CN109267154A - Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method - Google Patents
Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method Download PDFInfo
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- CN109267154A CN109267154A CN201811139690.3A CN201811139690A CN109267154A CN 109267154 A CN109267154 A CN 109267154A CN 201811139690 A CN201811139690 A CN 201811139690A CN 109267154 A CN109267154 A CN 109267154A
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000005520 cutting process Methods 0.000 title claims abstract description 24
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 23
- 238000005530 etching Methods 0.000 title claims abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 54
- 239000010703 silicon Substances 0.000 claims abstract description 54
- 210000002268 wool Anatomy 0.000 claims abstract description 41
- 235000008216 herbs Nutrition 0.000 claims abstract description 38
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 14
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 8
- 239000010452 phosphate Substances 0.000 claims abstract description 8
- -1 siloxanes Chemical class 0.000 claims abstract description 8
- 125000000129 anionic group Chemical group 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 32
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 26
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 22
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 9
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 6
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 229910001868 water Inorganic materials 0.000 claims description 5
- 238000002242 deionisation method Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 3
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims 5
- 229940068984 polyvinyl alcohol Drugs 0.000 claims 2
- 238000006136 alcoholysis reaction Methods 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 20
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000002310 reflectometry Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- NONFLFDSOSZQHR-UHFFFAOYSA-N 3-(trimethylsilyl)propionic acid Chemical compound C[Si](C)(C)CCC(O)=O NONFLFDSOSZQHR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- GTTGLTZAOFBCRM-UHFFFAOYSA-N P(O)(O)(O)=O.C[SiH](C)C Chemical compound P(O)(O)(O)=O.C[SiH](C)C GTTGLTZAOFBCRM-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02363—Special surface textures of the semiconductor body itself, e.g. textured active layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic Table
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Electromagnetism (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Weting (AREA)
Abstract
The invention discloses a kind of Buddha's warrior attendant wire cutting monocrystalline silicon surface etching methods, anionic siloxanes phosphate surfactant additive is prepared first, then PVA aqueous solution is prepared, additive and PVA aqueous solution are added in aqueous slkali, prepare Woolen-making liquid: after the removal of silicon wafer damaging layer, silicon wafer is put into Woolen-making liquid and carries out making herbs into wool, after the completion of making herbs into wool, neutralize the remaining aqueous slkali of silicon chip surface and removal metal ion, finally, silicon wafer in dryer under nitrogen protection with quickly being dried, while effectively removing silicon chip surface droplet, silicon chip surface is prevented to be oxidized again.Wet-method etching new method proposed by the present invention, compared to using conventional KOH-IPA process for etching, the surface average reflectance of Buddha's warrior attendant wire cutting monocrystalline silicon reduces 1.1% after making herbs into wool, and minority carrier life time improves 20%, and the making herbs into wool time does not increase but.
Description
Technical field
The invention belongs to technical field of solar batteries, more particularly to a kind of Buddha's warrior attendant wire cutting monocrystalline silicon surface making herbs into wool side
Method.
Background technique
At present in photovoltaic industry, the Buddha's warrior attendant line cutting technology of monocrystalline silicon replacing traditional mortar wire cutting and gradually at
It is in particular in that cutting speed is fast, joint-cutting loss is low, surface damage mainly due to its apparent cost advantage for mainstream technology
Hurt that layer is shallow, environmental pollution is small etc..The monocrystalline silicon making herbs into wool of Buddha's warrior attendant wire cutting, overwhelming majority enterprise still uses standard at present
Mortar wire cutting monocrystalline silicon wet-method etching.Its making herbs into wool chemical reagent is mainly alkali (potassium hydroxide (KOH or sodium hydroxide
(NaOH)), isopropanol (IPA), additive etc., the main function of isopropanol are the hydrogen for inhibiting to generate in chemical reaction process
Bubble, to eliminate the bubble spot of silicon chip surface, still, there are two disadvantages for this KOH-IPA etchant solution.First the disadvantage is that
The lasting evaporation of IPA in corrosion process, making herbs into wool temperature is usually maintained in 80 DEG C, and the boiling point of IPA is 82.4 DEG C, therefore, is being made
It constantly to add IPA during suede or carry out making herbs into wool in a closed container, this will increase dramatically the cost of making herbs into wool.
Second the disadvantage is that, KOH-IPA corrosive liquid is very sensitive to the monocrystalline silicon characteristic of cutting, that is to say, different types of silicon wafer (ratio
The different parts of such as silicon single crystal rod, different manufacturers) pyramid size, pattern, the density etc. that obtain after making herbs into wool is endless
Exactly the same.
Some researches show that the monocrystalline silicon piece of Buddha's warrior attendant wire cutting exists on surface with a thickness of 200~600nm's or so in recent years
Amorphous silicon layer, this layer of amorphous silicon will slow down the process of chemical attack during wet-method etching, so that the making herbs into wool time
It is longer than traditional mortar cutting silicon wafer, and making herbs into wool effect is also less better.It therefore, cannot be complete for silicon wafer cut by diamond wire
The full wet-method texturing manufacturing process using mortar cutting silicon wafer, it should improve on this basis.
Summary of the invention
The object of the present invention is to provide a kind of more efficient Buddha's warrior attendant wire cutting monocrystalline silicon surface etching methods.
For this purpose, the technical solution adopted by the present invention is that such: Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method, feature
It is: the following steps are included:
1) prepare anionic siloxanes phosphate surfactant additive: taking weight percent is the three of 1.0~2.0%
(trimethyl silane) phosphate (TMSP, molecular formula C9H27O4PSi3), weight percent be 0.2~0.5% tributyl phosphate
(TBP, molecular formula C12H27O4P), surplus is deionized water, is sufficiently dissolved；
2) prepared by PVA aqueous solution: 1.0~2.0gPVA17-88 (degree of polymerization 1700, alcohol being added in 30g deionized water
Xie Du be 88% polyvinyl alcohol), 0.1~0.3g octanol, heat with water-bath and water temperature is gradually heated up by the mode stirred, liter
Warm rate is no more than 2 DEG C/min, and temperature stops heating after reaching 95 DEG C, cooling straight room temperature is stand-by；
3) aqueous slkali (weight the preparation of Woolen-making liquid: is added in the resulting PVA aqueous solution of the additive and step 2) of step 1)
KOH the or NaOH aqueous solution that percentage is 1.0~2.0%) in, additive by weight percentage: PVA aqueous solution: aqueous slkali=
0.1~0.3:1:1 is uniformly mixed；
4) silicon wafer damaging layer removes: hydrogen peroxide (H2O2) with alkali (concentration be 20% KOH or NaOH) be according to volume ratio
1:15~20 are configured to mixed liquor, are heated to 50~60 DEG C, then the monocrystalline silicon piece of Buddha's warrior attendant wire cutting are put into wherein, after 120s
It takes out, then is rinsed 3 times with deionized water；
5) it silicon wafer wool making: is made being put into the Woolen-making liquid of step 3) preparation by the resulting monocrystalline silicon piece of step 4)
Suede, making herbs into wool temperature are 95 DEG C, and the time is 900~1800s, then take out silicon wafer and are rinsed 3~5 times with deionized water；Making herbs into wool is complete
Cheng Hou is existed to neutralize the remaining aqueous slkali of silicon chip surface and removal metal ion using the hydrochloric acid (HCl) that concentration is 20%
Pickling 180s is carried out at room temperature, is then rinsed 3 times with deionized water；Later, in order to remove the oxide layer of silicon chip surface, utilization is dense
Degree impregnates 60~90s for 1% hydrofluoric acid (HF) at room temperature, is then rinsed 3 times with deionization；Finally, silicon wafer is protected in nitrogen
With quickly being dried in dryer under shield, while being effectively removed silicon chip surface droplet, prevent silicon chip surface again by
Oxidation.
Polyvinyl alcohol (PVA) is white plates, cotton-shaped or pulverulent solids, and fusing point is 230 DEG C, glass transition temperature 75~85
DEG C, embrittlement can just be occurred by being heated to 100 DEG C or more in air.PVA aqueous solution has good hydrophilic and oil-wet behavior, is changing
It learns to play to adsorb in reaction-ure surface in reaction and to form protective film, reduce the effects of interfacial tension, monocrystalline silicon system can be eliminated
The bubble hydrogen generated during suede.Meanwhile PVA aqueous solution lower than 100 DEG C at a temperature of, than 80 DEG C temperature of evaporation capacity of PVA
IPA evaporation capacity under degree is greatly reduced.
Anionic siloxanes phosphate is a kind of tension, super permeability, super wetability and chemistry with ultralow boundary
The high surfactant of stability can be aligned in solution surface, be reduced when it is added in monocrystalline silicon making herbs into wool solution
The surface tension of lye and silicon face improves hydroxide ion (OH-) to the corrosion rate of silicon, shorten Buddha's warrior attendant wire cutting
The making herbs into wool time of silicon wafer.Simultaneously as the addition of surfactant, changes the anisotropic feature of alkali, so that (111) of silicon
Etch ratio (100) face of crystal face is increased larger, and the corrosion rate for reducing by two crystal faces is poor, this is equal to form sample ruler cun
Even, the complete pyramid of shape creates good condition.
In the present invention, KOH-IPA is substituted using KOH-PVA, anionic siloxanes phosphate is as additive, making herbs into wool
Temperature is 95 DEG C, the evaporation of IPA present in conventional KOH-IPA process for etching can be effectively avoided, to different type monocrystalline
The problems such as dependence of silicon, while when solving the amorphous silicon as existing for the monocrystalline silicon surface of Buddha's warrior attendant wire cutting and extending making herbs into wool
Between the problem of.Using wet-method etching new method proposed by the present invention, compared to the KOH-IPA process for etching using routine, making herbs into wool
The surface average reflectance of Buddha's warrior attendant wire cutting monocrystalline silicon reduces 1.1% afterwards, and minority carrier life time improves 20%, and the making herbs into wool time does not have but
There is increase.
Detailed description of the invention
It is described in further detail below in conjunction with attached drawing and embodiments of the present invention
Fig. 1 is the reflectivity of silicon wafer after two kinds of distinct methods making herbs into wool；S1 is the reflectivity of silicon wafer after conventional making herbs into wool, and S2 is this
The reflectivity of silicon wafer after invention the method making herbs into wool.
Specific embodiment
Etching method described in the present embodiment, comprising the following steps:
1) anionic siloxanes phosphate surfactant additive: it is formed and its weight percent is 1.0~2.0%
Three (trimethyl silane) phosphate (TMSP, molecular formula C9H27O4PSi3), 0.2~0.5% tributyl phosphate (TBP, molecular formula
For C12H27O4P), surplus is deionized water (resistivity is greater than 1.0M Ω cm).
2) prepared by PVA aqueous solution: 1.0~2.0gPVA17-88 (degree of polymerization 1700, alcohol being added in 30g deionized water
Xie Du be 88% polyvinyl alcohol), 0.1~0.3g octanol, heat with water-bath and water temperature is gradually heated up by the mode stirred, liter
Warm rate is no more than 2 DEG C/min, and temperature stops heating after reaching 95 DEG C, cooling straight room temperature is stand-by.
3) preparation of Woolen-making liquid: aqueous slkali (weight is added in the resulting PVA aqueous solution of the additive and step 2 that step 1 is matched
Measure KOH the or NaOH aqueous solution that percentage is 1.0~2.0%) in, (additive: PVA aqueous solution: aqueous slkali by weight percentage
=0.1~0.3:1:1) it is uniformly mixed.
4) silicon wafer damaging layer removes: utilizing hydrogen peroxide (H2O2) and alkali (KOH or NaOH) removal silicon chip surface contained by impurity
And mechanical damage layer, dominant mechanism are: H2O2It is reacted with silicon wafer and generates oxidation film, the oxidation film is again by caustic corrosion, after corrosion
It aoxidizes again, silicon powder, resin, metal for being constantly repeated with oxidation and corrosion, therefore being attached to silicon chip surface etc.
Grain is also fallen into cleaning solution with corrosion layer, and the organic matter of silicon chip surface is broken down into CO2、H2O and be removed.Concrete technology
Are as follows: hydrogen peroxide (H2O2) it with alkali (KOH or NaOH that concentration is 20%) according to volume ratio is that 1:15~20 are configured to mixed liquor,
50~60 DEG C are heated to, then the monocrystalline silicon piece of Buddha's warrior attendant wire cutting is put into wherein, is taken out after 120s, then is rinsed with deionized water
3 times.
5) monocrystalline silicon piece for eliminating surface impurity and damaging layer by step 4 silicon wafer wool making: is put into what step 3 was prepared
Making herbs into wool is carried out in Woolen-making liquid, making herbs into wool temperature is 95 DEG C, and the time is 900~1800s, then takes out silicon wafer and is rinsed with deionized water
3~5 times.It is 20% using concentration to neutralize the remaining aqueous slkali of silicon chip surface and removal metal ion after the completion of making herbs into wool
Hydrochloric acid (HCl) carries out pickling 180s at room temperature, is then rinsed 3 times with deionized water.Later, in order to remove silicon chip surface
Oxide layer is impregnated 60~90s using the hydrofluoric acid (HF) that concentration is 1% at room temperature, is then rinsed 3 times with deionization.Finally,
Silicon wafer with quickly being dried in dryer, while effectively removing silicon chip surface droplet, prevents silicon wafer under nitrogen protection
Surface is oxidized again.
6) test analysis:
In order to which with conventional alkali (KOH or NaOH), compared with IPA making herbs into wool, according to above-mentioned steps, PVA is substituted for IPA, does not have
Using anionic siloxanes phosphate surfactant additive, other techniques are identical, and silicon wafer is anti-after measurement making herbs into wool
Penetrate rate and minority carrier life time.Fig. 1 gives the variation of silicon wafer reflectivity after two methods making herbs into wool, it will be seen from figure 1 that using this hair
After the new method making herbs into wool of bright use, average reflectance of the silicon wafer within the scope of a length of 300~1100nm of sunlight wave is 11.4%,
And conventional etching method is 12.5%, reflectivity reduces 1.1%.Further by comparing using two kinds of distinct methods making herbs into wool
Silicon chip minority carrier life afterwards, silicon chip minority carrier life is improved than the silicon wafer of conventional making herbs into wool after the new method making herbs into wool that the present invention uses
20%.Moreover, the evaporation capacity by the PVA in comparison new method Woolen-making liquid after making herbs into wool, finds PVA waving during making herbs into wool
Hair is far smaller than the volatilization of Traditional IP A.
Claims (1)
1. Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method, it is characterised in that: the following steps are included:
1) prepare anionic siloxanes phosphate surfactant additive: taking weight percent is the three (three of 1.0~2.0%
Methyl-monosilane) phosphate (TMSP), the tributyl phosphate (TBP) that weight percent is 0.2~0.5%, surplus is deionized water,
Sufficiently dissolution；
2) prepared by PVA aqueous solution: be added in 30g deionized water 1.0~2.0g degree of polymerization be 1700, alcoholysis degree be 88% it is poly-
Vinyl alcohol (PVA17-88), 0.1~0.3g octanol, are heated with water-bath and water temperature is gradually heated up by the mode stirred, heating speed
Rate is no more than 2 DEG C/min, and temperature stops heating after reaching 95 DEG C, cooling straight room temperature is stand-by；
3) preparation of Woolen-making liquid: it is 1.0 that weight percent, which is added, in the resulting PVA aqueous solution of the additive and step 2) of step 1)
In the aqueous slkali of~2.0% KOH or NaOH, additive by weight percentage: PVA aqueous solution: aqueous slkali=0.1~0.3:1:
1 is uniformly mixed；
4) silicon wafer damaging layer removes: H2O2The KOH for being 20% with concentration or NaOH is that 1:15~20 are configured to mix according to volume ratio
Liquid is closed, 50~60 DEG C is heated to, then the monocrystalline silicon piece of Buddha's warrior attendant wire cutting is put into wherein, is taken out after 120s, then uses deionization
Water rinses 3 times；
5) silicon wafer wool making: making herbs into wool is carried out being put into the Woolen-making liquid of step 3) preparation by the resulting monocrystalline silicon piece of step 4), is made
Suede temperature is 95 DEG C, and the time is 900~1800s, then takes out silicon wafer and is rinsed 3~5 times with deionized water；After the completion of making herbs into wool,
In order to neutralize the remaining aqueous slkali of silicon chip surface and removal metal ion, using concentration be 20% hydrochloric acid (HCl) at room temperature
Pickling 180s is carried out, is then rinsed 3 times with deionized water；Later, in order to remove the oxide layer of silicon chip surface, it is using concentration
1% hydrofluoric acid (HF) impregnates 60~90s at room temperature, is then rinsed 3 times with deionization；Finally, silicon wafer is under nitrogen protection
With quickly being dried in dryer, while being effectively removed silicon chip surface droplet, silicon chip surface is prevented to be oxidized again.
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| CN201811139690.3A CN109267154A (en) | 2018-09-28 | 2018-09-28 | Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method |
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| CN201811139690.3A CN109267154A (en) | 2018-09-28 | 2018-09-28 | Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| 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 |
| CN113913188A (en) * | 2021-12-14 | 2022-01-11 | 绍兴拓邦电子科技有限公司 | Monocrystalline silicon texturing agent and preparation method of textured monocrystalline silicon |
| CN114573931A (en) * | 2022-03-04 | 2022-06-03 | 中国工程物理研究院激光聚变研究中心 | Preparation and application of colloid for repairing damaged pit on surface of optical element |
| CN114573931B (en) * | 2022-03-04 | 2023-05-09 | 中国工程物理研究院激光聚变研究中心 | Preparation and application of colloid for repairing surface damage pits of optical elements |
| CN115000241A (en) * | 2022-05-27 | 2022-09-02 | 重庆臻宝实业有限公司 | Low-reflectivity monocrystalline silicon and texturing method thereof |
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