal RIE prepares the cleaning process before black silicon |
| CN110165018A (en) * | 2019-04-18 | 2019-08-23 | 横店集团东磁股份有限公司 | A kind of polycrystalline cleaning process of decline electric leakage raising efficiency |
| CN111074280A (en) * | 2019-12-20 | 2020-04-28 | 中建材浚鑫科技有限公司 | Novel alkali polishing process |
| CN111554758A (en) * | 2020-04-24 | 2020-08-18 | 中威新能源(成都)有限公司 | Texturing pretreatment system and method suitable for different texturing additives |
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Address after: Solar photovoltaic industry park Tianhe Road 213031 north of Jiangsu Province, Changzhou City, No. 2 Patentee after: TRINA SOLAR Co.,Ltd. Address before: Solar photovoltaic industry park Tianhe Road 213031 north of Jiangsu Province, Changzhou City, No. 2 Patentee before: trina solar Ltd. |
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