CN114318549A - Monocrystalline silicon texturing additive for weak rough polishing process and use method - Google Patents
Monocrystalline silicon texturing additive for weak rough polishing process and use method Download PDFInfo
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Abstract
The invention discloses a monocrystalline silicon texturing additive for a weak rough polishing process and a using method thereof. Compared with the texturing additive of the existing texturing process without rough polishing, the monocrystalline silicon texturing additive is matched with the weak rough polishing process, so that the yield of monocrystalline silicon battery pieces is effectively improved, the large-size flaking development of silicon pieces is promoted, and the manufacturing cost of solar battery pieces is reduced; the additive has a large using window, is suitable for the process of reducing weight of 0.03-0.10g of the silicon wafer by rough polishing, and has strong operability. The surface of the silicon wafer after the weak rough polishing is still flat, and the additive can be used for texturing to form a better textured surface, so that the light trapping effect of the silicon wafer is improved, the lower reflectivity is obtained, and the photoelectric conversion efficiency of the solar cell is improved.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon battery production, and particularly relates to a monocrystalline silicon texturing additive for a weak rough polishing process and a using method thereof.
Background
With the improvement of the technological level, people are increasingly aware of renewable energy sources, and especially the development and utilization of solar energy are increasingly paid more attention. Photovoltaic power generation is one of important methods for directly utilizing solar energy, and the silicon surface is textured to form a pyramid through wet etching, so that the surface reflectivity of the silicon wafer is reduced, and the photoelectric conversion efficiency is improved.
Solar cells have high requirements on the surface cleanliness of silicon, which is the most important material in solar photovoltaic modules. The earliest silicon wafer surface pre-cleaning is to remove the dirt such as particles, organic matters, finger marks and the like on the silicon surface by a rough polishing process, the weight of rough polishing is reduced to more than 0.2g, and the weight of texturing is reduced to more than 0.4g, so that certain requirements are required for the thickness of the silicon wafer, the silicon wafer cannot be too thin, and otherwise, the silicon wafer has a high fragment rate.
The theoretical photoelectric conversion efficiency of the silicon solar cell is about 33 percent, but the actual solar conversion efficiency is between 22 and 25 percent at present, the photoelectric conversion efficiency of the solar cell is more and more limited, in order to reduce the manufacturing cost of the solar cell, the silicon slice is flaked and large-sized to become the next development trend, the mainstream texturing process in the market is not rough polished at present, but the diamond line marks of the silicon slice are more and more obvious along with the popularization of the diamond line cutting silicon slice process, the stains such as the diamond line marks on the silicon surface, particles on the surface, organic matters, fingerprints and the like are difficult to remove by the texturing process without rough polishing at present, the stains and the diamond line marks are difficult to realize only by the texturing etching, but the silicon slice is thinner and cannot adapt to the previous high-weight-reducing rough polishing process, so the diamond line marks and the stains can only be removed by the weak rough polishing, and the texturing additive which is corresponding to the weak rough polishing process is required to be developed, the method has great significance for promoting the development of the solar cell.
Disclosure of Invention
In order to reduce the manufacturing cost of the solar cell, promote the thinning and large-size development of the silicon wafer and effectively remove a damaged layer and dirt of the silicon wafer, the invention provides the monocrystalline silicon texturing additive for the weak rough polishing process and the use method thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme: a monocrystalline silicon texturing additive for a weak rough polishing process comprises a defoaming agent, an auxiliary nucleating agent, a surfactant, a pH regulator, a complexing agent, organic acid and deionized water.
Preferably, the monocrystalline silicon texturing additive comprises the following components in percentage by weight:
preferably, the defoaming agent can make the generated bubbles quickly separate from the silicon surface to promote the further corrosion of the silicon wafer, and the silicon wafer is a glycoside compound which mainly comprises one or more of dehydrodicladol glucoside, isolarch phenol glucoside, hyperoside, quercetin arabinoside, quercetin rhamnosyl, isorhamnetin galactoside, icariin, phenethyl rutinoside and phenethyl glucoside. The role of the defoaming agent is to ensure that the generated bubbles are quickly separated from the silicon surface and promote the further corrosion of the silicon wafer.
Preferably, the auxiliary nucleating agent enhances the anisotropic corrosion of the etching solution on the silicon wafer, and is a phenolic acid compound mainly comprising any one or more of gallic acid, caffeic acid, chlorogenic acid, vanillic acid, protocatechuic acid, syringic acid and ferulic acid. The auxiliary nucleating agent is used for enhancing the anisotropic corrosion effect of the corrosive liquid on the silicon wafer.
Preferably, the surfactant has excellent wettability, promotes sufficient contact between silicon and a corrosive solution, and is favorable for anisotropic corrosion of silicon, and the surfactant is an anionic surfactant mainly comprising one or more of dodecyl sulfate potassium salt, polyoxyethylene ether phosphate potassium salt, fatty alcohol phosphate potassium salt, isomeric dodecyl phosphate potassium salt, phenol ether phosphate potassium salt, isomeric tridecyl alcohol phosphate potassium salt, lauryl phosphate potassium salt, and cetyl alcohol phosphate potassium salt. The surfactant provides excellent wettability, promotes the silicon to be fully contacted with the corrosive liquid, and is beneficial to anisotropic corrosion of the silicon.
Preferably, the PH regulator is one or more of sodium carbonate, sodium bicarbonate, sodium citrate, sodium acetate, sodium lactate, and sodium formate. The PH regulator is mainly used for controlling the stability of the monocrystalline silicon texturing additive and is beneficial to the uniformity of etched pyramids.
Preferably, in order to complex the metal ions adsorbed on the surface of the silicon wafer, the complexing agent is any one or more of sodium pyrophosphate, thiosulfate, sulfite, sodium ethoxide and ethylenediamine tetraacetic acid.
Preferably, the organic acid plays a role in controlling the reaction rate to obtain uniform pyramids, and the pyramids are one or more of tartaric acid, oxalic acid, malic acid, benzoic acid and salicylic acid.
A method of using a monocrystalline silicon texturing additive for a soft rough polishing process, the method comprising the steps of:
step 1), preparing a texturing additive: mixing the defoaming agent, the auxiliary nucleating agent, the surfactant, the pH regulator, the complexing agent, the organic acid and the deionized water according to the weight percentage to prepare the monocrystalline silicon texturing additive;
step 2), preparing alkali liquor: weighing a certain mass of alkali, adding the alkali into deionized water to prepare an alkali solution with the concentration of 0.50-2.00 wt%, wherein the alkali is sodium hydroxide or potassium hydroxide;
step 3), preparing a texturing solution: adding the texturing additive prepared in the step 1) into the alkali solution prepared in the step 2), and stirring and circulating to obtain a monocrystalline silicon texturing solution;
step 4), silicon wafer cleaning: preparing 0.05-0.70 wt% of alkali liquor, placing the silicon wafer into the alkali liquor for weak rough polishing, cleaning the silicon wafer with alkali-containing hydrogen peroxide water after the weak rough polishing, and then washing with water to prepare the silicon wafer for removing the damaged layer and dirt, wherein the alkali liquor in the step 4 is 0.05-0.70 wt% of potassium hydroxide or sodium hydroxide, and the alkali-containing hydrogen peroxide is a mixed solution of 1-5 wt% of hydrogen peroxide water and 0.2-0.5 wt% of potassium hydroxide or sodium hydroxide;
step 5), texturing: immersing the silicon wafer after the weak rough polishing into monocrystalline silicon texturing solution suitable for the weak rough polishing process for texturing, and etching the surface of the silicon wafer to form a pyramid textured surface;
step 6), soaking the textured monocrystalline silicon wafer in the step 5) in deionized water at room temperature for cleaning for 2min, and then performing mixed acid cleaning for 5-10min, wherein the mixed acid liquid in the step 6) is HF/HCL, and the concentration of the mixed acid is 1-4 mol/L;
and 7), immersing the monocrystalline silicon wafer after acid washing in deionized water for washing for 2min, then immersing in the deionized water at 60 ℃ for slowly pulling out, and drying the monocrystalline silicon wafer in a drying box at 80 ℃ for 30 min.
Preferably, the cleaning temperature of the silicon wafer is 60-75 ℃; the silicon wafer cleaning time is 100-150 s; the temperature of the wool making liquid is 75-85 ℃; the texturing time is 300-500 s.
The invention has the beneficial effects that: compared with the texturing additive of the existing texturing process without rough polishing, the monocrystalline silicon texturing additive is matched with the weak rough polishing process, so that the yield of monocrystalline silicon battery pieces is effectively improved, the large-size flaking development of silicon pieces is promoted, and the manufacturing cost of solar battery pieces is reduced; the additive has a large using window, is suitable for the process of reducing weight of 0.03-0.10g of the silicon wafer by rough polishing, and has strong operability. The surface of the silicon wafer after the weak rough polishing is still flat, and the additive can be used for texturing to form a better textured surface, so that the light trapping effect of the silicon wafer is improved, the lower reflectivity is obtained, and the photoelectric conversion efficiency of the solar cell is improved.
Drawings
FIG. 1 is an SEM image of a silicon wafer surface after texturing of example 1;
FIG. 2 is an SEM image of the surface of a textured silicon wafer of example 2;
FIG. 3 is an SEM image of the surface of a textured silicon wafer of example 3.
FIG. 4 is an SEM image of the surface of a silicon wafer after texturing of a comparative example.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1) Preparing an additive: using 1L of deionized water as a solvent, sequentially adding 10g of dehydrodibastic glucoside, 4g of protocatechuic acid, 0.02g of potassium fatty alcohol phosphate, 0.6g of sodium carbonate, 0.2g of sodium thiosulfate and 0.6g of oxalic acid, and fully stirring and uniformly mixing the above substances; 2) preparing a texturing solution: adding 500g of sodium hydroxide into 50L of deionized water, adding 250ml of additive, and fully and uniformly stirring to obtain alkaline texturing solution; 3) preparing a silicon wafer cleaning solution: adding 100g of sodium hydroxide into 50L of deionized water, fully dissolving and uniformly stirring to prepare a silicon wafer cleaning solution; 4) preparing a hydrogen peroxide precleaning liquid: adding 500ml of 30% hydrogen peroxide into 50L of deionized water, adding 100g of alkali, and uniformly stirring to obtain hydrogen peroxide pre-cleaning liquid; 5) preparing a mixed acid solution: HF and HCl in a molar ratio of 1: 2, preparing mixed acid with the concentration of 1.5 moL/L; 6) putting a silicon wafer into silicon wafer cleaning liquid for weak rough polishing, wherein the corrosion weight is reduced by 0.03g, putting the roughly polished wafer into a hydrogen peroxide pre-cleaning tank for cleaning for 120s, then cleaning for 120s with pure water, putting the cleaned wafer into a texturing liquid for reaction for 300s, and the texturing temperature is 78 ℃; 7) putting the textured sheet into a mixed acid solution for 120s, and then cleaning the textured sheet for 120s by using deionized water; 8) and after being cleaned by deionized water, the silicon wafer is dipped in the deionized water at 60 ℃ and slowly pulled out, and the silicon wafer is dried in a drying oven at 70 ℃ for 30 min. The surface of the crystal silicon wafer prepared in this example was observed as shown in fig. 1. As can be seen from FIG. 1, the surface of the silicon wafer after the weak rough polishing is still flat, so that a better suede can be formed by using the additive for texturing, the light trapping effect of the silicon wafer is improved, and the lower reflectivity is obtained.
Example 2
1) Preparing an additive: taking 1L of deionized water as a solvent, sequentially adding 15g of quercetin rhamnosyl, 2g of gallic acid, 0.04g of potassium lauryl phosphate, 0.3g of sodium carbonate, 0.1g of sodium thiosulfate and 0.4g of malic acid, and fully stirring and uniformly mixing the above substances; 2) preparing a texturing solution: adding 750g of sodium hydroxide into 50L of deionized water, adding 250ml of additive, and fully and uniformly stirring to obtain alkaline texturing solution; 3) preparing a silicon wafer cleaning solution: adding 125g of sodium hydroxide into 50L of deionized water, fully dissolving and uniformly stirring to prepare a silicon wafer cleaning solution; 4) preparing a hydrogen peroxide precleaning liquid: adding 500ml of 30% hydrogen peroxide into 50L of deionized water, adding 100g of alkali, and uniformly stirring to obtain hydrogen peroxide pre-cleaning liquid; 5) preparing a mixed acid solution: HF and HCl in a molar ratio of 1: 2, preparing mixed acid with the concentration of 1.5 moL/L; 6) putting a silicon wafer into silicon wafer cleaning liquid for weak rough polishing, wherein the corrosion weight is reduced by 0.04g, putting the roughly polished wafer into a hydrogen peroxide pre-cleaning tank for cleaning for 120s, then cleaning for 120s with pure water, putting the cleaned wafer into a texturing liquid for reaction for 350s, and the texturing temperature is 76 ℃; 7) putting the textured sheet into a mixed acid solution for 120s, and then cleaning the textured sheet for 120s by using deionized water; 8) and after being cleaned by deionized water, the silicon wafer is dipped in the deionized water at 60 ℃ and slowly pulled out, and the silicon wafer is dried in a drying oven at 70 ℃ for 30 min. Observing the surface of the silicon wafer prepared in this example, the surface of the silicon wafer after the weak rough polishing is still flat, as shown in fig. 2.
Example 3
1) Preparing an additive: taking 1L of deionized water as a solvent, sequentially adding 15g of dehydrodibastic glucoside, 4g of syringic acid, 0.04g of potassium polyoxyethylene ether phosphate, 0.5g of sodium citrate, 0.2g of sodium sulfite and 0.8g of oxalic acid, and fully stirring and uniformly mixing the above substances; 2) preparing a texturing solution: adding 500g of sodium hydroxide into 50L of deionized water, adding 250ml of additive, and fully and uniformly stirring to obtain alkaline texturing solution; 3) preparing a silicon wafer cleaning solution: adding 150g of sodium hydroxide into 50L of deionized water, fully dissolving and uniformly stirring to prepare a silicon wafer cleaning solution; 4) preparing a hydrogen peroxide precleaning liquid: adding 500ml of 30% hydrogen peroxide into 50L of deionized water, adding 100g of alkali, and uniformly stirring to obtain hydrogen peroxide pre-cleaning liquid; 5) preparing a mixed acid solution: HF and HCl in a molar ratio of 1: 2, preparing mixed acid with the concentration of 1.5 moL/L; 6) putting a silicon wafer into silicon wafer cleaning liquid for weak rough polishing, wherein the corrosion weight is reduced by 0.05g, putting the roughly polished wafer into a hydrogen peroxide pre-cleaning tank for cleaning for 120s, then cleaning for 120s with pure water, putting the cleaned wafer into a texturing liquid for reaction for 300s, and the texturing temperature is 78 ℃; 7) putting the textured sheet into a mixed acid solution for 120s, and then cleaning the textured sheet for 120s by using deionized water; 8) and after being cleaned by deionized water, the silicon wafer is dipped in the deionized water at 60 ℃ and slowly pulled out, and the silicon wafer is dried in a drying oven at 70 ℃ for 30 min. Observing the surface of the silicon wafer prepared in this example, the surface of the silicon wafer after the weak rough polishing is still flat, as shown in fig. 3.
Comparative example
1) Preparing an additive: taking 1L of deionized water as a solvent, sequentially adding 15g of dehydrodibastic glucoside, 4g of syringic acid, 0.04g of potassium polyoxyethylene ether phosphate, 0.5g of sodium citrate, 0.2g of sodium sulfite and 0.8g of oxalic acid, and fully stirring and uniformly mixing the above substances; 2) preparing a texturing solution: adding 500g of sodium hydroxide into 50L of deionized water, adding 250ml of additive, and fully and uniformly stirring to obtain alkaline texturing solution; 3) preparing a silicon wafer cleaning solution: adding 150g of sodium hydroxide into 50L of deionized water, fully dissolving and uniformly stirring to prepare a silicon wafer cleaning solution; 4) preparing a hydrogen peroxide precleaning liquid: adding 500ml of 30% hydrogen peroxide into 50L of deionized water, adding 100g of alkali, and uniformly stirring to obtain hydrogen peroxide pre-cleaning liquid; 5) preparing a mixed acid solution: HF and HCl in a molar ratio of 1: 2, preparing mixed acid with the concentration of 1.5 moL/L; 6) directly putting the slices into a hydrogen peroxide pre-cleaning tank to be cleaned for 120s without weak rough polishing, then cleaning the slices with pure water for 120s, putting the cleaned slices into a wool making solution to react for 300s, wherein the wool making temperature is 78 ℃; 7) putting the textured sheet into a mixed acid solution for 120s, and then cleaning the textured sheet for 120s by using deionized water; 8) and after being cleaned by deionized water, the silicon wafer is dipped in the deionized water at 60 ℃ and slowly pulled out, and the silicon wafer is dried in a drying oven at 70 ℃ for 30 min. Observing the surface of the crystal silicon wafer prepared by the comparative example, the surface of the crystal silicon wafer is uneven and flat, the suede is small, and the diamond wire mark is serious, as shown in figure 4.
The emissivity of the silicon wafers treated in examples 1, 2 and 3 was measured, and the results are shown in the following table. As can be seen from the emissivity test result, after the texturing additive for the weak rough polishing texturing process and the using method are used, the emissivity of the silicon wafer can be obviously reduced.
| Group of | Reflectivity of light |
| Example 1 | 9.5％ |
| Example 2 | 9.4％ |
| Example 3 | 9.6％ |
| Comparative example | 10.20 |
It should be noted that the technical features related to the present patent application, such as texture making, should be regarded as the prior art, and the specific structure, operation principle, control mode and spatial arrangement mode of the technical features may be selected conventionally in the field, and should not be regarded as the invention point of the present patent, and the present patent is not further specifically described in detail.
Having described preferred embodiments of the present invention in detail, it is to be understood that modifications and variations may be resorted to without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The monocrystalline silicon texturing additive for the weak rough polishing process is characterized by comprising a defoaming agent, an auxiliary nucleating agent, a surfactant, a pH regulator, a complexing agent, organic acid and deionized water.
2. The monocrystalline silicon texturing additive for the weak rough polishing process as claimed in claim 1, wherein the monocrystalline silicon texturing additive comprises the following components in percentage by weight:
3. the monocrystalline silicon texturing additive for the light rough polishing process according to claim 2, wherein the defoaming agent is any one or more of dehydrodiconiferyl alcohol glucoside, isolarch resin glucoside, hyperoside, quercetin arabinoside, quercetin rhamnosyl, isorhamnetin galactoside, icariin, phenethyl rutinoside and phenethyl glucoside.
4. The monocrystalline silicon texturing additive for the soft rough polishing process according to claim 2, wherein the auxiliary nucleating agent is any one or more of gallic acid, caffeic acid, chlorogenic acid, vanillic acid, protocatechuic acid, syringic acid and ferulic acid.
5. The additive for texturing single crystal silicon used in a soft rough polishing process according to claim 2, wherein the surfactant is any one or more of a potassium dodecyl sulfate ester, a potassium polyoxyethylene ether phosphate ester, a potassium fatty alcohol phosphate ester, a potassium isomeric decyl alcohol phosphate ester, a potassium phenolic ether phosphate ester, a potassium isomeric tridecyl alcohol phosphate ester, a potassium lauryl phosphate ester and a potassium cetyl alcohol phosphate ester.
6. The additive for texturing monocrystalline silicon for use in a soft rough polishing process according to claim 2, wherein the pH regulator is any one or more of sodium carbonate, sodium bicarbonate, sodium citrate, sodium acetate, sodium lactate and sodium formate.
7. The monocrystalline silicon texturing additive for the rough polishing process according to claim 2, wherein the complexing agent is any one or more of sodium pyrophosphate, thiosulfate, sulfite, sodium ethoxide and ethylenediamine tetraacetic acid.
8. The monocrystalline silicon texturing additive for the weak rough polishing process according to claim 2, wherein the organic acid is any one or more of tartaric acid, oxalic acid, malic acid, benzoic acid and salicylic acid.
9. Use of a monocrystalline silicon texturing additive for a soft rough polishing process according to any one of claims 3 to 8, characterized in that it comprises the following steps:
step 1), preparing a texturing additive: mixing the defoaming agent, the auxiliary nucleating agent, the surfactant, the pH regulator, the complexing agent, the organic acid and the deionized water according to the weight percentage to prepare the monocrystalline silicon texturing additive;
step 2), preparing alkali liquor: weighing a certain mass of alkali, adding the alkali into deionized water to prepare an alkali solution with the concentration of 0.50-2.00 wt%, wherein the alkali is sodium hydroxide or potassium hydroxide;
step 3), preparing a texturing solution: adding the texturing additive prepared in the step 1) into the alkali solution prepared in the step 2), and stirring and circulating to obtain a monocrystalline silicon texturing solution;
step 4), silicon wafer cleaning: preparing 0.05-0.70 wt% of alkali liquor, placing the silicon wafer into the alkali liquor for weak rough polishing, cleaning the silicon wafer with alkali-containing hydrogen peroxide water after the weak rough polishing, and then washing with water to prepare the silicon wafer for removing the damaged layer and dirt, wherein the alkali liquor in the step 4 is 0.05-0.70 wt% of potassium hydroxide or sodium hydroxide, and the alkali-containing hydrogen peroxide is a mixed solution of 1-5 wt% of hydrogen peroxide water and 0.2-0.5 wt% of potassium hydroxide or sodium hydroxide;
step 5), texturing: immersing the silicon wafer after the weak rough polishing into monocrystalline silicon texturing solution suitable for the weak rough polishing process for texturing, and etching the surface of the silicon wafer to form a pyramid textured surface;
step 6), soaking the textured monocrystalline silicon wafer in the step 5) in deionized water at room temperature for cleaning for 2min, and then performing mixed acid cleaning for 5-10min, wherein the mixed acid liquid in the step 6) is HF/HCL, and the concentration of the mixed acid is 1-4 mol/L;
and 7), immersing the monocrystalline silicon wafer after acid washing in deionized water for washing for 2min, then immersing in the deionized water at 60 ℃ for slowly pulling out, and drying the monocrystalline silicon wafer in a drying box at 80 ℃ for 30 min.
10. The method of using the monocrystalline silicon texturing additive for the soft rough polishing process as claimed in claim 9, wherein the silicon wafer cleaning temperature is 60-75 ℃; the silicon wafer cleaning time is 100-150 s; the temperature of the wool making liquid is 75-85 ℃; the texturing time is 300-500 s.
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