CN103789839A - Flocking method of weak oxidation monocrystalline silicon piece - Google Patents
Flocking method of weak oxidation monocrystalline silicon piece Download PDFInfo
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- CN103789839A CN103789839A CN201410058182.8A CN201410058182A CN103789839A CN 103789839 A CN103789839 A CN 103789839A CN 201410058182 A CN201410058182 A CN 201410058182A CN 103789839 A CN103789839 A CN 103789839A
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- monocrystalline silicon
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Abstract
The invention discloses a flocking method of a weak oxidation monocrystalline silicon piece. The flocking method comprises the steps: placing a cleaned monocrystalline silicon piece in an HF (Hydrogen Fluoride) water solution to remove a thicker oxidation layer on the surface of a silicon piece, then oxidizing the silicon piece in an H2O2 water solution, forming a thinner oxidizing layer on the surface of the silicon piece, and finally, placing the silicon piece in a flocking solution to obtain a high-quality pyramid fabric surface. By adopting the method disclosed by the invention, a high-quality fabric surface which is of a complete and independent pyramid structure with uniform size and is dense in pyramids can be prepared, so that the reflectivity of the surface of the monocrystalline silicon piece is remarkably reduced.
Description
Technical field
The invention belongs to crystal silicon solar batteries production making herbs into wool technical field, be specifically related to a kind of etching method of weak oxide monocrystalline silicon piece.
Background technology
In photovoltaic industry, how to realize the raising of conversion efficiency of solar cell and the reduction of cost is the Important Problems of research always.For monocrystalline silicon battery, an important means that improves conversion efficiency of solar cell is to reduce the reflection of sunlight at silicon chip surface.In order to reduce reflection loss, conventionally silicon chip surface is carried out to making herbs into wool or at battery surface depositing antireflection film.Wherein simply, chemical corrosion method enjoys favor in silicon chip surface making herbs into wool cheaply.
Monocrystalline silicon chip of solar cell making herbs into wool is at present the technique of comparative maturity, tradition leather producing process is to make matte take sodium hydroxide, Virahol and making herbs into wool additive as Woolen-making liquid, its principle is mainly to utilize the anisotropic etch of basic solution to monocrystalline silicon piece, can form the suede structure of pyramid shape at monocrystalline silicon sheet surface, make sunlight carry out multiple reflections and improve the absorption of solar cell to light at silicon chip surface, thereby improve battery efficiency.But the pyramid size obtaining by this technique is not too even, reduce the anti-reflection effect of matte.In view of this,, in order further to improve the absorption of single crystal silicon solar cell to light, be necessary to explore a kind of method of the high quality suede structure that can form pyramid size uniform.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of etching method of weak oxide monocrystalline silicon piece, adopts this method to prepare to have complete, independence, the uniform pyramid structure of size and the intensive high-quality matte of pyramid.
Solving the problems of the technologies described above adopted technical scheme is: it is 10% the HF aqueous solution that cleaned monocrystalline silicon piece is placed in to massfraction, soak at room temperature 0.5～2 minute, remove silicon chip surface thicker zone of oxidation, then monocrystalline silicon piece is put into massfraction and be 2%～20% H
2o
2in the aqueous solution, 50～70 ℃ are oxidized 2～12 minutes, form the very thin zone of oxidation of one deck at silicon chip surface, then the silicon chip after oxidation is placed in to Woolen-making liquid, obtain the monocrystalline silicon piece of pyramid matte, and wherein corresponding reaction equation is as follows:
SiO
2+6HF→H
2SiF
6+2H
2O (1)
Si+2H
2O
2→SiO
2+2H
2O (2)
Si+2NaOH+H
2O→Na
2SiO
3+2H
2↑ (3)
SiO
2+2NaOH→Na
2SiO
3+H
2O (4)
Top condition of the present invention is: it is the 10%HF aqueous solution that cleaned monocrystalline silicon piece is placed in to massfraction, and then soak at room temperature 1 minute puts into monocrystalline silicon piece massfraction and be 5% H
2o
2in the aqueous solution, 65 ℃ are oxidized 8 minutes, then the silicon chip after oxidation is placed in to Woolen-making liquid, obtain the monocrystalline silicon piece of pyramid matte.
Above-mentioned Woolen-making liquid can be selected any one Woolen-making liquid using in the disclosed fine-hair maring using monocrystalline silicon slice technique of prior art, the Woolen-making liquid that the NaOH aqueous solution that preferred mass mark of the present invention is 2%～3% and Virahol, making herbs into wool additive form for 730:20:1 by volume, described making herbs into wool additive is provided by Kunshan great Yuan Chemical Industry Science Co., Ltd, model is DY-810, monocrystalline silicon piece after weak oxide is placed in to this Woolen-making liquid, 80 ℃ are reacted 20～30 minutes, obtain the monocrystalline silicon piece of pyramid matte.
The present invention passes through H
2o
2monocrystalline silicon sheet surface is carried out to weak oxide, make silicon chip surface form the very thin zone of oxidation of one deck, to reduce the speed of reaction of silicon chip and Woolen-making liquid, thereby form complete, independence, the uniform pyramid structure of size and the intensive high-quality matte of pyramid at silicon chip surface, the reflectivity of monocrystalline silicon sheet surface is significantly reduced.
Accompanying drawing explanation
Fig. 1 is the pyramidal SEM figure of the prepared monocrystalline silicon sheet surface of embodiment 1.
Fig. 2 is the pyramidal SEM figure of the prepared monocrystalline silicon sheet surface of embodiment 2.
Fig. 3 is the pyramidal SEM figure of the prepared monocrystalline silicon sheet surface of embodiment 3.
Fig. 4 is the pyramidal SEM figure of the prepared monocrystalline silicon sheet surface of comparative example 1.
Fig. 5 is the reflected light spectrogram of the prepared monocrystalline silicon piece of embodiment 1～3 and comparative example's 1 prepared monocrystalline silicon piece, and wherein a, b, c, d are the reflection spectrum curve of embodiment 1,2,3 and comparative example's 1 prepared monocrystalline silicon piece successively.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the present invention is not limited only to following embodiment.
Embodiment 1
N-shaped monocrystalline silicon piece (100) is placed in to NH
4oH and H
2o
2, H
2the volume ratio of O is in the scavenging solution of 1:1:5, and 70～80 ℃ of heating in water bath 30 minutes are removed the organic pollutant of silicon chip surface, then put into HCl and H
2o
2, H
2the volume ratio of O is in the scavenging solution of 1:1:5, and 70～80 ℃ of heating in water bath 30 minutes are removed the metallic impurity of silicon chip surface.It is in 10% the HF aqueous solution that cleaned monocrystalline silicon piece is positioned over to massfraction, and soak at room temperature 1 minute, removes the thicker zone of oxidation of silicon chip surface, puts into massfraction and be 5% H after then silicon chip extracting being dried up by washed with de-ionized water and with nitrogen
2o
2in the aqueous solution, 65 ℃ are oxidized 8 minutes, make silicon chip surface form the very thin zone of oxidation of one deck, then the silicon chip extracting after oxidation is dried up by washed with de-ionized water and with nitrogen, to in the Woolen-making liquid of 80 ℃ of the silicon chip immersions after oxidation, react 25 minutes again, wherein Woolen-making liquid is that massfraction is 3% the NaOH aqueous solution and Virahol, the mixed solution that the volume ratio of making herbs into wool additive DY-810 is 730:20:1, wherein making herbs into wool additive DY-810 is provided by Kunshan great Yuan Chemical Industry Science Co., Ltd, finally dry up by washed with de-ionized water and with nitrogen, obtain the monocrystalline silicon piece (see figure 1) of pyramid matte.
H used in the present embodiment
2o
2the massfraction of the aqueous solution is 10%, 65 ℃ of oxidation 5 minutes, and other steps are identical with embodiment 1, obtain the monocrystalline silicon piece (see figure 2) of pyramid matte.
Embodiment 3
H used in the present embodiment
2o
2the massfraction of the aqueous solution is 20%, 65 ℃ of oxidation 3 minutes, and other steps are identical with embodiment 1, obtain the monocrystalline silicon piece (see figure 3) of pyramid matte.
Comparative example 1
According to the method for embodiment 1, N-shaped monocrystalline silicon piece (100) is cleaned, then cleaned monocrystalline silicon piece is positioned over to massfraction and is in 10% the HF aqueous solution, soak at room temperature 1 minute, remove the thicker zone of oxidation of silicon chip surface, then will in the Woolen-making liquid of 80 ℃ of monocrystalline silicon piece immersions, react 25 minutes, wherein Woolen-making liquid is that massfraction is 3% the NaOH aqueous solution and Virahol, the mixed solution that the volume ratio of making herbs into wool additive DY-810 is 730:20:1, wherein making herbs into wool additive DY-810 is provided by Kunshan great Yuan Chemical Industry Science Co., Ltd, dry up by washed with de-ionized water and with nitrogen again, obtain the monocrystalline silicon piece (see figure 4) of pyramid matte.
As seen from the figure, pyramid that monocrystalline silicon sheet surface that embodiment 1～3 obtains forms is complete, independence, size are even and intensive, the pyramid size that monocrystalline silicon sheet surface that comparative example 1 obtains forms is inhomogeneous, and part pyramid is stacked, illustrates that the inventive method passes through H
2o
2monocrystalline silicon sheet surface is carried out to weak oxide, can reduce the speed of reaction of silicon chip and Woolen-making liquid, thereby obtain high-quality matte.Adopt that the outer of the Japanese Shimadzu UV-3600 of company type purple can be shown in that near infrared spectrometer obtains embodiment 1～3 and comparative example 1 monocrystalline silicon piece carry out the test of reflection spectrum, the results are shown in Figure 5, as seen from the figure, the average reflectance of the monocrystalline silicon piece that comparative example 1 obtains is 12.47%, the average reflectance of the monocrystalline silicon piece that embodiment 1～3 obtains is followed successively by 11.23%, 10.38%, 9.89%, significantly reduces compared with comparative example 1.
Embodiment 4
H used in the present embodiment
2o
2the massfraction of the aqueous solution is 2%, 70 ℃ of oxidation 12 minutes, and other steps are identical with embodiment 1, obtain the monocrystalline silicon piece of pyramid matte.
Embodiment 5
H used in the present embodiment
2o
2the massfraction of the aqueous solution is 15%, 50 ℃ of oxidation 10 minutes, and other steps are identical with embodiment 1, obtain the monocrystalline silicon piece of pyramid matte.
Purging method and the Woolen-making liquid of monocrystalline silicon piece of the present invention are not limited only to above-described embodiment, and the above specific embodiment is only not used in and limits the scope of the invention for the present invention is described.It should be pointed out that all distortion that those of ordinary skill in the art directly derives or associate according to content disclosed by the invention are all in protection scope of the present invention.
Claims (4)
1. an etching method for weak oxide monocrystalline silicon piece, is characterized in that: it is the 10%HF aqueous solution that cleaned monocrystalline silicon piece is placed in to massfraction, and then soak at room temperature 0.5～2 minute puts into monocrystalline silicon piece massfraction and be 2%～20% H
2o
2in the aqueous solution, 50～70 ℃ are oxidized 3～12 minutes, then the silicon chip after oxidation is placed in to Woolen-making liquid, obtain the monocrystalline silicon piece of pyramid matte.
2. the etching method of weak oxide monocrystalline silicon piece according to claim 1, is characterized in that: it is the 10%HF aqueous solution that cleaned monocrystalline silicon piece is placed in to massfraction, and then soak at room temperature 1 minute puts into monocrystalline silicon piece massfraction and be 5% H
2o
2in the aqueous solution, 65 ℃ are oxidized 8 minutes, then the silicon chip after oxidation is placed in to Woolen-making liquid, obtain the monocrystalline silicon piece of pyramid matte.
3. the etching method of weak oxide monocrystalline silicon piece according to claim 1 and 2, is characterized in that: described Woolen-making liquid is that massfraction is the mixed solution that the volume ratio of 2%～3% the NaOH aqueous solution and Virahol, making herbs into wool additive is 730:20:1.
4. the etching method of weak oxide monocrystalline silicon piece according to claim 3, is characterized in that: the silicon chip after oxidation is placed in to Woolen-making liquid, and 80 ℃ are reacted 20～30 minutes, obtain the monocrystalline silicon piece of pyramid matte.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104409529A (en) * | 2014-11-27 | 2015-03-11 | 浙江昱辉阳光能源江苏有限公司 | Manufacturing process for microstructural textured polycrystalline silicon solar cell |
| CN104465863A (en) * | 2014-07-30 | 2015-03-25 | 上饶光电高科技有限公司 | Polycrystalline silicon chip preprocessing method capable of improving photoelectric conversion efficiency |
| CN104562211A (en) * | 2014-12-26 | 2015-04-29 | 横店集团东磁股份有限公司 | Texture surface making method capable of improving conversion efficiency of monocrystal cell |
| CN108221050A (en) * | 2018-01-19 | 2018-06-29 | 温岭汉德高分子科技有限公司 | A kind of monocrystalline silicon piece with bimodal pyramid suede structure |
| CN108251894A (en) * | 2018-01-19 | 2018-07-06 | 温岭汉德高分子科技有限公司 | A kind of etching method of monocrystalline silicon piece |
| CN112899789A (en) * | 2021-01-19 | 2021-06-04 | 西安交通大学 | Texturing method for pretreating surface of monocrystalline silicon wafer by electrochemical method |
Citations (5)
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|---|---|---|---|---|
| JPS58217500A (en) * | 1982-06-11 | 1983-12-17 | Nippon Telegr & Teleph Corp <Ntt> | Production of pyramid-shaped micro presser |
| US20110070744A1 (en) * | 2009-09-18 | 2011-03-24 | Zhi-Wen Sun | Silicon Texturing Formulations for Solar Applications |
| CN102231404A (en) * | 2011-05-20 | 2011-11-02 | 浙江星宇能源科技有限公司 | Technology for cleaning solar monocrystalline wafer |
| CN102586887A (en) * | 2012-03-15 | 2012-07-18 | 苏州先拓光伏科技有限公司 | Suede-making additive for low-reflectivity monocrystalline silicon |
| CN102810596A (en) * | 2012-04-24 | 2012-12-05 | 上澎太阳能科技(嘉兴)有限公司 | Suede preparation method of metallurgical-grade single crystal and mono-like silicon |
-
2014
- 2014-02-20 CN CN201410058182.8A patent/CN103789839B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58217500A (en) * | 1982-06-11 | 1983-12-17 | Nippon Telegr & Teleph Corp <Ntt> | Production of pyramid-shaped micro presser |
| US20110070744A1 (en) * | 2009-09-18 | 2011-03-24 | Zhi-Wen Sun | Silicon Texturing Formulations for Solar Applications |
| CN102231404A (en) * | 2011-05-20 | 2011-11-02 | 浙江星宇能源科技有限公司 | Technology for cleaning solar monocrystalline wafer |
| CN102586887A (en) * | 2012-03-15 | 2012-07-18 | 苏州先拓光伏科技有限公司 | Suede-making additive for low-reflectivity monocrystalline silicon |
| CN102810596A (en) * | 2012-04-24 | 2012-12-05 | 上澎太阳能科技(嘉兴)有限公司 | Suede preparation method of metallurgical-grade single crystal and mono-like silicon |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104465863A (en) * | 2014-07-30 | 2015-03-25 | 上饶光电高科技有限公司 | Polycrystalline silicon chip preprocessing method capable of improving photoelectric conversion efficiency |
| CN104409529A (en) * | 2014-11-27 | 2015-03-11 | 浙江昱辉阳光能源江苏有限公司 | Manufacturing process for microstructural textured polycrystalline silicon solar cell |
| CN104562211A (en) * | 2014-12-26 | 2015-04-29 | 横店集团东磁股份有限公司 | Texture surface making method capable of improving conversion efficiency of monocrystal cell |
| CN108221050A (en) * | 2018-01-19 | 2018-06-29 | 温岭汉德高分子科技有限公司 | A kind of monocrystalline silicon piece with bimodal pyramid suede structure |
| CN108251894A (en) * | 2018-01-19 | 2018-07-06 | 温岭汉德高分子科技有限公司 | A kind of etching method of monocrystalline silicon piece |
| CN112899789A (en) * | 2021-01-19 | 2021-06-04 | 西安交通大学 | Texturing method for pretreating surface of monocrystalline silicon wafer by electrochemical method |
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| CN103789839B (en) | 2016-11-09 |
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