CN102181935B - Method and corrosive liquid for making texture surface of monocrystalline silicon - Google Patents
Method and corrosive liquid for making texture surface of monocrystalline silicon Download PDFInfo
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- CN102181935B CN102181935B CN201010519958A CN201010519958A CN102181935B CN 102181935 B CN102181935 B CN 102181935B CN 201010519958 A CN201010519958 A CN 201010519958A CN 201010519958 A CN201010519958 A CN 201010519958A CN 102181935 B CN102181935 B CN 102181935B
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Abstract
The invention provides a corrosive liquid for making the texture surface of monocrystalline silicon. The corrosive liquid comprises the following components based on mass concentration: 0.1 to 0.5 percent of NaOH and/or KOH, 5 to 8 percent of isopropyl alcohol and/or ethanol, 0.3 to 0.5 percent of sodium lactate, 1 to 2 percent of urea and the balance of water; and the sodium lactate and the ureaare selected as additives and are matched with an alkali solution and an alcoholic solution to prepare the corrosive liquid. Compared with the prior art, the invention has the advantages that: experimental results show that the reflectivity of solar light can be reduced to between 6 and 8 percent by adopting the texture surface of the monocrystalline silicon prepared by the corrosive liquid. Moreover, the texture surface of the monocrystalline silicon has higher short-circuit current and higher photoelectric conversion efficiency.
Description
Technical field
The present invention relates to be used to prepare the single silicon field of solar cell, be specifically related to a kind of method and corrosive liquid of making monocrystalline silicon suede.
Background technology
Solar-energy photo-voltaic cell abbreviates photovoltaic cell as, is used for being converted into electric energy to the luminous energy of the sun.Compare with conventional energy resource, photovoltaic cell is a kind of renewable and clean energy resource, helps environmental protection, and can save the very expensive transmission line of cost, so photovoltaic cell has broad application prospects.Monocrystalline silicon piece or polysilicon chip are the critical pieces of preparation photovoltaic cell, and when solar light irradiation was on monocrystalline silicon piece or polysilicon chip, luminous energy can change electric energy into.
Solar light irradiation generally has the reverberation more than 40% at silicon chip surface, in order to improve photoelectric conversion efficiency, needs to increase the assimilation effect of silicon chip to sunlight, makes reflectivity reduce to minimum.At present; In order to reduce the reflectivity of sunlight at silicon chip surface; Need carry out surface treatment to form tiny and uniform suede structure at silicon chip surface to silicon chip, suede structure can absorb more sunlight, reduces the reflection of light rate; Thereby the raising short circuit current finally reaches the effect that improves photoelectric conversion efficiency.
At present, the monocrystalline silicon suede preparation method has chemical corrosion method, plasma etching method and mechanical carving groove method etc.Compare with other two kinds of methods, chemical corrosion method have cheap be applicable to the advantage of industrialization, therefore be widely used in preparing monocrystalline silicon suede at present.The basic principle that chemical corrosion method prepares monocrystalline silicon suede is; Select for use the corrosive liquid of specific composition that monocrystalline silicon is carried out corrosion treatment; Because (100) crystal face of monocrystalline silicon is compared like (111) crystal face or (110) crystal face with other crystal face; Have corrosion rate faster, therefore can form similar pyramidal suede structure on the surface of monocrystalline silicon.
In the prior art, the multiple corrosive liquid that is used to prepare the monocrystalline silicon suede structure is disclosed.At present, corrosive liquid commonly used is generally the mixed solution of NaOH, isopropyl alcohol and sodium metasilicate, and NaOH wherein is as oxidant, and isopropyl alcohol can be removed the hydrogen gas bubbles of generation, and sodium metasilicate uses as additive.Experimental result shows; Adopt sodium metasilicate all undesirable for the effect of the reflectivity that reduces sunlight, raising short circuit current and raising photoelectric conversion efficiency, so the present use of such corrosive liquid receive certain restriction as the monocrystalline silicon suede of the corrosive liquid preparation of additive.
Summary of the invention
The problem that the present invention will solve is to provide a kind of corrosive liquid that is used to prepare monocrystalline silicon suede, uses the monocrystalline silicon suede of this corrosive liquid preparation can reduce the reflectivity for sunlight, can improve short circuit current, improves photoelectric conversion efficiency.
In order to solve above technical problem, the present invention provides a kind of corrosive liquid that is used to prepare monocrystalline silicon suede, in mass concentration, comprising:
NaOH and/or KOH 0.1%～0.5%;
Isopropyl alcohol and/or ethanol 5%～8%;
Sodium lactate 0.3%～0.5%;
Urea 1%～2%;
Excess water.
Preferably, said corrosive liquid comprises 0.15%～0.45% NaOH.
Preferably, said corrosive liquid comprises 0.55%～7.5% isopropyl alcohol.
Preferably, said corrosive liquid comprises 0.35%～0.5% sodium lactate.
Preferably, said corrosive liquid comprises 1%～1.5% urea.
The present invention also provides a kind of method of making monocrystalline silicon suede, comprising:
Monocrystalline silicon is corroded in the described corrosive liquid of above arbitrary technical scheme, and corrosion temperature is 65 ℃～83 ℃, and etching time is 12 minutes～35 minutes.
Preferably, said corrosion temperature is 66 ℃～80 ℃.
Preferably, said etching time is 15 minutes～25 minutes.
Preferably,, said monocrystalline silicon also comprises before being corroded in corrosive liquid:
Monocrystalline silicon is carried out rough polishing handle in aqueous slkali, said aqueous slkali comprises 5%～15% NaOH and/or KOH in mass concentration.
Preferably, the time that said rough polishing is handled is 0.5 minute～1.5 minutes, and said rough polishing treatment temperature is 60 ℃～70 ℃.
The present invention cooperates with aqueous slkali and alcoholic solution and processes corrosive liquid through selecting for use sodium lactate and urea as additive.The experimental result table; Compared with prior art; The monocrystalline silicon suede that adopts corrosive liquid provided by the invention preparation can be reduced to 6%～8% to the reflectivity of sunlight, and the monocrystalline silicon suede of the present invention's preparation has the photoelectric conversion efficiency of higher short circuit current and Geng Gao.
Description of drawings
Fig. 1 is the SEM photo of the monocrystalline silicon suede of the embodiment of the invention 1 preparation;
Fig. 2 is the SEM photo of the monocrystalline silicon suede of comparative example 1 preparation of the present invention.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
The present invention provides a kind of corrosive liquid that is used to make monocrystalline silicon suede, in mass concentration, comprising:
NaOH and/or KOH 0.1%～0.5%;
Isopropyl alcohol and/or ethanol 5%～8%;
Sodium lactate 0.3%～0.5%;
Urea 1%～2%;
Excess water.
In the corrosive liquid provided by the invention, in mass concentration, comprise 0.1%～0.5% NaOH and/or KOH, preferred, the mass concentration of NaOH and/or KOH is 0.15%～0.45%, more preferably 0.2%～4%, more preferably 0.25%～0.35%.In the corrosive liquid provided by the invention, in mass concentration, also comprise 5%～8% isopropyl alcohol and/or ethanol, preferred, the mass concentration of isopropyl alcohol and/or ethanol is 5.5%～7.5%, more preferably 6%～7%.
NaOH and/or KOH produce hydrogen at monocrystalline silicon surface when monocrystalline silicon surface is made matte, hydrogen gas bubbles is easily attached to silicon face, thereby can hinder part and the NaOH and/or the KOH reaction of being blocked by bubble, thereby cause the inhomogeneous of reaction.Because isopropyl alcohol and/or ethanol have the capillary effect of good reduction, can also eliminate the hydrogen gas bubbles that produces in the reaction, thereby help preparing the matte of stable homogeneous.
According to the present invention, also comprise 0.3%～0.5% sodium lactate in the said corrosive liquid in mass concentration, preferred, the mass concentration of said sodium lactate is preferably 0.35%～0.45%, and more preferably 0.35%～0.4%.In the corrosive liquid provided by the invention, also comprise 1%～2% urea in mass concentration, preferred, the mass concentration 1.1%～1.9% of urea, more preferably 1.2%～1.8%, more preferably 1.3%～1.5%.Sodium lactate that adds among the present invention and urea can improve the stability of corrosive liquid, reduce the surface tension of corrosive liquid, thereby help the more stable matte of preparation quality
A kind of embodiment of making the method for monocrystalline silicon suede provided by the invention comprises:
Monocrystalline silicon is corroded in the described corrosive liquid of above technical scheme, and corrosion temperature is 65 ℃～83 ℃, and etching time is 12 minutes～35 minutes.
According to the present invention, when utilizing above-mentioned corrosive liquid that monocrystalline silicon surface is corroded, corrosion temperature is preferably 68 ℃～81 ℃, more preferably 70 ℃～78 ℃.Temperature is crossed when hanging down, and reaction can not be carried out fully, thereby influences the surface quality of matte.If temperature is too high, active ingredient is wherein volatilized easily, the less stable of corrosive liquid.The preferred etching time of the present invention is 15 minutes～30 minutes, more preferably 18 minutes～25 minutes, and more preferably 20 minutes～24 minutes.When etching time was too short, corrosive effect was relatively poor; If etching time is long, then may other crystal face be eroded, thereby influence the surface quality of matte.
According to the present invention, before monocrystalline silicon being utilized above-mentioned corrosive liquid corrode, comprise also monocrystalline silicon carried out the rough polishing processed steps that the purpose that rough polishing is handled is to remove mechanical damage layer.Said rough polishing processed steps is preferably: utilizing concentration is that 5%～15% NaOH and/or KOH carry out rough polishing as polishing fluid to monocrystalline silicon and handle; Preferably; Said polishing fluid comprises 7%～12% NaOH and/or KOH; More preferably 8%～11% NaOH and/or KOH, more preferably 10%.
According to the present invention, carry out the rough polishing treatment temperature and be preferably 60 ℃～85 ℃, more preferably 62 ℃～82 ℃, more preferably 65 ℃～80 ℃, more preferably 68 ℃～75 ℃.According to the present invention, the time of carrying out the rough polishing processing is preferably 0.5～10 minute, and more preferably 1 minute～8 minutes, more preferably 1 minute～5 minutes, more preferably 1 minute～1.5 minutes.
After monocrystalline silicon carried out rough polishing and handle to remove mechanical damage layer, remove the residue of monocrystalline silicon surface with the mode of cleaning, cleaning fluid can be in pure water, acetone, the ethanol one or more.After removing the residue on surface, monocrystalline silicon is placed on carries out corrosion treatment in the corrosive liquid, the preparation matte.Behind the preparation matte, remove the residue on the monocrystalline silicon suede with cleaning fluid, cleaning fluid can be in pure water, acetone, the ethanol one or more.After washing the residue on the monocrystalline silicon suede, monocrystalline silicon piece is being dried processing.
Below with specific embodiment effect of the present invention is described, but protection scope of the present invention does not receive the restriction of embodiment.
In following examples, silicon chip is the p type single crystal silicon sheet, and resistivity is 5 Ω cm.
Embodiment 1
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.1% NaOH, 8% isopropyl alcohol, 0.3% sodium lactate, 1% urea, excess water.
Operating procedure is following:
1) monocrystalline silicon piece being dropped into temperature is that 65 ℃, concentration are that 10% NaOH solution carries out rough polishing and handles and remove mechanical damage layer, and the time that rough polishing is handled is 1.5 minutes;
2), remove surface residue with the monocrystalline silicon after the purified rinse water rough polishing;
3) monocrystalline silicon being dropped into temperature is to make matte in 78 ℃ the corrosive liquid, and etching time is 20 minutes;
4) with the monocrystalline silicon after the purified rinse water corrosion, remove surface residue;
5) in drier, monocrystalline silicon piece is dried.
Observe the monocrystalline silicon surface pattern with SEM, as shown in Figure 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 2
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.5% NaOH, 5% isopropyl alcohol, 0.5% sodium lactate, 2% urea, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 3
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.2% NaOH, 6% isopropyl alcohol, 0.25% sodium lactate, 1% urea, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 4
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.3% NaOH, 5.5% isopropyl alcohol, 0.45% sodium lactate, 2% urea, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 5
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.3% NaOH, 6% isopropyl alcohol, 0.4% sodium lactate, 1.5% urea, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 6
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.1% NaOH and 0.2% KOH, 6% isopropyl alcohol, 0.4% sodium lactate, 1.5% urea, excess water.
In the operating procedure, the corrosive liquid temperature in the step 3) is 75 ℃, and etching time is 15 minutes, and all the other operating procedures are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 7
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.2% NaOH and 0.1% KOH, 3% isopropyl alcohol and 1% ethanol, 0.4% sodium lactate, 1.5% urea, excess water.
In the operating procedure, the corrosive liquid temperature in the step 3) is 70 ℃, and etching time is 25 minutes, and all the other operating procedures are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 8
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.1% NaOH and 0.1% KOH, 1% isopropyl alcohol and 2% ethanol, 0.3% sodium lactate, 1.5% urea, excess water.
In the operating procedure, the corrosive liquid temperature in the step 3) is 68 ℃, and etching time is 25 minutes, and all the other operating procedures are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 9
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.15% NaOH and 0.13% KOH, 1.5% isopropyl alcohol and 1.5% ethanol, 0.4% sodium lactate, 1.5% urea, excess water.
In the operating procedure, the corrosive liquid temperature in the step 3) is 78 ℃, and etching time is 20 minutes, and all the other operating procedures are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 10
The corrosive liquid that uses in the present embodiment comprises in mass concentration: 0.12% Na0H and 0.18% KOH, 1.3% isopropyl alcohol and 1.7% ethanol, 0.38% sodium lactate, 1.6% urea, excess water.
In the operating procedure, the corrosive liquid temperature in the step 3) is 75 ℃, and etching time is 18 minutes, and all the other operating procedures are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, and measurement performance is listed in table 1.
The The performance test results of the monocrystalline silicon piece of table 1 embodiment of the invention preparation
Comparative example 1
The corrosive liquid that uses in this comparative example comprises in mass concentration: 0.1NaOH%, 0.3% sodium metasilicate, 6% isopropyl alcohol, excess water.
Operating procedure is identical with embodiment 1.
Observe the monocrystalline silicon surface pattern with SEM, as shown in Figure 2.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 2
The corrosive liquid that uses in this comparative example comprises in mass concentration: 0.2NaOH%, 0.3% sodium metasilicate, 6% isopropyl alcohol, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 3
The corrosive liquid that uses in this comparative example comprises in mass concentration: 0.2NaOH%, 0.2% sodium metasilicate, 5% isopropyl alcohol, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 4
The corrosive liquid that uses in this comparative example comprises in mass concentration: 0.3NaOH%, 0.3% sodium metasilicate, 5% isopropyl alcohol, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 5
The corrosive liquid that uses in this comparative example comprises in mass concentration: 0.2NaOH%, 0.3% sodium metasilicate, 4% isopropyl alcohol, excess water.
Operating procedure is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 6
The corrosive liquid that uses in this comparative example is identical with comparative example 1.
Operating procedure is identical with embodiment 6.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 7
The corrosive liquid that uses in this comparative example is identical with comparative example 2.
Operating procedure is identical with embodiment 7.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 8
The corrosive liquid that uses in this comparative example is identical with comparative example 3.
Operating procedure is identical with embodiment 8.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 9
The corrosive liquid that uses in this comparative example is identical with comparative example 4.
Operating procedure is identical with embodiment 9.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
Comparative example 10
The corrosive liquid that uses in this comparative example is identical with comparative example 5.
Operating procedure is identical with embodiment 10.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 2.
The The performance test results of the monocrystalline silicon piece of table 2 comparative example preparation of the present invention
The SEM result of comparison diagram 1 and Fig. 2 can find that the monocrystalline silicon suede of embodiment of the invention preparation has tiny and uniform suede structure more.The result of contrast table 1 and table 2 can find that the reflectivity of the monocrystalline silicon of present embodiment preparation is 6%～9%, is lower than 11%～16% in the comparative example, has higher assimilation effect for solar energy.In addition, the monocrystalline silicon suede of embodiment of the invention preparation has higher short circuit current and high photoelectric conversion efficiency.
More than the method that is used to make the corrosive liquid of monocrystalline silicon suede and utilizes this corrosive liquid to make monocrystalline silicon suede provided by the present invention has been carried out detailed introduction.Used concrete example among this paper principle of the present invention and execution mode are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection range of claim of the present invention.
Claims (10)
1. corrosive liquid that is used to make monocrystalline silicon suede in mass concentration, comprising:
NaOH and/or KOH 0.1%～0.5%;
Isopropyl alcohol and/or ethanol 5%～8%;
Sodium lactate 0.3%～0.5%;
Urea 1%～2%;
Excess water.
2. corrosive liquid according to claim 1 is characterized in that, comprising:
NaOH 0.15％～0.45％。
3. corrosive liquid according to claim 1 is characterized in that, comprising:
Isopropyl alcohol 5.5%～7.5%.
4. corrosive liquid according to claim 1 is characterized in that, comprising:
Sodium lactate 0.35%～0.5%.
5. corrosive liquid according to claim 1 is characterized in that, comprising:
Urea 1%～1.5%.
6. a method of making the solar monocrystalline silicon matte is characterized in that, comprising:
Monocrystalline silicon is corroded in each described corrosive liquid of claim 1 to 5, and corrosion temperature is 65 ℃～83 ℃, and etching time is 12 minutes～35 minutes.
7. method according to claim 6 is characterized in that, said corrosion temperature is 66 ℃～80 ℃.
8. method according to claim 6 is characterized in that, said etching time is 15 minutes～25 minutes.
9. method according to claim 6 is characterized in that, before said monocrystalline silicon is corroded in corrosive liquid, also comprises:
Monocrystalline silicon is carried out rough polishing handle in aqueous slkali, said aqueous slkali comprises 5%～15% NaOH and/or KOH by weight percentage.
10. method according to claim 9 is characterized in that, the time that said rough polishing is handled is 0.5 minute～1.5 minutes, and said rough polishing treatment temperature is 60 ℃～70 ℃.
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| CN103184523B (en) * | 2011-12-27 | 2016-01-27 | 中建材浚鑫科技股份有限公司 | The preparation method of a kind of silicon single crystal Wool-making agent and textured mono-crystalline silicon |
| US20140004701A1 (en) * | 2012-06-27 | 2014-01-02 | Rohm And Haas Electronic Materials Llc | Texturing of monocrystalline semiconductor substrates to reduce incident light reflectance |
| CN102856189B (en) * | 2012-09-20 | 2015-09-09 | 苏州易益新能源科技有限公司 | A kind of crystal silicon chip surface-treated method |
| CN102912450B (en) * | 2012-10-22 | 2015-07-01 | 江苏荣马新能源有限公司 | Monocrystalline silicon flocking additive |
| CN104347756A (en) * | 2013-08-08 | 2015-02-11 | 上海神舟新能源发展有限公司 | One-sided polishing method for monocrystalline silicon wafer for solar battery |
| CN104988581A (en) * | 2015-08-04 | 2015-10-21 | 绍兴拓邦电子科技有限公司 | Monocrystalline silicon piece spraying and texturing additive with high boiling point |
| CN105133024A (en) * | 2015-08-21 | 2015-12-09 | 合肥中南光电有限公司 | Low-residue monocrystalline silicon slice texturing solution and preparation method thereof |
| CN105113010A (en) * | 2015-08-21 | 2015-12-02 | 合肥中南光电有限公司 | Environmentally-friendly monocrystalline silicon wafer texturing liquor and preparation method thereof |
| CN105696083B (en) * | 2016-01-29 | 2018-03-09 | 盐城阿特斯协鑫阳光电力科技有限公司 | A kind of preparation method of solar battery pile face |
| CN107338480A (en) * | 2017-08-24 | 2017-11-10 | 嘉兴尚能光伏材料科技有限公司 | A kind of monocrystalline silicon silicon wafer fine hair making method and its flocking additive |
| CN108004598A (en) * | 2017-12-01 | 2018-05-08 | 绍兴拓邦电子科技有限公司 | A kind of crystalline silicon etching edge additive and its application method |
| CN111501105B (en) * | 2020-05-25 | 2021-02-05 | 常州时创能源股份有限公司 | Monocrystalline silicon piece texturing additive and application thereof |
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| CN101851757A (en) * | 2010-06-08 | 2010-10-06 | 常州时创能源科技有限公司 | Additive of wool making solution for monocrystalline silicon pieces and using method |
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