CN102134754A - Manufacturing method of submicron suede of monocrystalline silicon slice with crystal orientation being [100] - Google Patents
Manufacturing method of submicron suede of monocrystalline silicon slice with crystal orientation being [100] Download PDFInfo
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- CN102134754A CN102134754A CN 201110060146 CN201110060146A CN102134754A CN 102134754 A CN102134754 A CN 102134754A CN 201110060146 CN201110060146 CN 201110060146 CN 201110060146 A CN201110060146 A CN 201110060146A CN 102134754 A CN102134754 A CN 102134754A
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Abstract
The invention discloses a manufacturing method of submicron suede of a monocrystalline silicon slice with crystal orientation being [100], which comprises the following steps of: (1) selecting the monocrystalline silicon slice with specific resistance of 0.5-20 omega cm, the crystal orientation of (100) and thickness of 180 plus or minus 40 [mu]m; (2) pre-cleaning the silicon slice, cleaning the silicon slice in an aqueous solution containing 3%-7% of drine and 1%-2% of NaOH in weight ratio for 4-6 minutes, and controlling the temperature of the solution at 50-60 DEG C; (3) removing a damaged layer, placing the monocrystalline silicon slice in an aqueous solution with concentration of 10%-15% NaOH in weight ratio for 2-6 minutes, and controlling the temperature at 60-80 DEG C; and (4) sueding, placing the monocrystalline silicon slice in an aqueous solution containing 1%-1.5% NaOH, 0.05%-1% Na3PO4*12H2O, 1%-1.5% sodium benzoate and 0.1%-0.5% sodium molybdate in weight ratio for 5-25 minutes, and controlling the temperature at 70-83 DEG C. By using the method, the thickness reduction of the monocrystalline silicon slice is 1/5-1/6 of the thickness reduction of a conventional sueding method under the condition that the average reflectance of a battery is not changed in a visible light range, the degree of curvature and the fragmentation ratio of the battery are reduced obviously, the cost is decreased, and the efficiency is improved.
Description
Technical field
The present invention relates to a kind of manufacture method of crystal silicon chip matte.
Background technology
At present, the photovoltaic generation cost is 2～3 times of thermoelectricity cost, and cost is too high to be the major obstacle of restriction photovoltaic generation large-scale application.Improve the production efficiency of crystal silicon battery, reduce cost, make its cost of electricity-generating near or equal the thermoelectricity cost, for solving present energy shortage and environmental pollution problems, realize national economy and social sustainable development, have great reality and far-reaching significance.
The cost of monocrystalline silicon piece accounts for 60% of assembly cost, this shows that reducing the monocrystalline silicon piece cost is one of the most effective direction that reduces the crystal silicon battery cost of electricity-generating.The thickness of past monocrystalline silicon piece is at 400um, and along with the development of state of the art, the thickness of monocrystalline silicon piece is reduced to 180um now, also will continue from now on to reduce, and this is the main flow of development.The reduction of monocrystalline silicon piece thickness, thereupon to device fabrication, the requirement of workman's operant level and technology is also more and more higher, in the making herbs into wool process of monocrystalline silicon piece, adopt common process, the attenuate amount of monocrystalline silicon piece is excessive, and the thickness of monocrystalline silicon piece is thinner, cause the sinuousness and the fragmentation rate of battery obviously to improve, strengthened the production cost of monocrystalline silicon piece.Urgent need is wanted a kind of etching method now, reduces the attenuate amount of monocrystalline silicon piece in the reflectivity of assurance or reduction monocrystalline silicon piece, its yield rate is uprised, old of the production of reduction monocrystalline silicon piece.
The monocrystalline polished silicon slice, in visible-range, the average reflectance of silicon chip is 33%, and silicon chip is after process making herbs into wool, if the continuous even compact of silicon chip, then reflectivity is 11%, because crystalline structure, under normal making herbs into wool condition, the shape of matte is identical, have only size discrimination, reflectivity is not change with the size of matte.
Summary of the invention
Goal of the invention: the objective of the invention is at the deficiencies in the prior art, a kind of manufacture method of monocrystalline silicon piece submicron matte is provided, this method can guarantee under the battery average reflectance is constant in visible-range the situation, the attenuate amount that makes monocrystalline silicon piece is 1/5～1/6 of a conventional etching method attenuate amount, the sinuousness and the fragmentation rate of its battery are obviously reduced, reduce cost, improved efficient.
Technical scheme: in order to realize the foregoing invention purpose, the technical solution adopted in the present invention is:
A kind of crystal orientation is the manufacture method of [100] monocrystalline silicon piece submicron matte, comprises the following steps:
(1) selecting resistivity is 0.5～20 Ω .cm, and the crystal orientation is [100], and silicon wafer thickness is the monocrystalline silicon piece of 180 ± 40um;
(2) silicon chip pre-washing is cleaned in the aqueous solution of the NaOH weight ratio that comprises 3%～7% monarch and 150 and 1%～2%, and solution temperature is controlled at 50～60 ℃, and the time is 4～6 minutes;
(3) remove affected layer, monocrystalline silicon piece is put into the aqueous solution that concentration is 10%～15%NaOH weight ratio, temperature is controlled at 60～80 ℃, and the time is 2～6 minutes;
(4) making herbs into wool is put into 1%～1.5% NaOH with monocrystalline silicon piece, 0.05%～1% Na
3PO
4.12H2O, 1%～1.5% Sodium Benzoate, in the aqueous solution of 0.1%～0.5% Sodium orthomolybdate weight, temperature is controlled at 70～83 ℃, and the time is 5～25 minutes.
Beneficial effect: the present invention compared with prior art, its beneficial effect is:
1, adopt the attenuate amount of this method making herbs into wool monocrystalline silicon piece be conventional etching method battery attenuate amount 1/5～1/6, the corresponding thickness that increases battery, and in visible-range, under the condition that monocrystalline ghost sheet average reflectance remains unchanged, the sinuousness and the fragmentation rate of its battery are obviously reduced, reduce cost, improved production efficiency:
2, step (2) is wanted thoroughly monocrystalline silicon sheet surface pre-washing, otherwise can influence the continuity and the homogeneity of matte;
3, step (3) is removed affected layer, and after the assurance making herbs into wool, the matte size is even, and height evenly;
4; Sodium Benzoate in the step (4) is in the silicon chip surface feature absorption of monocrystalline; blocked the silicon ion process; perhaps in the silicon chip surface oxidation; generate extremely fine and close protective oxide film; it stops matte oversize; Sodium orthomolybdate is a kind of low contaminative metal-salt; be effective corrosion inhibitors in the safe alkaline medium; the aqueous solution of Sodium orthomolybdate and sodium phosphate has the effect of synergistic slow corrosion to erosion rate, and the threshold concentration of its inhibiter reduces, when both total concns are 0.0015mg/L; and ratio is in 40: 60～10: 80; average corrosion inhibition rate reaches 91.5%, the aqueous solution of sodium phosphate, PO
4 3-Hydrolysis produces a large amount of OH
-With corrosion monocrystalline silicon piece, PO simultaneously
4 3-Or HPO
4 2-Play a part Virahol too, eliminate the gas big gun and slow down the corrosive effect.
Description of drawings
Accompanying drawing is a matte pyramid structure synoptic diagram.
Embodiment
Below in conjunction with accompanying drawing, by a most preferred embodiment, technical solution of the present invention is elaborated, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1
(1) selecting resistivity is 0.5 Ω .cm, and the crystal orientation is [100], and silicon wafer thickness is the monocrystalline silicon piece of 140um;
(2) silicon chip pre-washing is cleaned in the aqueous solution of the NaOH weight that comprises 3% monarch and 150 and 1%, and solution temperature is controlled at 50～60 ℃, and the time is 4～6 minutes;
(3) remove affected layer, it is the 10%NaOH aqueous solution that monocrystalline silicon piece is put into concentration, and temperature is controlled at 60～80 ℃, and the time is 2～6 minutes;
(4) making herbs into wool is put into 1% NaOH with monocrystalline silicon piece, 0.05% Na
3PO
4.12H2O, 1% Sodium Benzoate, in the aqueous solution of 0.1% Sodium orthomolybdate weight, temperature is controlled at 70～83 ℃, and the time is 5～25 minutes.
Produce the monocrystalline silicon piece of submicron matte after testing.
Embodiment 2
(1) selecting resistivity is 20 Ω .cm, and the crystal orientation is [100], and silicon wafer thickness is the monocrystalline silicon piece of 220um;
(2) silicon chip pre-washing is cleaned in the aqueous solution of the NaOH weight that comprises 7% monarch and 150 and 2%, and solution temperature is controlled at 50～60 ℃, and the time is 4～6 minutes;
(3) remove affected layer, it is the 15%NaOH aqueous solution that monocrystalline silicon piece is put into concentration, and temperature is controlled at 60～80 ℃, and the time is 2～6 minutes;
(4) making herbs into wool is put into 1.5% NaOH with monocrystalline silicon piece, 1% Na
3PO
4.12H2O, 1.5% Sodium Benzoate, in the aqueous solution of 0.5% Sodium orthomolybdate weight, temperature is controlled at 70～83 ℃, and the time is 5～25 minutes.
Produce the monocrystalline silicon piece of submicron matte after testing.
Embodiment 3
(1) selecting resistivity is 10 Ω .cm, and the crystal orientation is [100], and silicon wafer thickness is the monocrystalline silicon piece of 180um;
(2) silicon chip pre-washing is cleaned in the aqueous solution of the NaOH weight that comprises 5% monarch and 150 and 2%, and solution temperature is controlled at 50～60 ℃, and the time is 4～6 minutes;
(3) remove affected layer, it is the 13%NaOH aqueous solution that monocrystalline silicon piece is put into concentration, and temperature is controlled at 60～80 ℃, and the time is 2～6 minutes;
(4) making herbs into wool is put into 1.5% NaOH with monocrystalline silicon piece, 0.5% Na
3PO
4.12H2O, 1.2% Sodium Benzoate, in the aqueous solution of 0.3% Sodium orthomolybdate weight, temperature is controlled at 70～83 ℃, and the time is 5～25 minutes.
Produce the monocrystalline silicon piece of submicron matte after testing.
Matte forms mechanism:
NaOH solution is preferential etch to the corrosion of monocrystalline silicon piece, and on the different crystal faces of silicon, the number difference of dangling bonds causes response speed difference on different crystal faces, and this is the most basic the most direct reason that forms the pyramid matte.
As everyone knows, the monocrystalline of monocrystalline silicon piece is a diamond lattic structure, because the face velocity difference of each crystal face, corrodes selectively to each crystal face, and experiment learns that etch ratio [111] face of [100] face is big 35 times.The reason of preferential etch is: the shielding effect of water molecules, stopped the effect of Siliciumatom and OH radical ion, and the shielding effect of water molecules is relevant with atomic arrangement speed, the high more shielding of speed is obvious more, on [111] crystal face, each Siliciumatom has the atomic linkage of three covalent linkage and crystal face inside, dangling bonds that are exposed to the lattice outside are only arranged, [100] each Siliciumatom of crystal face has two covalent linkage and two dangling bonds, when corrosion reaction is carried out, OH root in the etchant solution combines with dangling bonds and forms etching, and the unit surface dangling bonds on the new lattice are many more, can cause the chemical reaction on surface to speed naturally.
The relation of the size of pyramid matte and monocrystalline silicon piece etch amount:
As shown in the figure, because silicon chip is a diamond lattic structure, pyramidal usually drift angle 70.52 degree of going up, inferior horn is 54.74 degree.The pros and cons of common silicon chip etching is simultaneously calculated if pyramid is approximately equilateral triangle when suede corrosion, if when the length of side is 5um, pyramidal height is 4.33um
When if the length of side is 0.8um, pyramidal height is 0.64um
When if the length of side is 0.6um, pyramidal height is 0.52um
So, the pyramidal height of 5um is respectively 0.8um and 0.6um pyramid height 6.7～8.3 times, in the manufacturing processed of matte, it is preferential etch, only [100] face is than [111] fast 35 times, [111] also in corrosion, if consider the factor of this respect, the etch amount of Great Pyramid is also bigger than above-mentioned calculating in fact.
Make the technical factor of monocrystalline silicon piece submicron matte:
1, silicon chip surface pre-washing is wanted thoroughly, otherwise can influence the continuity and the homogeneity of matte;
2, in the NaOH solution, the concentration of OH root is high more, the temperature height, and the time is long more, and then matte is big more;
If it is not thorough that 3 affected layers are removed, defectiveness exists, and can cause the matte size, and height is inhomogeneous, and is well-known, and chemical reaction is at first from some highly active local (defective where, active height) certainly;
4, Sodium Benzoate has blocked the silicon ion process in the absorption of silicon chip surface feature, perhaps in the silicon chip surface oxidation, generates extremely fine and close protective oxide film, and it stops matte oversize;
5, Sodium orthomolybdate is a kind of low contaminative metal-salt, is effective corrosion inhibitors in the safe alkaline medium, and Sodium orthomolybdate is a kind of passivation type inhibiter;
6, the aqueous solution of Sodium orthomolybdate and sodium phosphate has the effect of synergistic slow corrosion to erosion rate, and the threshold concentration of its inhibiter reduces, and when both total concns are 0.0015mg/L, and ratio be in (40: 60)～(10: 80), and on average corrosion inhibition rate reaches 91.5%;
7, the thermostability height of Sodium orthomolybdate, when temperature is higher than 70 ℃, in the solution of PH＞9, and other inhibiter is difficult to accomplish;
8, the aqueous solution of sodium phosphate, PO
4 3-Hydrolysis produces a large amount of OH
-With corrosion silicon single crystal, PO simultaneously
4 3-Or HPO
4 2-Play a part Virahol too, eliminate the gas big gun and slow down the corrosive effect.
Claims (1)
1. the manufacture method that the crystal orientation is [100] monocrystalline silicon piece submicron matte is characterized in that comprising the following steps:
(1) selecting resistivity is 0.5～20 Ω .cm, and the crystal orientation is [100], and silicon wafer thickness is the monocrystalline silicon piece of 180 ± 40um;
(2) silicon chip pre-washing is cleaned in the aqueous solution of the NaOH weight ratio that comprises 3%～7% monarch and 150 and 1%～2%, and solution temperature is controlled at 50～60 ℃, and the time is 4～6 minutes;
(3) remove affected layer, it is 10%～15%NaOH weight ratio water solution that monocrystalline silicon piece is put into concentration, and temperature is controlled at 60～80 ℃, and the time is 2～6 minutes;
(4) making herbs into wool is put into 1%～1.5% NaOH with monocrystalline silicon piece, 0.05%～1% Na
3PO
4.12H2O, 1%～1.5% Sodium Benzoate, in the aqueous solution of 0.1%～0.5% Sodium orthomolybdate weight ratio, temperature is controlled at 70～83 ℃, and the time is 5～25 minutes.
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Cited By (3)
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| CN103531656A (en) * | 2013-09-05 | 2014-01-22 | 西南科技大学 | Preparation method of textures of monocrystalline silicon piece of solar cell |
| CN104659156A (en) * | 2015-03-03 | 2015-05-27 | 中节能太阳能科技（镇江）有限公司 | Etching method of single crystalline silicon solar cell |
| CN108020537A (en) * | 2018-01-02 | 2018-05-11 | 中国计量大学 | A kind of preparation method of wide area surface enhancing Raman scattering substrate |
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| EP2019420A1 (en) * | 2003-05-07 | 2009-01-28 | Universität Konstanz | Device for texturising surfaces of silicon discs and uses of this device |
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| CN103531656A (en) * | 2013-09-05 | 2014-01-22 | 西南科技大学 | Preparation method of textures of monocrystalline silicon piece of solar cell |
| CN103531656B (en) * | 2013-09-05 | 2016-01-20 | 西南科技大学 | The preparation method of monocrystalline silicon chip of solar cell matte |
| CN104659156A (en) * | 2015-03-03 | 2015-05-27 | 中节能太阳能科技（镇江）有限公司 | Etching method of single crystalline silicon solar cell |
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| CN108020537A (en) * | 2018-01-02 | 2018-05-11 | 中国计量大学 | A kind of preparation method of wide area surface enhancing Raman scattering substrate |
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Application publication date: 20110727 |