CN103132079A - Additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and application method thereof - Google Patents
Additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and application method thereof Download PDFInfo
- Publication number
- CN103132079A CN103132079A CN2013100495527A CN201310049552A CN103132079A CN 103132079 A CN103132079 A CN 103132079A CN 2013100495527 A CN2013100495527 A CN 2013100495527A CN 201310049552 A CN201310049552 A CN 201310049552A CN 103132079 A CN103132079 A CN 103132079A
- Authority
- CN
- China
- Prior art keywords
- additive
- wool
- acid
- making herbs
- diamond wire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000654 additive Substances 0.000 title claims abstract description 76
- 230000000996 additive effect Effects 0.000 title claims abstract description 76
- 238000005520 cutting process Methods 0.000 title claims abstract description 64
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 59
- 239000002253 acid Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 48
- 230000008569 process Effects 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 235000008216 herbs Nutrition 0.000 claims description 76
- 210000002268 wool Anatomy 0.000 claims description 76
- 229910003460 diamond Inorganic materials 0.000 claims description 58
- 239000010432 diamond Substances 0.000 claims description 58
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 52
- 229920005591 polysilicon Polymers 0.000 claims description 49
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 28
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 26
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 26
- -1 polyoxyethylene Polymers 0.000 claims description 26
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 25
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 25
- 239000010985 leather Substances 0.000 claims description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 8
- 238000006136 alcoholysis reaction Methods 0.000 claims description 6
- 238000002310 reflectometry Methods 0.000 abstract description 6
- 239000002202 Polyethylene glycol Substances 0.000 abstract 1
- 230000009972 noncorrosive effect Effects 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 23
- 229910052710 silicon Inorganic materials 0.000 description 21
- 239000010703 silicon Substances 0.000 description 21
- 238000003756 stirring Methods 0.000 description 16
- 230000009471 action Effects 0.000 description 11
- 239000004570 mortar (masonry) Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 7
- 238000007654 immersion Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000001788 irregular Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003631 wet chemical etching Methods 0.000 description 1
Images
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Weting (AREA)
Abstract
The invention provides an additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and an application method of the additive in the acid texturing process of diamond-wire-cutting polycrystalline silicon slices. The additive for acid texturing comprises the components of polyving akohol, polyethylene glycol and deionized water and is applied to the acid texturing process of diamond-wire-cutting polycrystalline silicon slices. Due to the fact that the additive is applied to the acid texturing process of diamond-wire-cutting polycrystalline silicon slices, reflectivity of the textured diamond-wire-cutting polycrystalline silicon slices is approximately 6% lower than that of the conventionally textured diamond-wire-cutting polycrystalline silicon slices. The additive for acid texturing is non-toxic and non-corrosive, preparation and application processes are simple, and practical application value is high.
Description
Technical field
The present invention relates to sour making herbs into wool additive and preparation method thereof and using method, refer in particular to for the additive of diamond wire cutting polysilicon chip acid making herbs into wool and the using method of cutting polysilicon chip acid leather producing process at diamond wire thereof.
Background technology
Mortar multi-wire saw technology is mainly adopted in the cutting of photovoltaic industry crystal silicon chip used at present, but there are the problems such as cutting technique inefficiency, the cutting processing cost is high, the exhaust emission rear waste mortar of cutting is large in this technology.By contrast, cutting efficiency is high because having, the cutting processing cost is low and the advantage such as clean environment for solid abrasive diamond fretsaw cutting (being called for short the diamond wire cutting) technology, receive increasing concern, be expected to become the future thrust of the hard and fragile material microtomies such as crystalline silicon.
The mortar multi-wire saw is to utilize very long one by one Stainless Steel Wire to be looped around on driving wheel and tightening pulley, carries out the cutting technique of high-speed cutting under the drive of the driving wheel that runs up.In cutting process, line of cut does not carry out machining, and its Main Function is to bring at a high speed cutting zone into take polyoxyethylene glycol and silicon carbide micro-powder as the grinding slurry of main body and to the abrasive material applied load, finally by abrasive material, silicon materials to be carried out the grinding cutting.Diamond fretsaw is normally to electroplate or method that resin is fixing anchors at diamond particles and makes in the Stainless Steel Wire top layer.In cutting process, diamond fretsaw runs up, and with certain pressure, silicon materials is directly carried out the grinding cutting.Compare with " the trisome processing " of mortar multi-wire saw, diamond fretsaw belongs to " disome processing ", its working (machining) efficiency is the several times of mortar multi-wire saw, and need not to add ground slurry when the cutting processing silicon chip, and tooling cost and the environmental pollution of energy decrease silicon chip are little.
Because the incision principle of diamond wire cutting is different from the incision principle of mortar multi-wire saw, so there is very big-difference in the pattern of the silicon chip surface that two kinds of cutting techniques obtain.The pattern that the silicon chip surface of mortar multi-wire saw mainly breaks to form take brittle crush is as main, and there are a lot of small irregular pits (as shown in Figure 1) in silicon chip surface.And the silicon chip surface of diamond wire cutting is except the irregular pit that exists brittle crush to break to form, also there is the smooth cutting line that is formed by the ductile grinding cutting in a large number, so the silicon chip surface of final diamond wire cutting presents the mixing pattern (as shown in Figure 2) of fragility and plasticity.
In the manufacture of solar cells process, silicon chip surface texturing (making herbs into wool) is reducing the surface albedo important role, is also one of effective means that improves the solar cell photoelectric transformation efficiency.The leather producing process of polysilicon chip adopts HF-HNO more at present
3-H
2The wet-chemical etching technique of the acidic solution of O system, this acidic solution utilization be that the various defectives of silicon chip surface are carried out isotropic etch, thereby reduce the silicon chip surface reflectivity.Mortar multiline cut silicon chips surface is mainly irregular pit, and the defect distribution good uniformity is therefore pass through HF-HNO
3-H
2The leather producing process of O system can obtain whole corrosion uniform matte (as shown in Figure 3).But the silicon wafer cut by diamond wire surface is the mixing pattern that irregular pit and smooth cutting line form, and therefore the surface imperfection skewness is by conventional HF-HNO
3-H
2The leather producing process of O system can't obtain whole corrosion uniform matte (as shown in Figure 4).
Application number is the etching method that 201110112185.1 Chinese patent has been announced a kind of silicon wafer cut by diamond wire.This patent is at HF-HNO
3Add H in system
2SO
4Or H
3PO
4, pass through H
2SO
4Or H
3PO
4Catalysis and shock absorption control speed of reaction, thereby reduce the surface albedo of silicon chip after making herbs into wool, but this patent need add a large amount of H
2SO
4Or H
3PO
4Reach the target that reduces reflectivity, the making herbs into wool cost is higher, and the making herbs into wool system of this patent is rich HF system, and after making herbs into wool, silicon chip surface is prone to the dark line that is formed by the deep corrosion hole, can the electricity conversion of solar cell be had a negative impact.Application number is the additive that 201010540761.8 and 201110212876.9 Chinese patent discloses respectively two kinds of polycrystalline silicon wafer acidity texture preparation liquids, and wherein application number is that 201010540761.8 the described additive component of patent is H
2SO
4, H
3PO
4And H
2O, application number are that 201110212876.9 the described additive component of patent is polyvinylpyrrolidone, trolamine and water, and the polysilicon chip that these two pieces of patents all do not indicate this additive application is conventional slurry multiline cut silicon chips or silicon wafer cut by diamond wire.Have no at present specially for the additive of diamond wire cutting polysilicon chip acid making herbs into wool and the report of using method.
So, develop a kind of addition low, can improve the additive that is not prone to the diamond wire cutting polysilicon chip acid making herbs into wool that the silicon chip surface reflectivity is low after dark line, making herbs into wool after diamond wire cutting polysilicon chip matte homogeneity, making herbs into wool and have good actual application value.
Bibliography
1. Tianhe Optical Energy Co., Ltd., Changzhou. a kind of etching method of silicon wafer cut by diamond wire [P]: China, 201110112185.1,2011-04-30.
2. Dalian Sandaaoke Chemistry Co., Ltd.. the acid Wool-making agent of polysilicon solar battery slice is with additive [P]: China, 201010540761.8,2010-11-12.
3. Changzhou time wound Energy Science Co., Ltd. a kind of additive of polycrystalline silicon wafer acidity texture preparation liquid and using method [P]: China, 201110212876.9,2011-07-27.
Summary of the invention
The purpose of this invention is to provide a kind of silicon chip surface matte good uniformity, the obviously dark line of nothing, the additive that is used for the sour making herbs into wool of diamond wire cutting polysilicon chip that reflectivity is low.For this reason, the present invention adopts following technical scheme:
Described additive comprises following component: polyvinyl alcohol, polyoxyethylene glycol and deionized water.
The present invention simultaneously also provides the using method of a kind of this additive in diamond wire cutting polysilicon chip acid leather producing process.The present invention adopts following technical scheme:
Described sour leather producing process comprises the steps: a) additive preparation: polyvinyl alcohol and polyoxyethylene glycol are dissolved in deionized water, make additive; B) prepare acid Woolen-making liquid: hydrofluoric acid and nitric acid are dissolved in make sour mixing solutions in deionized water, the additive that then step a) is made joins in this acid mixing solutions, obtains acid Woolen-making liquid; C) making herbs into wool: diamond wire is cut polysilicon chip be immersed in the acid Woolen-making liquid that step b) obtains and carry out making herbs into wool.
After by above-mentioned additive and this additive of application, diamond wire cutting polysilicon chip being carried out sour making herbs into wool, silicon chip surface matte good uniformity, without obviously dark line, low 6% left and right of diamond wire cutting polysilicon chip after the making herbs into wool of luminance factor routine.And this additive nontoxicity, non-corrosiveness, preparation and operation are simple, have good actual application value.
Description of drawings
Fig. 1 is the scanning electron microscope diagram sheet of mortar multi-wire saw polysilicon chip.
Fig. 2 is the scanning electron microscope diagram sheet of diamond wire cutting polysilicon chip.
Fig. 3 is the scanning electron microscope diagram sheet after the conventional making herbs into wool of mortar multi-wire saw polysilicon chip.
Fig. 4 is the scanning electron microscope diagram sheet after the conventional making herbs into wool of diamond wire cutting polysilicon chip.
Fig. 5 is the scanning electron microscope diagram sheet after diamond wire cutting polysilicon chip is used the additive making herbs into wool of the embodiment of the present invention 2, as seen from the figure, and silicon chip surface matte good uniformity.
Embodiment
The invention provides a kind of additive for diamond wire cutting polysilicon chip acid making herbs into wool and described additive in the using method of diamond wire cutting polysilicon chip acid leather producing process.Described sour making herbs into wool additive comprises following component: polyvinyl alcohol, polyoxyethylene glycol and deionized water, and be applied to the sour making herbs into wool process that diamond wire cuts polysilicon chip.The present invention is by with the sour leather producing process of this additive application in diamond wire cutting polysilicon chip, can make low 6% left and right of reflectivity of diamond wire cutting polysilicon chip after the conventional leather producing process making herbs into wool of luminance factor of diamond wire cutting polysilicon chip after making herbs into wool.Additive nontoxicity of the present invention, non-corrosiveness, preparation and operation are simple, have good actual application value.
Specifically, the invention provides a kind of additive for diamond wire cutting polysilicon chip acid making herbs into wool, described additive comprises following component: polyvinyl alcohol, polyoxyethylene glycol and deionized water.
Wherein, the weight percentage of described polyvinyl alcohol is 0.5 ~ 2%, and the weight percentage of described polyoxyethylene glycol is 0.5 ~ 2%.
The alcoholysis degree of described polyvinyl alcohol is 88% or 98%, and preferred alcoholysis degree is 88%.
The optional business trade mark of described polyvinyl alcohol is the various products such as 0588,0599,1788,1799,2088,2099, and preferred alcoholysis degree is 0588,1788,2088 product of 88% left and right.
The molecular weight of described polyoxyethylene glycol is 200 ~ 5000, and preferred molecular weight is 400 ~ 1000.
The optional molecular weight of described polyoxyethylene glycol is the various products such as 200,300,400,600,1000,1500,2000,4000,5000, and preferred molecular weight is 400,600,1000 product.
The present invention provides the using method of described additive in diamond wire cutting polysilicon chip acid leather producing process simultaneously, and described sour leather producing process comprises the steps: a) additive preparation: polyvinyl alcohol and polyoxyethylene glycol are dissolved in deionized water, make additive; B) prepare acid Woolen-making liquid: hydrofluoric acid and nitric acid are dissolved in make sour mixing solutions in deionized water, the additive that then step a) is made joins in this acid mixing solutions, obtains acid Woolen-making liquid; C) making herbs into wool: diamond wire is cut polysilicon chip be immersed in the acid Woolen-making liquid that step b) obtains and carry out making herbs into wool.
In described step a), the weight percentage of described polyvinyl alcohol is 0.5 ~ 2%.
The optional business trade mark of described polyvinyl alcohol is the various products such as 0588,0599,1788,1799,2088,2099, and preferred alcoholysis degree is 0588,1788,2088 product of 88% left and right.
In described step a), the weight percentage of described polyoxyethylene glycol is 0.5 ~ 2%.
The optional molecular weight of described polyoxyethylene glycol is the various products such as 200,300,400,600,1000,1500,2000,4000,5000, and preferred molecular weight is 400,600,1000 product.
In described step b), the weight percentage of hydrofluoric acid is 5 ~ 25%.
In described step b), the weight percentage of nitric acid is 30 ~ 60%.
In described step b), the weight percentage of additive is 0.4 ~ 1%.
In described step c), the making herbs into wool temperature of making herbs into wool process is 5 ~ 25
oC, the making herbs into wool time is 60 ~ 200s, preferred making herbs into wool temperature is 5 ~ 10
oC, the preferred making herbs into wool time is 100 ~ 150s.
Be further elaborated by the following examples.
Embodiment 1 provides a Comparative Examples, for not using the conventional etching method of additive of the present invention:
Adopt following steps:
1), prepare acid Woolen-making liquid: under stirring action, be that 49% hydrofluoric acid, nitric acid and the 5L deionized water that 8L concentration is 65-68% mix with 2L concentration;
2), making herbs into wool: diamond wire is cut in the above-mentioned acid Woolen-making liquid of polysilicon chip immersion carry out making herbs into wool, the making herbs into wool temperature is 7
oC, the making herbs into wool time is 90s.
Diamond wire cutting polysilicon chip surface albedo after making herbs into wool is 27.0%.Fig. 4 has provided the scanning electron microscope diagram sheet of the diamond wire cutting polysilicon chip surface matte that obtains, and has obtained as can be known from picture that size is uneven, the matte of skewness.
Embodiment 2
Adopt following steps:
A), additive preparation: under stirring action, 1.0g polyvinyl alcohol (the business trade mark 0588) and 1.5g polyoxyethylene glycol (molecular weight 400) are dissolved in the 97.5g deionized water (that is: in the additive for preparing, the weight percentage of described polyvinyl alcohol is 1%, the weight percentage of described polyoxyethylene glycol be 1.5%);
B), prepare acid Woolen-making liquid: under stirring action, be that 49% hydrofluoric acid, nitric acid and the 5.5L deionized water that 8L concentration is 65-68% mix with 1.5L concentration, then add the above-mentioned additive of 75mL, stir (that is: in the acid Woolen-making liquid for preparing, the weight percentage of described hydrofluoric acid is 5%, the weight percentage of described nitric acid is 40%, and the weight percentage of described additive is 0.4%);
C), making herbs into wool: diamond wire is cut in the above-mentioned acid Woolen-making liquid of polysilicon chip immersion carry out making herbs into wool, the making herbs into wool temperature is 7
oC, the making herbs into wool time is 120s.
Diamond wire cutting polysilicon chip surface albedo after making herbs into wool is 20.5%.Fig. 5 has provided the scanning electron microscope diagram sheet of the surperficial matte of diamond wire cutting polysilicon chip that obtains, and uses as we know from the figure additive of the present invention diamond wire is cut the matte size that obtains after polycrystalline silicon texturing and distributes all better than conventional making herbs into wool.
Embodiment 3
Adopt following steps:
A), additive preparation: under stirring action, 2.0g polyvinyl alcohol (the business trade mark 1799) and 0.5g polyoxyethylene glycol (molecular weight 1000) are dissolved in the 97.5g deionized water (that is: in the additive for preparing, the weight percentage of described polyvinyl alcohol is 2%, the weight percentage of described polyoxyethylene glycol be 0.5%);
B), prepare acid Woolen-making liquid: under stirring action, be that 49% hydrofluoric acid, nitric acid and the 4L deionized water that 8.5L concentration is 65-68% mix with 2.5L concentration, then add the above-mentioned additive of 130mL, stir (that is: in the acid Woolen-making liquid for preparing, the weight percentage of described hydrofluoric acid is 8%, the weight percentage of described nitric acid is 42%, and the weight percentage of described additive is 0.7%);
C), making herbs into wool: diamond wire is cut in the above-mentioned Woolen-making liquid of polysilicon chip immersion carry out making herbs into wool, the making herbs into wool temperature is 10
oC, the making herbs into wool time is 100s.
Diamond wire cutting polysilicon chip surface albedo after making herbs into wool is 21.0%.Matte size and distribution are all better than conventional making herbs into wool.
Embodiment 4
Adopt following steps:
A), additive preparation: under stirring action, 0.5g polyvinyl alcohol (the business trade mark 2088) and 2.0g polyoxyethylene glycol (molecular weight 600) are dissolved in the 97.5g deionized water (that is: in the additive for preparing, the weight percentage of described polyvinyl alcohol is 0.5%, the weight percentage of described polyoxyethylene glycol be 2%);
B), prepare acid Woolen-making liquid: under stirring action, be that 49% hydrofluoric acid, nitric acid and the 4L deionized water that 7L concentration is 65-68% mix with 4L concentration, then add the above-mentioned additive of 180mL, stir (that is: in the acid Woolen-making liquid for preparing, the weight percentage of described hydrofluoric acid is 12%, the weight percentage of described nitric acid is 35%, and the weight percentage of described additive is 1.0%);
C), making herbs into wool: diamond wire is cut in the above-mentioned Woolen-making liquid of polysilicon chip immersion carry out making herbs into wool, the making herbs into wool temperature is 6
oC, the making herbs into wool time is 150s.
Diamond wire cutting polysilicon chip surface albedo after making herbs into wool is 21.0%.Matte size and distribution are all better than conventional making herbs into wool.
Embodiment 5
Adopt following steps:
A), additive preparation: under stirring action, 2.0g polyvinyl alcohol (the business trade mark 1788) and 1.0g polyoxyethylene glycol (molecular weight 2000) are dissolved in the 96.5g deionized water (that is: in the additive for preparing, the weight percentage of described polyvinyl alcohol is 2%, the weight percentage of described polyoxyethylene glycol be 1%);
B), prepare acid Woolen-making liquid: under stirring action, be that 49% hydrofluoric acid, nitric acid and the 1L deionized water that 6L concentration is 65-68% mix with 8L concentration, then add the above-mentioned additive of 150mL, stir (that is: in the acid Woolen-making liquid for preparing, the weight percentage of described hydrofluoric acid is 24%, the weight percentage of described nitric acid is 30%, and the weight percentage of described additive is 0.8%);
C), making herbs into wool: diamond wire is cut in the above-mentioned Woolen-making liquid of polysilicon chip immersion carry out making herbs into wool, the making herbs into wool temperature is 5
oC, the making herbs into wool time is 200s.
Diamond wire cutting polysilicon chip surface albedo after making herbs into wool is 21.5%.Matte size and distribution are all better than conventional making herbs into wool.
Embodiment 6
Adopt following steps:
A), additive preparation: under stirring action, 1.0g polyvinyl alcohol (the business trade mark 0599) and 2.0g polyoxyethylene glycol (molecular weight 4000) are dissolved in the 97g deionized water (that is: in the additive for preparing, the weight percentage of described polyvinyl alcohol is 1%, the weight percentage of described polyoxyethylene glycol be 2%);
B), prepare acid Woolen-making liquid: under stirring action, be that 49% hydrofluoric acid, nitric acid and the 0.5L deionized water that 12.5L concentration is 65-68% mix with 2L concentration, then add the above-mentioned additive of 100mL, stir (that is: in the acid Woolen-making liquid for preparing, the weight percentage of described hydrofluoric acid is 6%, the weight percentage of described nitric acid is 57%, and the weight percentage of described additive is 0.5%);
C), making herbs into wool: diamond wire is cut in the above-mentioned Woolen-making liquid of polysilicon chip immersion carry out making herbs into wool, the making herbs into wool temperature is 25
oC, the making herbs into wool time is 60s.
Diamond wire cutting polysilicon chip surface albedo after making herbs into wool is 22.0%.Matte size and distribution are all better than conventional making herbs into wool.
For reaching illustration purpose; with the preferred embodiments narration as above, so it is not to limit the present invention to this patent, and any affiliated technical field without departing from the spirit and scope of the present invention; when can do a little change and polishing, so protection scope of the present invention is when being limited with claims.
Claims (10)
1. an additive that is used for diamond wire cutting polysilicon chip acid making herbs into wool, is characterized in that described additive comprises following component: polyvinyl alcohol, polyoxyethylene glycol and deionized water.
2. additive as claimed in claim 1, the weight percentage that it is characterized in that described polyvinyl alcohol is 0.5 ~ 2%.
3. additive as claimed in claim 1, the weight percentage that it is characterized in that described polyoxyethylene glycol is 0.5 ~ 2%.
4. additive as claimed in claim 1, the alcoholysis degree that it is characterized in that described polyvinyl alcohol is 88% or 98%, preferred alcoholysis degree is 88%.
5. additive as claimed in claim 1, the molecular weight that it is characterized in that described polyoxyethylene glycol is 200 ~ 5000, preferred molecular weight is 400 ~ 1000.
6. the described additive of claim 1 using method in diamond wire cutting polysilicon chip acid leather producing process, it is characterized in that described sour leather producing process comprises the steps: a) additive preparation: polyvinyl alcohol and polyoxyethylene glycol are dissolved in deionized water, make additive; B) prepare acid Woolen-making liquid: hydrofluoric acid and nitric acid are dissolved in make sour mixing solutions in deionized water, the additive that then step a) is made joins in this acid mixing solutions, obtains acid Woolen-making liquid; C) making herbs into wool: diamond wire is cut polysilicon chip be immersed in the acid Woolen-making liquid that step b) obtains and carry out making herbs into wool.
7. the using method of additive in diamond wire cutting polysilicon chip acid leather producing process as claimed in claim 6, it is characterized in that in described step a), the weight percentage of described polyvinyl alcohol is 0.5 ~ 2%, and the weight percentage of described polyoxyethylene glycol is 0.5 ~ 2%.
8. the using method of additive in diamond wire cutting polysilicon chip acid leather producing process as claimed in claim 6, is characterized in that in described step b), and the weight percentage of hydrofluoric acid is 5 ~ 25%, and the weight percentage of nitric acid is 30 ~ 60%.
9. the using method of additive in diamond wire cutting polysilicon chip acid leather producing process as claimed in claim 6, is characterized in that in described step b), and the weight percentage of additive is 0.4 ~ 1%.
10. the using method of additive in diamond wire cutting polysilicon chip acid leather producing process as claimed in claim 6, is characterized in that in described step c), and the making herbs into wool temperature of making herbs into wool process is 5 ~ 25
oC, the making herbs into wool time is 60 ~ 200s, preferred making herbs into wool temperature is 5 ~ 10
oC, the preferred making herbs into wool time is 100 ~ 150s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310049552.7A CN103132079B (en) | 2013-02-07 | 2013-02-07 | Additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and application method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310049552.7A CN103132079B (en) | 2013-02-07 | 2013-02-07 | Additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and application method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103132079A true CN103132079A (en) | 2013-06-05 |
| CN103132079B CN103132079B (en) | 2015-07-08 |
Family
ID=48492509
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310049552.7A Expired - Fee Related CN103132079B (en) | 2013-02-07 | 2013-02-07 | Additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and application method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103132079B (en) |
Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409808A (en) * | 2013-09-04 | 2013-11-27 | 常州时创能源科技有限公司 | Texturization additive for polycrystalline silicon slices and use method of texturization additive |
| CN103710705A (en) * | 2013-12-23 | 2014-04-09 | 北京合德丰材料科技有限公司 | Additive for acidic texturing liquid of polycrystalline silicon wafers and application thereof |
| CN104342702A (en) * | 2013-08-05 | 2015-02-11 | 南京科乃迪科环保科技有限公司 | Auxiliary chemical composition for monocrystalline silicon or polycrystalline silicon acidic wool making |
| WO2015032153A1 (en) * | 2013-09-04 | 2015-03-12 | 常州时创能源科技有限公司 | Monocrystalline silicon wafer texturizing additive and use thereof |
| CN104651949A (en) * | 2015-02-11 | 2015-05-27 | 常州君合科技股份有限公司 | Multi-crystalline silicon wafer texturization additive |
| CN105040108A (en) * | 2015-08-21 | 2015-11-11 | 浙江启鑫新能源科技股份有限公司 | Texture surface making method for polycrystalline silicon solar battery |
| CN105304734A (en) * | 2015-11-03 | 2016-02-03 | 苏州旭环光伏科技有限公司 | Polycrystalline silicon wafer texturing auxiliary and application method thereof |
| CN106009963A (en) * | 2016-08-01 | 2016-10-12 | 安庆瑞泰化工有限公司 | Water-based paint containing graphite and preparation method thereof |
| CN106119976A (en) * | 2016-08-19 | 2016-11-16 | 常州时创能源科技有限公司 | The additive of polycrystalline black silicon making herbs into wool reaming acid solution and application thereof |
| CN107177890A (en) * | 2017-06-12 | 2017-09-19 | 通威太阳能（合肥）有限公司 | The etching method and cell piece preparation technology of a kind of Buddha's warrior attendant wire cutting polysilicon chip |
| CN107217306A (en) * | 2017-05-19 | 2017-09-29 | 湖州三峰能源科技有限公司 | The Chemical composition that of polysilicon chip acid making herbs into wool optimization agent and its application |
| CN107245761A (en) * | 2017-08-10 | 2017-10-13 | 常州时创能源科技有限公司 | Diamond wire polycrystalline silicon texturing adjuvant and its application |
| CN109267154A (en) * | 2018-09-28 | 2019-01-25 | 横店集团东磁股份有限公司 | Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method |
| CN109355711A (en) * | 2018-12-18 | 2019-02-19 | 张占香 | A kind of flocking additive and its application for Buddha's warrior attendant wire cutting polysilicon chip |
| CN109537058A (en) * | 2018-09-30 | 2019-03-29 | 江苏顺风新能源科技有限公司 | The black silicon preparation process of wet process |
| CN109554762A (en) * | 2018-12-18 | 2019-04-02 | 武汉风帆电化科技股份有限公司 | A kind of polysilicon etch solution additive and its application |
| CN109750353A (en) * | 2019-03-14 | 2019-05-14 | 常州时创能源科技有限公司 | Monocrystalline silicon piece inverted pyramid making herbs into wool adjuvant and its application |
| CN110067028A (en) * | 2019-05-31 | 2019-07-30 | 大连理工大学 | A kind of additive and application for Buddha's warrior attendant wire cutting polysilicon chip acid making herbs into wool |
| WO2019145486A1 (en) | 2018-01-26 | 2019-08-01 | Singulus Technologies Ag | Method and device for cleaning etched surfaces of a semiconductor substrate |
| WO2019145485A1 (en) | 2018-01-26 | 2019-08-01 | Singulus Technologies Ag | Method and device for treating etched surfaces of a semiconductor substrate using a ozone-containing medium |
| 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 |
| CN110846721A (en) * | 2019-10-12 | 2020-02-28 | 湖南理工学院 | Monocrystalline silicon texturing additive formula containing polyalcohol and PEG |
| CN110872729A (en) * | 2018-08-30 | 2020-03-10 | 比亚迪股份有限公司 | Texturing and hole digging additive, texturing and silver sinking hole digging liquid, silicon wafer and solar cell of diamond wire cutting polycrystalline silicon wafer |
| CN111843836A (en) * | 2019-04-29 | 2020-10-30 | 苏州澳京光伏科技有限公司 | Surface treatment method for diamond wire cutting polycrystalline silicon wafer |
| 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 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019013706A1 (en) * | 2017-07-11 | 2019-01-17 | National University Of Singapore | A method of texturing photovoltaic silicon wafers |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009007136A1 (en) * | 2009-02-02 | 2010-08-12 | Sovello Ag | Etching mixture for producing a structured surface on silicon substrates |
| CN102134077A (en) * | 2011-01-25 | 2011-07-27 | 云南乾元光能产业有限公司 | Method for purifying polycrystalline silicon by wet method |
-
2013
- 2013-02-07 CN CN201310049552.7A patent/CN103132079B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009007136A1 (en) * | 2009-02-02 | 2010-08-12 | Sovello Ag | Etching mixture for producing a structured surface on silicon substrates |
| CN102134077A (en) * | 2011-01-25 | 2011-07-27 | 云南乾元光能产业有限公司 | Method for purifying polycrystalline silicon by wet method |
Non-Patent Citations (2)
| Title |
|---|
| 张存彪等: "《光伏电池制备工艺》", 29 February 2012, 化学工业出版社 * |
| 肖文明等: ""多晶Si太阳电池表面酸腐蚀制绒的研究"", 《微纳电子技术》 * |
Cited By (37)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104342702A (en) * | 2013-08-05 | 2015-02-11 | 南京科乃迪科环保科技有限公司 | Auxiliary chemical composition for monocrystalline silicon or polycrystalline silicon acidic wool making |
| KR101687767B1 (en) | 2013-09-04 | 2016-12-19 | 창쩌우 스추앙 에너지 테크놀로지 리미티드 코포레이션 | Additive for preparing suede on polycrystalline silicon chip and use method thereof |
| WO2015032154A1 (en) * | 2013-09-04 | 2015-03-12 | 常州时创能源科技有限公司 | Polycrystalline silicon wafer texturizing additive and use thereof |
| WO2015032153A1 (en) * | 2013-09-04 | 2015-03-12 | 常州时创能源科技有限公司 | Monocrystalline silicon wafer texturizing additive and use thereof |
| KR20150039128A (en) * | 2013-09-04 | 2015-04-09 | 창쩌우 스추앙 에너지 테크놀로지 리미티드 코포레이션 | Additive for preparing suede on polycrystalline silicon chip and use method thereof |
| CN103409808B (en) * | 2013-09-04 | 2015-10-21 | 常州时创能源科技有限公司 | Polycrystalline silicon texturing additive and using method thereof |
| CN103409808A (en) * | 2013-09-04 | 2013-11-27 | 常州时创能源科技有限公司 | Texturization additive for polycrystalline silicon slices and use method of texturization additive |
| CN103710705A (en) * | 2013-12-23 | 2014-04-09 | 北京合德丰材料科技有限公司 | Additive for acidic texturing liquid of polycrystalline silicon wafers and application thereof |
| CN103710705B (en) * | 2013-12-23 | 2016-01-20 | 北京合德丰材料科技有限公司 | A kind of additive of polycrystalline silicon wafer acidity texture preparation liquid and application thereof |
| CN104651949A (en) * | 2015-02-11 | 2015-05-27 | 常州君合科技股份有限公司 | Multi-crystalline silicon wafer texturization additive |
| CN105040108A (en) * | 2015-08-21 | 2015-11-11 | 浙江启鑫新能源科技股份有限公司 | Texture surface making method for polycrystalline silicon solar battery |
| CN105040108B (en) * | 2015-08-21 | 2017-11-17 | 浙江启鑫新能源科技股份有限公司 | The etching method of polysilicon solar cell |
| CN105304734A (en) * | 2015-11-03 | 2016-02-03 | 苏州旭环光伏科技有限公司 | Polycrystalline silicon wafer texturing auxiliary and application method thereof |
| CN106009963A (en) * | 2016-08-01 | 2016-10-12 | 安庆瑞泰化工有限公司 | Water-based paint containing graphite and preparation method thereof |
| CN106119976A (en) * | 2016-08-19 | 2016-11-16 | 常州时创能源科技有限公司 | The additive of polycrystalline black silicon making herbs into wool reaming acid solution and application thereof |
| CN107217306A (en) * | 2017-05-19 | 2017-09-29 | 湖州三峰能源科技有限公司 | The Chemical composition that of polysilicon chip acid making herbs into wool optimization agent and its application |
| CN107177890A (en) * | 2017-06-12 | 2017-09-19 | 通威太阳能（合肥）有限公司 | The etching method and cell piece preparation technology of a kind of Buddha's warrior attendant wire cutting polysilicon chip |
| CN107245761A (en) * | 2017-08-10 | 2017-10-13 | 常州时创能源科技有限公司 | Diamond wire polycrystalline silicon texturing adjuvant and its application |
| DE102018206980A1 (en) | 2018-01-26 | 2019-08-01 | Singulus Technologies Ag | Method and apparatus for cleaning etched surfaces of a semiconductor substrate |
| WO2019145486A1 (en) | 2018-01-26 | 2019-08-01 | Singulus Technologies Ag | Method and device for cleaning etched surfaces of a semiconductor substrate |
| WO2019145485A1 (en) | 2018-01-26 | 2019-08-01 | Singulus Technologies Ag | Method and device for treating etched surfaces of a semiconductor substrate using a ozone-containing medium |
| DE102018206978A1 (en) | 2018-01-26 | 2019-08-01 | Singulus Technologies Ag | Method and apparatus for treating etched surfaces of a semiconductor substrate using ozone-containing medium |
| CN110872729B (en) * | 2018-08-30 | 2021-07-20 | 比亚迪股份有限公司 | Texturing and hole digging additive, texturing and silver sinking hole digging liquid, silicon wafer and solar cell of diamond wire cutting polycrystalline silicon wafer |
| CN110872729A (en) * | 2018-08-30 | 2020-03-10 | 比亚迪股份有限公司 | Texturing and hole digging additive, texturing and silver sinking hole digging liquid, silicon wafer and solar cell of diamond wire cutting polycrystalline silicon wafer |
| CN109267154A (en) * | 2018-09-28 | 2019-01-25 | 横店集团东磁股份有限公司 | Buddha's warrior attendant wire cutting monocrystalline silicon surface etching method |
| CN109537058A (en) * | 2018-09-30 | 2019-03-29 | 江苏顺风新能源科技有限公司 | The black silicon preparation process of wet process |
| CN109537058B (en) * | 2018-09-30 | 2021-01-05 | 江苏顺风新能源科技有限公司 | Wet black silicon preparation process |
| CN109355711A (en) * | 2018-12-18 | 2019-02-19 | 张占香 | A kind of flocking additive and its application for Buddha's warrior attendant wire cutting polysilicon chip |
| CN109554762A (en) * | 2018-12-18 | 2019-04-02 | 武汉风帆电化科技股份有限公司 | A kind of polysilicon etch solution additive and its application |
| CN109750353A (en) * | 2019-03-14 | 2019-05-14 | 常州时创能源科技有限公司 | Monocrystalline silicon piece inverted pyramid making herbs into wool adjuvant and its application |
| 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 |
| CN111843836A (en) * | 2019-04-29 | 2020-10-30 | 苏州澳京光伏科技有限公司 | Surface treatment method for diamond wire cutting polycrystalline silicon wafer |
| CN110067028A (en) * | 2019-05-31 | 2019-07-30 | 大连理工大学 | A kind of additive and application for Buddha's warrior attendant wire cutting polysilicon chip acid making herbs into wool |
| CN110846721A (en) * | 2019-10-12 | 2020-02-28 | 湖南理工学院 | Monocrystalline silicon texturing additive formula containing polyalcohol and PEG |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103132079B (en) | 2015-07-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103132079B (en) | Additive for acid texturing of diamond-wire-cutting polycrystalline silicon slices and application method thereof | |
| CN103710705B (en) | A kind of additive of polycrystalline silicon wafer acidity texture preparation liquid and application thereof | |
| US8461057B2 (en) | Process for the rough-etching of silicon solar cells | |
| CN102220645B (en) | Method for texturing silicon wafer cut by diamond wire | |
| CN103614778A (en) | Alcohol-free alkaline texturing solution for mono-crystalline silicon wafer, texturing method for mono-crystalline silicon wafer, solar cell and manufacturing method for solar cell | |
| CN107268087A (en) | A kind of metal catalytic etching method for the polysilicon chip reflectivity for reducing Buddha's warrior attendant wire cutting | |
| CN104900509A (en) | Surface treatment method and texturing method for diamond wire cutting silicon wafers | |
| CN102965614B (en) | Preparation method of laser film | |
| CN106935669A (en) | A kind of etching method of the diamond wire section black silicon of polycrystalline | |
| CN105951184A (en) | Texturing method of diamond wire-cut polycrystalline silicon wafer | |
| CN106340446B (en) | A kind of method of wet process removal diamond wire saw polysilicon chip surface line marker | |
| CN103339738A (en) | Method for fabricating substrate for solar cell and solar cell | |
| CN104505437A (en) | Texturing preprocessing solution and method of diamond wire cutting polycrystalline silicon wafer, texturing preprocessing silicon wafer and application of texturing preprocessing silicon wafer | |
| CN107287597A (en) | Wool-making agent of monocrystalline silicon surface processing and preparation method thereof and application method | |
| CN102779902A (en) | Preparation method of Ge/Si substrate slice for GaAs solar cell | |
| CN101901832B (en) | Controlled silicon punchthrough structure formed by gallium diffusion and production method thereof | |
| CN111105995A (en) | Cleaning and texturing method of monocrystalline silicon wafer | |
| CN102867880A (en) | Method for preparing double acid etching textures on polycrystalline silicon surface | |
| CN101976705B (en) | Single-side acid-etching technology of crystalline silicon solar batteries | |
| CN105826410A (en) | Diamond wire cutting trace eliminated polysilicon texturizing method | |
| CN112251817B (en) | Inverted pyramid auxiliary texturing additive and application thereof | |
| CN102732969B (en) | Crystal bar surface nanocystalized process and wafer manufacture method | |
| CN103160930A (en) | Crystal bar surface nanocrystallization process, wafer manufacturing method and wafer | |
| CN107858757A (en) | Buddha's warrior attendant wire cutting polysilicon chip special acid flocking additive and its application method | |
| Li et al. | Effect of the anisotropy of etching surface morphology on light-trapping and photovoltaic conversion efficiencies of silicon solar cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210525 Address after: 322009 no.655, Haopai Road, Suxi Town, Yiwu City, Jinhua City, Zhejiang Province Patentee after: Ruina solar technology (Yiwu) Co.,Ltd. Address before: Room 1802-1803, Pudong Jiali City, 1155 Fangdian Road, Pudong New Area, Shanghai 201204 Patentee before: RENA (SHANGHAI) Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150708 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |