CN102181935A - 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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- CN102181935A CN102181935A CN2010105199583A CN201010519958A CN102181935A CN 102181935 A CN102181935 A CN 102181935A CN 2010105199583 A CN2010105199583 A CN 2010105199583A CN 201010519958 A CN201010519958 A CN 201010519958A CN 102181935 A CN102181935 A CN 102181935A
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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 urea are 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 fluid of making monocrystalline silicon suede.
Background technology
Solar-energy photo-voltaic cell abbreviates photovoltaic cell as, is used for the luminous energy of the sun is converted into electric energy.Compare with conventional energy resources, photovoltaic cell is a kind of renewable and clean energy resource, helps environment protection, and can save the very expensive transmitting line of cost, so photovoltaic cell has broad application prospects.Monocrystalline silicon piece or polysilicon chip are the major partss 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 reflected light more than 40% at silicon chip surface, in order to improve photoelectric transformation 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 to silicon chip at silicon chip surface, suede structure can absorb more sunlight, reduce the reflection of light rate, thereby the raising short-circuit current finally reaches the effect that improves photoelectric transformation 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 has cheap and is applicable to the advantage of industrialization, therefore is widely used in preparing monocrystalline silicon suede at present.The ultimate principle that chemical corrosion method prepares monocrystalline silicon suede is, select for use the corrosive fluid of specific composition that silicon single crystal is carried out corrosion treatment, because (100) crystal face of silicon single crystal is compared as (111) crystal face or (110) crystal face with other crystal face, have corrosion speed faster, therefore can form similar pyramidal suede structure on the surface of silicon single crystal.
In the prior art, the multiple corrosive fluid that is used to prepare the monocrystalline silicon suede structure is disclosed.At present, corrosive fluid commonly used is generally the mixing solutions of NaOH, Virahol and water glass, and NaOH wherein is as oxygenant, and Virahol can be removed the hydrogen gas bubbles of generation, and water glass uses as additive.Experimental result shows, adopt water glass all undesirable for the effect of the reflectivity that reduces sunlight, raising short-circuit current and raising photoelectric transformation efficiency, so the present use of such corrosive fluid is subjected to certain restriction as the monocrystalline silicon suede of the corrosive fluid preparation of additive.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of corrosive fluid that is used to prepare monocrystalline silicon suede, and the monocrystalline silicon suede that uses this corrosive fluid to prepare can reduce the reflectivity for sunlight, can improve short-circuit current, improves photoelectric transformation efficiency.
In order to solve above technical problem, the invention provides a kind of corrosive fluid that is used to prepare monocrystalline silicon suede, in mass concentration, comprising:
NaOH and/or KOH 0.1%～0.5%;
Virahol and/or ethanol 5%～8%;
Sodium.alpha.-hydroxypropionate 0.3%～0.5%;
Urea 1%～2%;
Excess water.
Preferably, described corrosive fluid comprises 0.15%～0.45% NaOH.
Preferably, described corrosive fluid comprises 0.55%～7.5% Virahol.
Preferably, described corrosive fluid comprises 0.35%～0.5% Sodium.alpha.-hydroxypropionate.
Preferably, described corrosive fluid comprises 1%～1.5% urea.
The present invention also provides a kind of method of making monocrystalline silicon suede, comprising:
Silicon single crystal is corroded in the described corrosive fluid of above arbitrary technical scheme, and corrosion temperature is 65 ℃～83 ℃, and etching time is 12 minutes～35 minutes.
Preferably, described corrosion temperature is 66 ℃～80 ℃.
Preferably, described etching time is 15 minutes～25 minutes.
Preferably, before being corroded in corrosive fluid, described silicon single crystal also comprises:
Silicon single crystal is carried out rough polishing handle in alkaline solution, described alkaline solution comprises 5%～15% NaOH and/or KOH in mass concentration.
Preferably, the time that described rough polishing is handled is 0.5 minute～1.5 minutes, and the temperature that described rough polishing is handled is 60 ℃～70 ℃.
The present invention cooperates with alkaline solution and alcoholic solution and makes corrosive fluid by selecting for use Sodium.alpha.-hydroxypropionate and urea as additive.The experimental result table, compared with prior art, the monocrystalline silicon suede that adopts corrosive fluid 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 transformation 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, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The invention provides a kind of corrosive fluid that is used to make monocrystalline silicon suede,, comprising in mass concentration:
NaOH and/or KOH 0.1%～0.5%;
Virahol and/or ethanol 5%～8%;
Sodium.alpha.-hydroxypropionate 0.3%～0.5%;
Urea 1%～2%;
Excess water.
In the corrosive fluid 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 fluid provided by the invention, in mass concentration, also comprise 5%～8% Virahol and/or ethanol, preferred, Virahol and/or alcoholic acid mass concentration are 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 Virahol 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.alpha.-hydroxypropionate in the described corrosive fluid in mass concentration, preferred, the mass concentration of described Sodium.alpha.-hydroxypropionate is preferably 0.35%～0.45%, and more preferably 0.35%～0.4%.In the corrosive fluid 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.alpha.-hydroxypropionate that adds among the present invention and urea can improve the stability of corrosive fluid, reduce the surface tension of corrosive fluid, 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:
Silicon single crystal is corroded in the described corrosive fluid 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 fluid 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, effective constituent is wherein volatilized easily, the less stable of corrosive fluid.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 other crystal face may be eroded, thereby influence the surface quality of matte.
According to the present invention, before silicon single crystal being utilized above-mentioned corrosive fluid corrode, comprise also silicon single crystal carried out the step that rough polishing is handled that the purpose that rough polishing is handled is to remove mechanical damage layer.The step that described rough polishing is handled is preferably: utilizing concentration is that 5%～15% NaOH and/or KOH carry out rough polishing as polishing fluid to silicon single crystal and handle, preferably, described 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, the temperature of carrying out the rough polishing processing is preferably 60 ℃～85 ℃, and 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 silicon single crystal carried out rough polishing and handle to remove mechanical damage layer, remove the residue of monocrystalline silicon surface with the mode of cleaning, scavenging solution can be in pure water, acetone, the ethanol one or more.After removing the residue on surface, silicon single crystal is placed on carries out corrosion treatment in the corrosive fluid, the preparation matte.Behind the preparation matte, remove residue on the monocrystalline silicon suede with scavenging solution, scavenging solution 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 is not subjected to 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 fluid that uses in the present embodiment comprises in mass concentration: 0.1% NaOH, 8% Virahol, 0.3% Sodium.alpha.-hydroxypropionate, 1% urea, excess water.
Operation steps is as follows:
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) with the silicon single crystal after the purified rinse water rough polishing, remove surface residue;
3) silicon single crystal being dropped into temperature is to make matte in 78 ℃ the corrosive fluid, and etching time is 20 minutes;
4) with the silicon single crystal 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 fluid that uses in the present embodiment comprises in mass concentration: 0.5% NaOH, 5% Virahol, 0.5% Sodium.alpha.-hydroxypropionate, 2% urea, excess water.
Operation steps is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 3
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.2% NaOH, 6% Virahol, 0.25% Sodium.alpha.-hydroxypropionate, 1% urea, excess water.
Operation steps is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 4
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.3% NaOH, 5.5% Virahol, 0.45% Sodium.alpha.-hydroxypropionate, 2% urea, excess water.
Operation steps is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 5
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.3% NaOH, 6% Virahol, 0.4% Sodium.alpha.-hydroxypropionate, 1.5% urea, excess water.
Operation steps is identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 6
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.1% NaOH and 0.2% KOH, 6% Virahol, 0.4% Sodium.alpha.-hydroxypropionate, 1.5% urea, excess water.
In the operation steps, the corrosive fluid temperature in the step 3) is 75 ℃, and etching time is 15 minutes, and all the other operation stepss are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 7
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.2% NaOH and 0.1% KOH, 3% Virahol and 1% ethanol, 0.4% Sodium.alpha.-hydroxypropionate, 1.5% urea, excess water.
In the operation steps, the corrosive fluid temperature in the step 3) is 70 ℃, and etching time is 25 minutes, and all the other operation stepss are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 8
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.1% NaOH and 0.1% KOH, 1% Virahol and 2% ethanol, 0.3% Sodium.alpha.-hydroxypropionate, 1.5% urea, excess water.
In the operation steps, the corrosive fluid temperature in the step 3) is 68 ℃, and etching time is 25 minutes, and all the other operation stepss are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 9
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.15% NaOH and 0.13% KOH, 1.5% Virahol and 1.5% ethanol, 0.4% Sodium.alpha.-hydroxypropionate, 1.5% urea, excess water.
In the operation steps, the corrosive fluid temperature in the step 3) is 78 ℃, and etching time is 20 minutes, and all the other operation stepss are identical with embodiment 1.
Monocrystalline silicon piece is assembled into battery, measures electrical property and list in table 1.
Embodiment 10
The corrosive fluid that uses in the present embodiment comprises in mass concentration: 0.12% Na0H and 0.18% KOH, 1.3% Virahol and 1.7% ethanol, 0.38% Sodium.alpha.-hydroxypropionate, 1.6% urea, excess water.
In the operation steps, the corrosive fluid temperature in the step 3) is 75 ℃, and etching time is 18 minutes, and all the other operation stepss 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 fluid that uses in this comparative example comprises in mass concentration: 0.1NaOH%, 0.3% water glass, 6% Virahol, excess water.
Operation steps 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 fluid that uses in this comparative example comprises in mass concentration: 0.2NaOH%, 0.3% water glass, 6% Virahol, excess water.
Operation steps 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 fluid that uses in this comparative example comprises in mass concentration: 0.2NaOH%, 0.2% water glass, 5% Virahol, excess water.
Operation steps 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 fluid that uses in this comparative example comprises in mass concentration: 0.3NaOH%, 0.3% water glass, 5% Virahol, excess water.
Operation steps 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 fluid that uses in this comparative example comprises in mass concentration: 0.2NaOH%, 0.3% water glass, 4% Virahol, excess water.
Operation steps 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 fluid that uses in this comparative example is identical with comparative example 1.
Operation steps 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 fluid that uses in this comparative example is identical with comparative example 2.
Operation steps 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 fluid that uses in this comparative example is identical with comparative example 3.
Operation steps 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 fluid that uses in this comparative example is identical with comparative example 4.
Operation steps 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 fluid that uses in this comparative example is identical with comparative example 5.
Operation steps 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 more tiny and uniform suede structure.The result of contrast table 1 and table 2 can find that the reflectivity of the silicon single crystal of present embodiment preparation is 6%～9%, is lower than 11%～16% in the comparative example, has higher assimilation effect for sun power.In addition, the monocrystalline silicon suede of embodiment of the invention preparation has higher short-circuit current and high photoelectric transformation efficiency.
More than the method that is used to make the corrosive fluid of monocrystalline silicon suede and utilizes this corrosive fluid to make monocrystalline silicon suede provided by the present invention is described in detail.Used specific case herein principle of the present invention and embodiment 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 domain of claim of the present invention.
Claims (10)
1. corrosive fluid that is used to make monocrystalline silicon suede in mass concentration, comprising:
NaOH and/or KOH 0.1%～0.5%;
Virahol and/or ethanol 5%～8%;
Sodium.alpha.-hydroxypropionate 0.3%～0.5%;
Urea 1%～2%;
Excess water.
2. corrosive fluid according to claim 1 is characterized in that, comprising:
NaOH 0.15％～0.45％。
3. corrosive fluid according to claim 1 is characterized in that, comprising:
Virahol 5.5%～7.5%.
4. corrosive fluid according to claim 1 is characterized in that, comprising:
Sodium.alpha.-hydroxypropionate 0.35%～0.5%.
5. corrosive fluid 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:
Silicon single crystal is corroded in each described corrosive fluid 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, described corrosion temperature is 66 ℃～80 ℃.
8. method according to claim 6 is characterized in that, described etching time is 15 minutes～25 minutes.
9. method according to claim 6 is characterized in that, also comprises before described silicon single crystal is corroded in corrosive fluid:
Silicon single crystal is carried out rough polishing handle in alkaline solution, described alkaline solution comprises 5%～15% NaOH and/or KOH by weight percentage.
10. method according to claim 9 is characterized in that, the time that described rough polishing is handled is 0.5 minute～1.5 minutes, and the temperature that described rough polishing is handled is 60 ℃～70 ℃.
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| CN111501105A (en) * | 2020-05-25 | 2020-08-07 | 常州时创能源股份有限公司 | Monocrystalline silicon piece texturing additive and application thereof |
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