CN110491971A - A kind of large scale imbrication battery process for etching - Google Patents
A kind of large scale imbrication battery process for etching Download PDFInfo
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- CN110491971A CN110491971A CN201910780093.7A CN201910780093A CN110491971A CN 110491971 A CN110491971 A CN 110491971A CN 201910780093 A CN201910780093 A CN 201910780093A CN 110491971 A CN110491971 A CN 110491971A
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- pickling
- silicon wafer
- wool
- oxide layer
- making herbs
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 230000008569 process Effects 0.000 title claims abstract description 48
- 238000005530 etching Methods 0.000 title claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 185
- 239000010703 silicon Substances 0.000 claims abstract description 184
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 184
- 238000005554 pickling Methods 0.000 claims abstract description 80
- 210000002268 wool Anatomy 0.000 claims abstract description 68
- 235000008216 herbs Nutrition 0.000 claims abstract description 67
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 55
- 230000003647 oxidation Effects 0.000 claims abstract description 51
- 238000001035 drying Methods 0.000 claims abstract description 32
- 238000012805 post-processing Methods 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 171
- 239000012530 fluid Substances 0.000 claims description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 56
- 229910001868 water Inorganic materials 0.000 claims description 55
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 48
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 45
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 238000004140 cleaning Methods 0.000 claims description 32
- 238000005498 polishing Methods 0.000 claims description 26
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 18
- 239000000654 additive Substances 0.000 claims description 15
- 230000000996 additive effect Effects 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 8
- 229910052731 fluorine Inorganic materials 0.000 claims description 8
- 239000011737 fluorine Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 150000002431 hydrogen Chemical class 0.000 claims 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 17
- 229910052751 metal Inorganic materials 0.000 abstract description 16
- 239000002184 metal Substances 0.000 abstract description 16
- 230000003749 cleanliness Effects 0.000 abstract description 8
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 235000012431 wafers Nutrition 0.000 description 94
- 239000010410 layer Substances 0.000 description 40
- 238000004519 manufacturing process Methods 0.000 description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 28
- 239000000243 solution Substances 0.000 description 22
- 238000001802 infusion Methods 0.000 description 21
- 230000002000 scavenging effect Effects 0.000 description 17
- 239000000377 silicon dioxide Substances 0.000 description 14
- 239000007788 liquid Substances 0.000 description 10
- 210000004027 cell Anatomy 0.000 description 8
- 238000002310 reflectometry Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000003814 drug Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000013589 supplement Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 5
- 229910001882 dioxygen Inorganic materials 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 239000008155 medical solution Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229910003638 H2SiF6 Inorganic materials 0.000 description 2
- 229910004074 SiF6 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000010301 surface-oxidation reaction Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 210000004483 pasc Anatomy 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- ZEFWRWWINDLIIV-UHFFFAOYSA-N tetrafluorosilane;dihydrofluoride Chemical compound F.F.F[Si](F)(F)F ZEFWRWWINDLIIV-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
-
- 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 provides a kind of large scale imbrication battery process for etching, carries out oxidation and first time pickling processes before making herbs into wool, including to silicon wafer, the oxidation is to carry out oxidation to the surface of the silicon wafer after feeding to form layer of oxide layer；The first time pickling is that greasy dirt of the pickling to remove the oxide layer and be pasted in the oxide layer is carried out to the oxide layer.Process for etching of the present invention, it is particularly suitable for having a size of 160-260mm square silicon wafer, a kind of oxide layer being easily removed is formed by the way that the metal impurities of silicon chip surface are carried out oxidation in advance, the oxide layer is complexed after first time pickling again, form a kind of water-soluble complex compound, and then the greasy dirt for being pasted on the oxide layer can be effectively removed, improve silicon chip surface cleanliness, good surface foundation is provided for the subsequent flannelette for preparing, it is successively preprocessed again, making herbs into wool, post-processing, after second of pickling and drying, it can get that surface texture is small and uniform silicon wafer, battery electrical property is set to improve 0.01-0.03%.
Description
Technical field
The invention belongs to crystal silicon solar batteries piece manufacture technology fields, more particularly, to a kind of large scale imbrication battery system
Suede technique.
Background technique
Solar-energy photo-voltaic cell process for etching is exactly the mechanical damage layer that silicon chip surface is removed using caustic corrosion, and forms gold
The tower-like flannelette of word reduces light in the reflection of silicon chip surface, and improves absorption of the silicon wafer to light, and then increases solar battery
Incident photon-to-electron conversion efficiency.As photovoltaic market develops, also needed to meet while production cost should be reduced to solar cell module
The requirement of high power and high conversion, therefore imbrication used in battery small size silicon wafer is because its effective area is small, battery converts function at present
Rate is low and is gradually eliminated.Prior art is after directly pre-processing to silicon wafer with regard to making herbs into wool, post-processing, pickling and drying,
The increase of imbrication cell silicon chip size causes silicon wafer to will appear more metal impurities and greasy dirt in cutting process, according to existing
Process for etching can not completely remove remaining impurity on large-sized silicon wafers surface, after making herbs into wool silicon chip surface be easy to appear it is dirty or
Spot seriously affects the electric conductivity of battery, causes cell piece transfer efficiency low, and component power is low, not can guarantee product quality.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of large scale imbrication battery process for etching, be especially adapted for use in having a size of
The making herbs into wool of 160-260mm square silicon wafer solves silicon chip surface greasy dirt and metal impurities removal during making herbs into wool in the prior art
The unclean and technical problem that causes battery electrical property low, improves silicon chip surface cleanliness.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of large scale imbrication battery process for etching carries out oxidation and first time pickling before making herbs into wool, including to silicon wafer
Processing, the oxidation are to carry out oxidation to the surface of the silicon wafer after feeding to form layer of oxide layer；The first time pickling
It is that greasy dirt of the pickling to remove the oxide layer and be pasted in the oxide layer is carried out to the oxide layer.
Further, the medical fluid of the oxidation includes ozone and sodium hydroxide, and the amount infused of the ozone is 5-25L/h,
The solution ratio of the sodium hydroxide is 3-4%.
Further, the temperature of the oxidation is 40-80 DEG C, time 1-5min.
Further, medical fluid used in the first time pickling is solution than the hydrofluoric acid for 10-15%, first hypo acid
Washing temperature is room temperature, pickling time 1-5min.
Further, rinsing bowl is equipped in the final step of the oxidation and the first time pickling.
Further, the making herbs into wool is carried out in sodium hydroxide medical fluid, also adds several additives, the sodium hydroxide
Solution ratio is 4-4.5%, and the solution ratio of the additive is 0.6-1%.
Further, the making herbs into wool temperature is 60-100 DEG C, time 3.5-9.5min.
Further, it is respectively equipped with pretreatment and post-processing before and after the making herbs into wool, the pretreatment is placed in the first time
After pickling, the pretreatment includes rough polishing and prerinse；The post-processing is cleaned after including；The rough polishing medical fluid is solution ratio
For the sodium hydroxide of 4-4.5%；Cleaning medical fluid is hydrogen peroxide and sodium hydroxide after described in the prerinse, the hydrogen peroxide with
The solution of the sodium hydroxide is than being respectively 4-7% and 0.2-0.5%.
Further, second of pickling and drying, second of pickling medical fluid are successively arranged after the post-processing
For the mixed liquor of hydrofluoric acid and hydrochloric acid, the hydrofluoric acid solution ratio is 10-15%, and the hydrochloric acid solution ratio is 10-15%；It is described
Drying completely lifts again high temperature drying for first hot water, and the drying temperature is 60-100 DEG C.
Further, in the pretreatment, the final step of the making herbs into wool and the post-processing and second of pickling
It is equipped with the rinsing bowl, the rinsing bowl solution is pure water, washing time 0.5-3.5min.
Process for etching designed by the invention is especially adapted for use in the making herbs into wool having a size of 160-260mm square silicon wafer, leads to
After in advance by the metal impurities of silicon chip surface carry out oxidation form a kind of oxide layer being easily removed, then after first time pickling it is right
The oxide layer is complexed, and forms a kind of water-soluble complex compound, and then can effectively remove the greasy dirt for being pasted on the oxide layer,
Silicon chip surface cleanliness is improved, provides good surface foundation for the subsequent flannelette for preparing.Then again successively preprocessed, making herbs into wool,
It after post-processing, second of pickling and drying, can get that surface texture is small and uniform silicon wafer, improve battery conductive performance
0.01-0.03%.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of large scale imbrication battery etching device of one embodiment of the invention；
Fig. 2 is a kind of flow chart of large scale imbrication battery process for etching of one embodiment of the invention；
Fig. 3 is the microgram (3000 times) for the silicon wafer suede that making herbs into wool obtains in the embodiment of the present invention one；
Fig. 4 is the microgram (3000 times) for the silicon wafer suede that making herbs into wool obtains in the embodiment of the present invention two；
Fig. 5 is the microgram (3000 times) for the silicon wafer suede that making herbs into wool obtains in the embodiment of the present invention three.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
A kind of large scale imbrication battery etching device is proposed in one embodiment of the invention, as shown in Figure 1, successively including oxidation
Unit, first time pickling unit, pretreatment unit, making herbs into wool unit, post-processing unit, second of pickling unit and drying unit,
And after oxidation unit, the first pickling unit, pretreatment unit, making herbs into wool unit, post-processing unit and second of pickling unit
It is respectively provided with an independent rinsing bowl.
Specifically, oxidation unit successively includes the feeding groove of 1#, the oxidation trough of 2# and 3# rinsing bowl, is arranged in 1# feeding groove
Have pure water, first to enter 1# feeding groove in silicon wafer carry out room temperature cleaning, 1# feeding groove be pressure pulse cleaning, it is therefore an objective to cleaning first
Remove the large granular impurity and silicon powder dust on silicon wafer outer surface.Enter in 2# oxidation trough from the silicon wafer come out in 1# feeding groove,
The admixing medical solutions of sodium hydroxide and water are placed in 2# oxidation trough, while leading to ozone gas into 2# oxidation trough, ozone can be with
Outermost pasc reaction generates layer of silicon dioxide oxide layer in two sided on silicon wafer, and silica oxide layer is encountering hydrogen fluorine
A kind of complex compound H for being dissolved in water can be generated when sour2SiF6.In the prior art, it commonly uses hydrogen peroxide and carrys out silica, but hydrogen peroxide is easily waved
Hair, is not easy to control with reacting for silicon, and when oxidation needs to monitor always the concentration of hydrogen peroxide solution in slot, prevents from excessively waving
Hair causes silicon chip insufficient；And hydrogen peroxide is polluted the environment using rear direct emission, is not easily recycled.It is controllable using ozone
Its flow is made, compared with hydrogen peroxide, the reaction speed speed of ozone and silicon is relatively slow, and can be fully oxidized；Ozone compares dioxygen simultaneously
The production cost of water is low, but also environmental protection, therefore it is preferred that ozone oxidation substitutes hydrogen peroxide.In oxidation process, need regular replenishment smelly
Oxygen amount keeps silicon chip surface oxidation effectiveness consistent to guarantee silicon chip surface oxidation sufficiently, and the amount infused of ozone is 5-25L/h.In 2#
In medical fluid in oxidation trough, sodium hydroxide medical fluid is used to remove the metal impurities on silicon chip surface, and the solution ratio of sodium hydroxide is
3-4%, remaining is pure water；Oxidizing temperature is 40-80 DEG C, oxidization time 1-5min.With becoming larger for die size, in making herbs into wool
In the process, the liquor ratio of matching of the whole volume of required medical fluid and each ingredient also correspondinglys increase in each step, to guarantee the making herbs into wool of silicon wafer
Effect.In the present embodiment, rotation is carried out after every production 400-600 frame silicon wafer and once supplement medical fluid, wherein every basket of storage silicon wafer
200-400 piece, subsequent every basket of installation silicon wafer quantity is identical, is not repeated.For the consistency for guaranteeing the liquor strength in slot, guarantee
The amount infused of the effect of oxidation quality, every wheel sodium hydroxide is 0.05-0.15L.Oxidation unit is to first pass through ozone gas for silicon
The silicon of piece bilayer outer surface carries out oxidation and forms one layer of silica oxide layer for being easy to be removed, while sticking on the oxide layer
On other surface impurities or greasy dirt, can be fallen together by subsequent pickling, it is miscellaneous not only to accelerate silicon chip surface metal in this way
The cleaning of matter, but also can farthest guarantee the cleannes of silicon chip surface, establish clean plane in advance for subsequent making herbs into wool
Basis.
3# rinsing bowl is equipped with after 2# oxidation trough, storage is pure water liquid, scavenging period 0.5- in 3# rinsing bowl
3.5min, periodically into 3# rinsing bowl, water storage is supplemented incessantly, it is therefore an objective to the medical fluid after removal oxidation on silicon chip surface, simultaneously
Metal impurities and greasy dirt on silicon chip surface also capable of washing.
Further, first time pickling unit includes 4# descaling bath and 5# rinsing bowl, and medical fluid is the mixed of hydrofluoric acid and pure water
Solution is closed, wherein the configuration solution ratio of hydrofluoric acid is 10-15%, and first time pickling unit is to carry out at normal temperature, pickling time
For 1-5min.In this course, hydrofluoric acid can carry out complex reaction with silicon chip surface oxide layer silica, and specific reaction is public
Formula:
6HF+SiO2=H2SiF6+2H2O
H2SiF6It is that a kind of complex compound for being readily dissolved in water is completely removed oxide layer titanium dioxide after 4# descaling bath pickling
Silicon and stick on greasy dirt in silica oxide layer, silicon chip surface cleanliness can be improved, for it is subsequent prepare flannelette provide it is good
Good surface foundation.In this unit, for the consistency for guaranteeing hydrofluoric acid concentration in 4# descaling bath medical fluid, every production 400-
Rotation is carried out after 600 frame silicon wafers and once supplements medical fluid, and the amount infused of every wheel hydrofluoric acid is 0.3-0.7L, can be without using other
Acid solution can complete the removal of oxide layer.Silicon wafer after pickling need to enter back into 5# rinsing bowl and be washed, to remove silicon wafer table
The pickling medical fluid in face, while also can remove the remaining metal impurities of silicon chip surface and greasy dirt, it is further ensured that the clear of silicon chip surface
It is clean.
The mixed solution for commonly using nitric acid and hydrofluoric acid in the prior art directly carries out pickling to the silicon chip surface after feeding, because
Silicon and nitric acid and hydrofluoric acid do not react individually, but when silicon and nitric acid and hydrofluoric acid are got along simultaneously, reaction acutely, is corroded
Fast speed, the bad control of corrosive effect, and the bad regulation of proportion of both acid, directly mix cleaning effect obtained
It is bad, it can not fully erased greasy dirt and metal impurities.And the application is step by step to the metal impurities and greasy dirt of silicon chip surface
Removal first forms layer of oxide layer silica in silicon chip surface with the ozone gas being of little use, is washed with water in oxide layer
Medical fluid clean up, then silica is reacted with hydrofluoric acid, forms a kind of complex compound H for being readily dissolved in water2SiF6,
And then make the oxide layer of silicon chip surface and stick on the greasy dirt for aoxidizing layer surface by a logical removal, it is discharged with water；And it is aoxidizing
Individually cleaning is carried out with the 5# rinsing bowl being independently arranged is passed through after first time pickling again, can remove on silicon chip surface remain completely
Metal impurities and greasy dirt, the cleaning effect of silicon chip surface is more preferable, is more advantageous to subsequent making herbs into wool.With the light of model M-2000 V
Spectrum formula ellipsometer, testing out silica layer depth in silicon chip surface is 1-2um, i.e. the single layer after first time pickling is thinned deep
Degree is 1-2um, fully controllable, is met the requirements.
Pretreatment unit includes the precleaning spout and 8# rinsing bowl of 6# rough polishing slot, 7#, places hydroxide in 6# rough polishing slot
The admixing medical solutions of sodium and pure water, it is therefore an objective to remove the cutting damage layer of silicon chip surface, formation one is two-sided smooth after corrosion thinning
Surface, be conducive to subsequent prepare flannelette；It also can remove remaining a small amount of metal ion and organic matter on silicon chip surface simultaneously.
In this unit, the medical fluid in 6# rough polishing slot is solution than the sodium hydroxide for 4-4.5%, 60-100 DEG C of rough polishing temperature, warp
After 1-5min, the rough polishing of silicon wafer can be completed, remove the damaging layer of silicon chip surface.To guarantee rough polishing effect, every production 400-600
Rotation is carried out after frame silicon wafer and once supplements medical fluid, and the amount infused of every wheel sodium hydroxide is 0.4-1.2L.Medicine in 7# precleaning spout
Liquid is the mixed solution of hydrogen peroxide and sodium hydroxide, the solution ratio respectively 4-7% and 0.2- of hydrogen peroxide and sodium hydroxide
0.5%, cleaning temperature is 40-80 DEG C, scavenging period 1-5min.Alkaline solution is in advance to the metal ion and organic matter on silicon wafer
It is cleaned, guarantees the cleannes for entering 9# texturing slot silicon wafer, for the stability for guaranteeing 7# precleaning spout Chinese medicine liquid concentration, every life
Progress rotation once supplements medical fluid after producing 400-600 frame silicon wafer, and every hydrogen peroxide and the amount infused of sodium hydroxide of taking turns is respectively 0.5-
1.5L and 0.05-0.15L.Enter the medical fluid in 8# rinsing bowl on cleaning silicon chip surface after prerinse.Because 6# rough polishing slot with
7# precleaning spout contains alkali, so cleaning it is not necessary that rinsing bowl is arranged after 6# rough polishing slot, it is only necessary to be arranged after 7# precleaning spout
8# rinsing bowl.
Making herbs into wool unit includes 9# texturing slot and 10# rinsing bowl, and sodium hydroxide, portions additive are placed in 9# texturing slot
With the admixing medical solutions of water, wherein sodium hydroxide solution ratio is 4-4.5%, and additive includes water, sodium acetate, defoaming agent and surface
Activating agent, the solution ratio of additive are 0.6-1%, and silicon wafer is in 60-100 DEG C after making herbs into wool 3.5-9.5min, just in making herbs into wool temperature
It can corrode to form several densely covered concave-convex types surface microstructures at silicon chip surface.Select solution than the hydrogen-oxygen for 4-4.5%
Change sodium, there can be the anisotropic etch characteristic of different corrosion rates in different crystal orientation to crystalline silicon, and then can be in silicon
Piece surface forms a pyramid shape flannelette that is small, uniform and being covered with entire silicon face, increases sunlight on cell piece surface
Number is reflected, improve cell piece to the absorption of light and reduces reflection, and then short circuit current can be improved, the final photoelectricity for improving battery
Transformation efficiency.Making herbs into wool effect is mainly related with the mobility of making herbs into wool temperature, the uniformity of liquor strength and medical fluid.In the present embodiment
In, it is preferable that making herbs into wool temperature can guarantee the mobility of medical fluid in 70-90 DEG C, while medical fluid need to be replenished in time, specifically, because
The making herbs into wool time is longer when making herbs into wool and requires the relatively high with liquid of wool making liquor, and the concentration of making herbs into wool time long meeting dilute liquid medicine influences
It matches liquor ratio, therefore need to carry out rotation after every production 200-300 frame silicon wafer and once supplement medical fluid, to guarantee the consistent of liquor strength
Property and uniformity, the amount infused of every wheel sodium hydroxide be 0.5-1.5L, the amount infused of additive is 0.05-0.15L.After making herbs into wool
Silicon wafer enters back into cleaning in 10# rinsing bowl, removes the alkaline medical fluid on silicon chip surface.
Post-processing unit includes the rear rinse bath of 11# and the rinsing bowl of 12#, and the medical fluid that the rear rinse bath of 11# is placed is double
The solution of the mixed solution of oxygen water and sodium hydroxide, hydrogen peroxide and sodium hydroxide is than being respectively 4-7% and 0.2-0.5%, cleaning
Temperature is 40-80 DEG C, scavenging period 1-5min.Alkaline solution is to remove the remaining additive of silicon chip surface and organic matter, rear clear
The medical fluid in 12# rinsing bowl on cleaning silicon chip surface is entered back into after washing, and improves the cleannes of silicon chip surface.To guarantee 11#
The stability of rinse bath Chinese medicine liquid concentration afterwards carries out rotation after every production 400-600 frame silicon wafer and once supplements medical fluid, every wheel dioxygen
The amount infused of water and sodium hydroxide is respectively 0.5-1.5L and 0.05-0.15L.
Second of pickling unit includes the descaling bath of 13# and the rinsing bowl of 14#, 13# descaling bath be placed hydrofluoric acid with
The mixed solution of hydrochloric acid, wherein the solution ratio of hydrofluoric acid is 10-15%, and the solution ratio of hydrochloric acid is 10-15%.Hydrofluoric acid can be gone
Except the oxide layer on silicon face, hydrochloric acid can remove the remaining metal impurities of silicon chip surface, and hydrochloric acid has acid and complexing agent
Double action, the chloride ion in hydrochloric acid can dissolve other metal ions that silicon chip surface stains.In second of acid cleaning process, it is
Pickling is carried out at normal temperature, and pickling time is 1-5min, for the stabilization for guaranteeing pickling medical fluid in slot, every production 400-600 frame silicon
Rotation is carried out after piece and once supplements medical fluid, and every wheel hydrofluoric acid amount infused is 0.3-0.9L, the amount infused of hydrochloric acid are as follows: 0.3-0.9L.
The purpose of pickling is the silica and metal ion for removing silicon chip surface, forms the preferable flannelette of hydrophobicity.It is passed through again after pickling
The cleaning of 14# rinsing bowl, removes the medical fluid of silicon chip surface.
Drying unit includes full lifting slot, the drying tank of 16# and the blanking groove of 17# of 15#, and 15# is completely lifted in slot and placed
Be hot water, temperature is 50-90 DEG C, it is preferable that temperature is 70-90 DEG C, and scavenging period is 0.5-3.5min, it is therefore an objective to clean silicon
Piece surface, and the water mark on surface is reduced, be conducive to subsequent drying and processing.Silicon wafer is after completely lifting again into such as 16# drying tank, drying
Temperature is 60-100 DEG C, it is preferable that temperature is 70-90 DEG C, drying time 4-8min, with the water of hot blast drying silicon chip surface,
Guarantee the cleanliness of silicon chip surface.
In the present embodiment, 3# rinsing bowl, 5# rinsing bowl, 8# rinsing bowl, 10# rinsing bowl, 12# rinsing bowl and 14# washing
Slot is the pure water under room temperature, scavenging period 0.5-3.5min.
The present invention forms a kind of oxide layer being easily removed by the way that the metal impurities of silicon chip surface are carried out oxidation in advance, then
The oxide layer is complexed after first time pickling, forms a kind of water-soluble complex compound, and then can effectively remove and stick
In the greasy dirt of the oxide layer, silicon chip surface cleanliness is improved, good surface foundation is provided for the subsequent flannelette for preparing, is conducive to silicon
The micro-structure in piece battery face is more uniform, silicon chip surface silica layer depth, that is, thinning single surface depth after first time pickling
It is fully controllable for 1-2um.Simultaneously after first time pickling, then successively pre-processed, making herbs into wool, post-processing, second of pickling and baking
After dry, can get monolithic and total weight is thinned is 0.45-1.45g and the uniform silicon wafer of micro-structure, improves battery conductive performance
0.01-0.03%.
Embodiment one:
Imbrication battery process for etching having a size of 160mm, specifically includes:
S1: oxidation
Silicon wafer enters in 2# oxidation trough from 1# feeding groove, synchronizes and is passed through ozone gas, and the medicine of 2# oxidation trough is arranged in advance
Liquid, the i.e. mixed liquor of the water of the sodium hydroxide of 4L and 220L, oxidizing temperature are 60 DEG C, oxidization time 3min.In oxidation process,
Fluid infusion of rotation after 500 frames of every production, every basket of installation silicon wafer 200, subsequent every basket of installation silicon wafer quantity is identical, no longer heavy
It is multiple；The amount infused of ozone is 10L/h, and the amount infused of sodium hydroxide is 0.1L.Silicon wafer after oxidation enters back into clear in 3# rinsing bowl
Wash 2min.
S2: first time pickling
Silicon wafer enters from 3# rinsing bowl carries out pickling in 4# descaling bath, wherein medical fluid in 4# descaling bath by 40L hydrogen fluorine
The water of acid and 260L mix, at normal temperature pickling 3min.In first time acid cleaning process, rotation one after 500 frames of every production
Secondary fluid infusion, the amount infused of hydrofluoric acid are 0.5L.It enters back into 5# rinsing bowl and is cleaned after pickling, scavenging period 2min.
S3: pretreatment
Silicon wafer from 5# rinsing bowl enter 6# rough polishing slot in corroded, the medical fluid in 6# rough polishing slot by 7L sodium hydroxide
It is mixed to form with the water of 220L, is that rough polishing corrodes 3min in 80 DEG C in temperature.During rough polishing, rotation after 500 frames of every production
Fluid infusion, the amount infused of sodium hydroxide are 0.5L.Subsequently into being cleaned in 7# precleaning spout, the medical fluid in 7# precleaning spout by
The water of the sodium hydroxide of 4L, the hydrogen peroxide of 12L and 220L mixes, and is to clean 2min in 60 DEG C in temperature.In prerinse
Cheng Zhong, fluid infusion of rotation after 500 frames of every production, the amount infused of hydrogen peroxide are 1L, and the amount infused of sodium hydroxide is 0.1L.Again into
Enter 8# rinsing bowl to be cleaned, scavenging period 2min.
S4: making herbs into wool
Silicon wafer enters from 8# rinsing bowl carries out making herbs into wool in 9# texturing slot, the medical fluid of 9# texturing slot is by 10L sodium hydroxide, 2L
The water of additive and 230L mix, and are making herbs into wool 6.5min in 80 DEG C in temperature.During making herbs into wool, after 250 frames of every production
Fluid infusion of rotation, the amount infused of sodium hydroxide are 0.8L, and the amount infused of additive is 0.1L.Then 10# rinsing bowl is entered back into
Interior cleaning, scavenging period 2min.
S5: post-processing
Silicon wafer enters after 11# from 10# rinsing bowl to be cleaned in rinse bath, the medical fluid after 11# in rinse bath by 12L dioxygen
The water of water, the sodium hydroxide of 4L and 220L is mixed to form, and cleans 1.5min under conditions of temperature is 60 DEG C.In rear cleaning process
In, fluid infusion of rotation after 500 frames of every production, the amount infused of hydrogen peroxide is 1L, and the amount infused of sodium hydroxide is 0.1L.Then again
It is cleaned in into 12# rinsing bowl, scavenging period 2min.
S6: second pickling
Silicon wafer enters in 13# descaling bath out of 12# rinsing bowl carries out pickling, and the medical fluid in 13# descaling bath is by 20L hydrogen fluorine
Acid, 20L hydrochloric acid and 130L water are mixed to form, and carry out pickling 3min at normal temperature.In second of acid cleaning process, every production 500
Fluid infusion of rotation after frame, the amount infused of hydrofluoric acid are 0.3L, and the amount infused of hydrochloric acid is 0.3L.It enters back into clear in 14# rinsing bowl
Wash 2min.
S7: drying
Silicon wafer completely lift in slot and is cleaned from entering 15# in 14# rinsing bowl, and it is 70 DEG C that 15#, which completely lifts hot water temperature in slot, clearly
Wash 2min；16# drying tank is entered back into be dried, 80 DEG C at a temperature of dry 6min；17# blanking groove is entered back into come out.
Performance parameter is carried out to the silicon wafer after making herbs into wool and appearance is tested.The silicon before and after test making herbs into wool on electronic balance instrument
Sheet weight, and its two-sided thinned weight is calculated, electronic balance is with model FA124；And with D8 reflectance test instrument to making herbs into wool
Silicon wafer afterwards carries out reflectivity detection, following identical.As shown in table 1, the two-sided thinned weight of the silicon wafer obtained in the present embodiment with
For central point reflectivity compared with standard requirements, the two-sided thinned weight of the silicon wafer of the present embodiment one is 0.53g, central point reflectivity
Are as follows: 7.8%, respectively less than standard requirements.Table 2 is the making herbs into wool silicon wafer with the present embodiment and the electrical parameter with prior art making herbs into wool silicon wafer
The comparison done, it is known that the silicon wafer of the 160mm done according to this process for etching is mentioned than the transformation efficiency for the silicon wafer that common process is 160mm
It is high by 0.03%.Microscopic appearance of the silicon wafer under 3000 times of scanning electron microscope after making herbs into wool, as shown in fig. 2, it can be seen that silicon wafer
Surface forms that one layer of structure is small, uniformly and is covered with the flannelette in entire silicon face, and silicon wafer complete appearance, without obvious color difference, it is dirty,
Spot or rupture.The uniform consistent flannelette of convex-concave can increase light in the refraction number on solar cell piece surface, be conducive to cell piece
Absorption to light improves the reflectivity for reducing light, improves short circuit current, the final photoelectric conversion efficiency for improving battery.
1 embodiment of table, one test result and standard requirements compare
The Contrast of Electrical Parameter of table 2 embodiment one and the prior art
Embodiment two:
Imbrication battery process for etching having a size of 200mm, specifically includes:
S1: oxidation
Silicon wafer enters in 2# oxidation trough from 1# feeding groove, synchronizes and is passed through ozone gas, and the medicine of 2# oxidation trough is arranged in advance
Liquid, the i.e. mixed liquor of the water of the sodium hydroxide of 6L and 240L, oxidizing temperature are 60 DEG C, oxidization time 3min.In oxidation process,
Fluid infusion of rotation after 500 frames of every production, the amount infused of ozone is 15L/h, and the amount infused of sodium hydroxide is 0.15L.After oxidation
Silicon wafer enter back into and clean 2min in 3# rinsing bowl.
S2: first time pickling
Silicon wafer enters from 3# rinsing bowl carries out pickling in 4# descaling bath, wherein medical fluid in 4# descaling bath by 50L hydrogen fluorine
The water of acid and 280L mix, at normal temperature pickling 3min.In first time acid cleaning process, rotation one after 500 frames of every production
Secondary fluid infusion, the amount infused of hydrofluoric acid are 0.8L.It enters back into 5# rinsing bowl and is cleaned after pickling, scavenging period 2min.
S3: pretreatment
Silicon wafer from 5# rinsing bowl enter 6# rough polishing slot in corroded, the medical fluid in 6# rough polishing slot by 9L sodium hydroxide
It is mixed to form with the water of 240L, is that rough polishing corrodes 3min in 80 DEG C in temperature.During rough polishing, rotation after 500 frames of every production
Fluid infusion, the amount infused of sodium hydroxide are 0.8L.Subsequently into being cleaned in 7# precleaning spout, the medical fluid in 7# precleaning spout by
The water of the sodium hydroxide of 6L, the hydrogen peroxide of 14L and 240L mixes, and is to clean 2min in 60 DEG C in temperature.In prerinse
Cheng Zhong, fluid infusion of rotation after 500 frames of every production, the amount infused of hydrogen peroxide are 1.5L, and the amount infused of sodium hydroxide is 0.15L.
It enters back into 8# rinsing bowl to be cleaned, scavenging period 2min.
S4: making herbs into wool
Silicon wafer enters from 8# rinsing bowl carries out making herbs into wool in 9# texturing slot, the medical fluid of 9# texturing slot is by 12L sodium hydroxide, 3L
The water of additive and 250L mix, and are making herbs into wool 6.5min in 80 DEG C in temperature.During making herbs into wool, after 250 frames of every production
Fluid infusion of rotation, the amount infused of sodium hydroxide are 1.2L, and the amount infused of additive is 0.15L.Then 10# rinsing bowl is entered back into
Interior cleaning, scavenging period 2min.
S5: post-processing
Silicon wafer enters after 11# from 10# rinsing bowl to be cleaned in rinse bath, the medical fluid after 11# in rinse bath by 14L dioxygen
The water of water, the sodium hydroxide of 6L and 240L is mixed to form, and cleans 1.5min under conditions of temperature is 60 DEG C.In rear cleaning process
In, fluid infusion of rotation after 500 frames of every production, the amount infused of hydrogen peroxide is 1.5L, and the amount infused of sodium hydroxide is 0.15L.So
After enter back into cleaning, scavenging period 2min in 12# rinsing bowl.
S6: second pickling
Silicon wafer enters in 13# descaling bath out of 12# rinsing bowl carries out pickling, and the medical fluid in 13# descaling bath is by 30L hydrogen fluorine
Acid, 30L hydrochloric acid and 150L water are mixed to form, and carry out pickling 3min at normal temperature.In second of acid cleaning process, every production 500
Fluid infusion of rotation after frame, the amount infused of hydrofluoric acid are 0.6L, and the amount infused of hydrochloric acid is 0.6L.It enters back into clear in 14# rinsing bowl
Wash 2min.
S7: drying
Silicon wafer completely lift in slot and is cleaned from entering 15# in 14# rinsing bowl, and it is 70 DEG C that 15#, which completely lifts hot water temperature in slot, clearly
Wash 2min；16# drying tank is entered back into be dried, 80 DEG C at a temperature of dry 6min；17# blanking groove is entered back into come out.
Performance parameter is carried out to the silicon wafer after making herbs into wool and appearance is tested.As shown in table 3, the silicon obtained in the present embodiment
With central point reflectivity compared with standard requirements, the two-sided thinned weight of the silicon wafer of the present embodiment one is the two-sided thinned weight of piece
0.82g, central point reflectivity are as follows: 7.8%, respectively less than standard requirements.Table 4 be with the making herbs into wool silicon wafer of the present embodiment with existing skill
The comparison that the electrical parameter of art making herbs into wool silicon wafer is done, it is known that the silicon wafer of the 200mm done according to this process for etching is 200mm than common process
The transformation efficiency of silicon wafer improve 0.03%.Microscopic appearance of the silicon wafer under 3000 times of scanning electron microscope after making herbs into wool, such as Fig. 3
It is shown, it can be seen that one layer of structure of silicon chip surface formation is small, convex-concave is uniform and is covered with the flannelette in entire silicon face, and outside silicon wafer
It sees completely, without obvious color difference, dirty, spot or rupture.In the present embodiment, either performance parameter and micrograph is qualified.
3 embodiment of table, two test result and standard requirements compare
The Contrast of Electrical Parameter of table 4 embodiment two and the prior art
Embodiment three:
Imbrication battery process for etching having a size of 260mm, specifically includes:
S1: oxidation
Silicon wafer enters in 2# oxidation trough from 1# feeding groove, synchronizes and is passed through ozone gas, and the medicine of 2# oxidation trough is arranged in advance
Liquid, the i.e. mixed liquor of the water of the sodium hydroxide of 8L and 260L, oxidizing temperature are 60 DEG C, oxidization time 3min.In oxidation process,
Fluid infusion of rotation after 500 frames of every production, the amount infused of ozone is 20L/h, and the amount infused of sodium hydroxide is 0.2L.After oxidation
Silicon wafer, which enters back into, cleans 2min in 3# rinsing bowl.
S2: first time pickling
Silicon wafer enters from 3# rinsing bowl carries out pickling in 4# descaling bath, wherein medical fluid in 4# descaling bath by 70L hydrogen fluorine
The water of acid and 300L mix, at normal temperature pickling 3min.In first time acid cleaning process, rotation one after 500 frames of every production
Secondary fluid infusion, the amount infused of hydrofluoric acid are 1.2L.It enters back into 5# rinsing bowl and is cleaned after pickling, scavenging period 2min.
S3: pretreatment
Silicon wafer from 5# rinsing bowl enter 6# rough polishing slot in corroded, the medical fluid in 6# rough polishing slot by 12L hydroxide
The water of sodium and 260L are mixed to form, and are that rough polishing corrodes 3min in 80 DEG C in temperature.During rough polishing, 500 frame rear-wheels of every production
A fluid infusion is changed, the amount infused of sodium hydroxide is 1.2L.Subsequently into being cleaned in 7# precleaning spout, the medical fluid in 7# precleaning spout
It is mixed by the water of the sodium hydroxide of 8L, the hydrogen peroxide of 16L and 260L, is to clean 2min in 60 DEG C in temperature.In prerinse
In the process, fluid infusion of rotation after 500 frames of every production, the amount infused of hydrogen peroxide are 2L, and the amount infused of sodium hydroxide is 0.2L.Again
It is cleaned into 8# rinsing bowl, scavenging period 2min.
S4: making herbs into wool
Silicon wafer enters from 8# rinsing bowl carries out making herbs into wool in 9# texturing slot, the medical fluid of 9# texturing slot is by 14L sodium hydroxide, 4L
The water of additive and 270L mix, and are making herbs into wool 6.5min in 80 DEG C in temperature.During making herbs into wool, after 250 frames of every production
Fluid infusion of rotation, the amount infused of sodium hydroxide are 1.8L, and the amount infused of additive is 0.2L.Then 10# rinsing bowl is entered back into
Interior cleaning, scavenging period 2min.
S5: post-processing
Silicon wafer enters after 11# from 10# rinsing bowl to be cleaned in rinse bath, the medical fluid after 11# in rinse bath by 16L dioxygen
The water of water, the sodium hydroxide of 8L and 260L is mixed to form, and cleans 1.5min under conditions of temperature is 60 DEG C.In rear cleaning process
In, fluid infusion of rotation after 500 frames of every production, the amount infused of hydrogen peroxide is 2L, and the amount infused of sodium hydroxide is 0.2L.Then again
It is cleaned in into 12# rinsing bowl, scavenging period 2min.
S6: second pickling
Silicon wafer enters in 13# descaling bath out of 12# rinsing bowl carries out pickling, and the medical fluid in 13# descaling bath is by 40L hydrogen fluorine
Acid, 40L hydrochloric acid and 180L water are mixed to form, and carry out pickling 3min at normal temperature.In second of acid cleaning process, every production 500
Fluid infusion of rotation after frame, the amount infused of hydrofluoric acid are 0.9L, and the amount infused of hydrochloric acid is 0.9L.It enters back into clear in 14# rinsing bowl
Wash 2min.
S7: drying
Silicon wafer completely lift in slot and is cleaned from entering 15# in 14# rinsing bowl, and it is 70 DEG C that 15#, which completely lifts hot water temperature in slot, clearly
Wash 2min；16# drying tank is entered back into be dried, 80 DEG C at a temperature of dry 6min；17# blanking groove is entered back into come out.
Performance parameter is carried out to the silicon wafer after making herbs into wool and appearance is tested.As shown in table 5, the silicon obtained in the present embodiment
With central point reflectivity compared with standard requirements, the two-sided thinned weight of the silicon wafer of the present embodiment one is the two-sided thinned weight of piece
1.39g, central point reflectivity are as follows: 7.8%, respectively less than standard requirements.Table 6 be with the making herbs into wool silicon wafer of the present embodiment with existing skill
The comparison that the electrical parameter of art making herbs into wool silicon wafer is done, it is known that the silicon wafer of the 260mm done according to this process for etching is done than existing process for etching
The transformation efficiency of silicon wafer of 260mm improve 0.03%.Microcosmic shape of the silicon wafer under 3000 times of scanning electron microscope after making herbs into wool
Looks, as shown in Figure 4, it can be seen that one layer of structure of silicon chip surface formation is small, convex-concave is uniform and is covered with the flannelette in entire silicon face,
And silicon wafer complete appearance, without obvious color difference, dirty, spot or rupture.In the present embodiment, either performance parameter and micrograph
It is qualified.
5 embodiment of table, three test result and standard requirements compare
The Contrast of Electrical Parameter of table 6 embodiment three and the prior art
The advantages and positive effects of the present invention are:
1, process for etching designed by the invention is especially adapted for use in the making herbs into wool having a size of 160-260mm square silicon wafer,
A kind of oxide layer being easily removed is formed by the way that the metal impurities of silicon chip surface are carried out oxidation in advance, then after first time pickling
The oxide layer is complexed, forms a kind of water-soluble complex compound, and then the oil for being pasted on the oxide layer can be effectively removed
Dirt improves silicon chip surface cleanliness, provides good surface foundation for the subsequent flannelette for preparing, be conducive to micro- knot in silicon chip battery face
Structure is more uniform, and silicon chip surface silica layer depth, that is, thinning single surface depth after first time pickling is 1-2um, completely may be used
Control.
2, pretreatment includes rough polishing processing and prerinse processing, and the purpose of rough polishing processing is to remove the cutting damage of silicon chip surface
Hurt layer, form an even curface after being thinned, is conducive to subsequent prepare flannelette；Prerinse is the removal remaining metal of silicon chip surface
Ion and organic matter.Making herbs into wool is exactly to form a pyramid shape flannelette that is small, uniform and being covered with entire silicon face in silicon chip surface.System
Silicon wafer after suede successively post-processed again, second of pickling and drying, wherein post-processing is that silicon chip surface is remaining adds for removal
Add agent and organic matter；Second of pickling is the silica and metal ion for removing silicon wafer and marking, and forms the preferable suede of hydrophobicity
Face；Drying includes that hot water completely lifts slot and drying tank, and hot water cleaning silicon chip Liquid Residue reduces the water mark of silicon chip surface, is conducive to
Subsequent drying；Drying tank is the water mark with hot blast drying silicon chip surface；Silicon wafer after drying comes out from blanking groove again, finally obtains
Obtaining monolithic and total weight is thinned is 0.45-1.45g and the uniform silicon wafer of micro-structure, and battery conductive performance is made to improve 0.01-
0.03%.
3, rinsing bowl, purpose are equipped with after oxidation, first time pickling, pretreatment, making herbs into wool, post-processing and second of pickling
It is to remove the medical fluid on silicon wafer surface layer, while can remove the remaining organic solvent of silicon chip surface and metal ion, is conducive to remove silicon
The residual of the metal impurities on piece surface improves silicon chip surface cleanliness, to promote the electrical property of battery.
The embodiments of the present invention have been described in detail above, content is only the preferred embodiment of the present invention, no
It can be believed to be used to limit the scope of the invention.Any changes and modifications in accordance with the scope of the present application,
It should still fall within the scope of the patent of the present invention.
Claims (10)
1. a kind of large scale imbrication battery process for etching, which is characterized in that carry out oxidation and the before making herbs into wool, including to silicon wafer
Pickling processes, the oxidation are to carry out oxidation to the surface of the silicon wafer after feeding to form layer of oxide layer；Described
Pickling is that greasy dirt of the pickling to remove the oxide layer and be pasted in the oxide layer is carried out to the oxide layer.
2. a kind of large scale imbrication battery process for etching according to claim 1, which is characterized in that the medical fluid of the oxidation
Including ozone and sodium hydroxide, the amount infused of the ozone is 5-25L/h, and the solution ratio of the sodium hydroxide is 3-4%.
3. a kind of large scale imbrication battery process for etching according to claim 2, which is characterized in that the temperature of the oxidation
It is 40-80 DEG C, time 1-5min.
4. a kind of large scale imbrication battery process for etching according to claim 1, which is characterized in that the first time pickling
Medical fluid used is solution than the hydrofluoric acid for 10-15%, and the first time pickling temperature is room temperature, pickling time 1-5min.
5. a kind of large scale imbrication battery process for etching according to claim 1-4, which is characterized in that described
The final step of oxidation and the first time pickling is equipped with rinsing bowl.
6. a kind of large scale imbrication battery process for etching according to claim 5, which is characterized in that the making herbs into wool is in hydrogen
Carried out in sodium oxide molybdena medical fluid, also add several additives, the sodium hydroxide solution ratio is 4-4.5%, the additive it is molten
Liquor ratio is 0.6-1%.
7. a kind of large scale imbrication battery process for etching according to claim 6, which is characterized in that the making herbs into wool temperature is
60-100 DEG C, time 3.5-9.5min.
8. a kind of large scale imbrication battery process for etching according to claim 6 or 7, which is characterized in that before the making herbs into wool
After be respectively equipped with pretreatment and post-processing, the pretreatment is placed in after the first time pickling, it is described pretreatment include rough polishing
And prerinse；The post-processing is cleaned after including；The rough polishing medical fluid is solution than the sodium hydroxide for 4-4.5%；It is described pre-
Cleaning the rear cleaning medical fluid is hydrogen peroxide and sodium hydroxide, and the solution ratio of the hydrogen peroxide and the sodium hydroxide is respectively
4-7% and 0.2-0.5%.
9. a kind of large scale imbrication battery process for etching according to claim 8, which is characterized in that in the post-processing
After be successively arranged second of pickling and drying, second of pickling medical fluid is the mixed liquor of hydrofluoric acid and hydrochloric acid, the hydrogen fluorine
Acid solution ratio is 10-15%, and the hydrochloric acid solution ratio is 10-15%；The drying completely lifts again high temperature drying, institute for first hot water
Stating drying temperature is 60-100 DEG C.
10. a kind of large scale imbrication battery process for etching according to claim 9, which is characterized in that it is described pretreatment,
The final step of the making herbs into wool and the post-processing and second of pickling is equipped with the rinsing bowl, the rinsing bowl solution
For pure water, washing time 0.5-3.5min.
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| CN112713103A (en) * | 2021-03-29 | 2021-04-27 | 西安奕斯伟硅片技术有限公司 | Method for measuring metal content in silicon wafer |
| CN114392966A (en) * | 2021-12-29 | 2022-04-26 | 江苏时代华宜电子科技有限公司 | Automatic cleaning equipment and cleaning method for molybdenum alloy substrate |
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