CN114361290B - Additive for removing poly-Si winding plating made of TOPCon battery and cleaning process thereof - Google Patents
Additive for removing poly-Si winding plating made of TOPCon battery and cleaning process thereof Download PDFInfo
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Abstract
The invention discloses an additive for removing poly-Si plating around TOPCon battery and a cleaning process thereof, which mainly comprises the following components in percentage by weight: 0.01 to 1.0 percent of composite surfactant; 0.5 to 2.0 percent of defoaming agent; 0.3 to 1.0 percent of complexing agent; 0.01 to 1.0 percent of front protective agent; 0.5 to 1.0 percent of reaction promoter; the balance being deionized water. The additive is used for removing the winding plating in an alkali system, the corrosion of monocrystalline silicon in alkali liquor has the characteristic of anisotropy, and the anisotropy can be further amplified under the action of the additive, so that the cleaning of the whole winding plating layer can be completed under the condition of not damaging the normal suede of the middle of a silicon wafer.
Description
Technical Field
The invention relates to the technical field of monocrystalline silicon battery piece manufacturing, in particular to an additive for removing poly-Si winding plating made of TOPCon batteries and a cleaning process thereof.
Background
Solar photovoltaic power generation technology is increasingly favored by the international energy industry due to its advantages of high efficiency, cleanliness, inexhaustibility, etc. The improvement of the photoelectric conversion efficiency of the solar cell and the reduction of the production and manufacturing cost in the development process of the solar cell are two permanent subjects facing the solar cell, and the most widely applied solar cell in the industry at present is a passivated emitter back contact solar cell (PERC) mainly using p-type monocrystalline silicon as a substrate in a traditional crystalline silicon cell, but the conversion efficiency is difficult to be improved to more than 23% due to the limitation of the quality of p-type silicon materials and the structural design of devices. Therefore, it is of great significance to develop more efficient batteries.
A high-efficiency crystalline silicon solar cell, namely a Tunnel Oxide Passivated Contact solar cell (TOPCon), has been developed rapidly in recent years. The battery is characterized in that the high-efficiency passivation and the selective collection of current carriers on the whole back of the battery are realized by adopting the high-quality ultrathin silicon oxide and the doped polycrystalline silicon layer, a silicon/metal contact interface is avoided, the open-circuit voltage is favorably improved, and the filling factor is favorably improved by collecting the current carriers in the whole area. In addition, the cell adopts a high-quality n-type monocrystalline silicon wafer as a substrate, and the light-induced attenuation effect of a p-type silicon wafer is avoided, so that a high-efficiency solar cell can be obtained. However, in the process of depositing the polysilicon on the back surface of the cell, a parasitic polysilicon winding coating (winding coating for short) is easily caused at the edge of the front surface of the silicon wafer, and the existence of the winding coating not only affects the appearance of the cell, but also affects the absorption of the front surface of the cell to light, thereby affecting the photoelectric conversion efficiency of the cell.
At present, HF and HNO are mainly used in the industrial production process3The mixed solution is removed by winding plating, because the poly-Si layer of the winding plating is not uniform on the whole front surface, namely the middle is thin and the edge is thick, and the crystalline silicon is isotropic in the acid corrosion solution, when the edge winding plating layer is completely cleaned, the middle thin winding plating layer is over-etched, so that the normal suede is damaged, and the final photoelectric conversion efficiency of the cell is influenced. In addition, the mixed acid cleaning is carried out on a chain type machine, the capacity is small, the post-treatment cost of the acid is high, and the requirements of reducing cost and improving efficiency of a production line are not met. Therefore, the poly-Si winding plating layer can be effectively removed on the premise of not damaging the front suede by designing the winding plating removing additive and adopting a tank type alkali liquor cleaning process.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide an additive for removing poly-Si winding plating manufactured by TOPCon batteries and a cleaning process thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
an additive for removing a poly-Si winding coating of a Topcon battery piece mainly comprises the following components in percentage by weight:
preferably, the composite surfactant is mainly formed by combining an anionic surfactant and a gemini surfactant, or mainly formed by combining a nonionic surfactant and a gemini surfactant:
the anionic surfactant is one or a composition of more than two of alpha-olefin sodium sulfonate, fatty alcohol-polyoxyethylene ether sodium sulfate and cyclohexyl sodium sulfamate; the nonionic surfactant is one or a composition of more than two of sorbate, fatty alcohol-polyoxyethylene ether and octylphenol-polyoxyethylene ether; the gemini surfactant is anionic gemini surfactant or nonionic gemini surfactant.
Preferably, the anionic gemini surfactant is mainly one or a combination of more than two of sulfate ester salt, sulfonate, carboxylate and phosphate ester; the nonionic gemini surfactant is mainly one or a composition of more than two of lauryl alcohol polyoxyethylene ether (3) carboxylate symmetrical succinic acid diester gemini surfactants and novel biquaternary ammonium carboxymethyl sodium salt amphoteric gemini surfactants.
Preferably, the defoaming agent is one or a composition of more than two of glucan, xylan, modified starch and polyvinyl alcohol;
the complexing agent is one or more of ethylenediamine tetraacetic acid, ethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentaethylene phosphonic acid and propylenediamine tetramethylene phosphonic acid, and ammonium salt, potassium salt, sodium salt and lithium salt thereof;
the front protective agent is one or a composition of more than two of PEG-400, PEG-600, alkyl glycoside and polyacrylamide;
the reaction promoter is one or a composition of more than two of tannic acid, gallic acid, nicotinic acid and tartaric acid.
A cleaning process for removing a poly-Si winding coating of a Topcon battery piece comprises the following steps:
(1) after double-sided texturing of the silicon wafer is finished, boron doping is carried out on the front side, a tunneling oxide layer is deposited after the back side is polished, and then phosphorus doping is carried out after a layer of polycrystalline silicon grows on the tunneling oxide layer;
(2) removing the phosphorus doped layers on the front side and the side surface on the original chain type acid polishing equipment of the production line;
(3) soaking the silicon wafer with the winding coating on the front surface obtained in the step (2) in hydrofluoric acid aqueous solution, removing an oxide layer, taking out and then transferring to a water tank for cleaning;
(4) putting the silicon chip obtained in the step (3) into an alkaline tank added with the additive of the invention for cleaning, and removing the polysilicon wound and plated on the front surface;
(5) transferring the silicon wafer subjected to alkali washing in the step (4) to a water tank for rinsing, and then putting the silicon wafer with H2O2Rinsing in the tank to remove organic matters adsorbed on the surface of the silicon wafer;
(6) h in step (5)2O2Transferring the silicon wafer subjected to the bath cleaning into a water tank for rinsing, and then putting the silicon wafer into an acid tank with HF/HCl for wetting to remove metal ions on the surface of the silicon wafer;
(7) transferring the silicon wafer after acid washing in the step (6) to a water tank for rinsing, and then putting the silicon wafer with HNO3Soaking the silicon wafer in an acid tank, and oxidizing and passivating the surface of the silicon wafer;
(8) and (5) transferring the silicon wafer subjected to acid passivation in the step (7) to a water tank for cleaning, then performing slow lifting dehydration treatment, and transferring to a drying tank for drying.
Preferably, in the step (1), the boron-doped rear sheet resistance is 110-210 Ω/Sq, and the thicknesses of the tunneling oxide layer and the polysilicon layer are 110-220 nm; the sheet resistance of the silicon wafer after phosphorus doping is 15-40 omega/Sq;
in the step (2), the concentration of hydrofluoric acid in the chain type acid polishing equipment is 20-30%, the time from the single silicon wafer to the moment of just contacting the acid liquor to the moment of completely separating the silicon wafer from the acid liquor is 50-70 s, and the temperature is 20-25 ℃;
in the step (3), the concentration of hydrofluoric acid is 5-15%, the rinsing time is 90-170 s, the temperature is 20-25 ℃, and an oxidized thin layer generated in air is removed, so that subsequent alkali cleaning is facilitated.
Preferably, in the step (4), the volume ratio of the additive to the alkali liquor is 1: 15-20, the alkali liquor is 40-45% potassium hydroxide or sodium hydroxide solution, the wound coating is guaranteed to be cleaned on the premise that the front suede is not damaged, the alkali washing time is 120-200 s, and the temperature is 75-88 ℃.
Preferably, in step (5), H2O2The content of (b) is 5-8%, the H2O2Concentration 30 wt%, H2O2The cleaning time of the tank is 120-150 s, and the temperature is 55-65 ℃.
Preferably, in the step (6), the volume ratio of HF to HCl is 1: 1-3; the rinsing time is 90-180S, and the temperature is 20-25 ℃, so that metal ions on the surface of the silicon wafer are complexed.
Preferably, in step (7), HNO3The content of (a) is 4-8%, the HNO3The concentration is 30 wt%; the rinsing time is 200-350 s, and the temperature is 50-65 ℃;
in the step (8), the drying time of the drying tank is 300-500 s, and the temperature is 80-90 ℃.
The additive for removing poly-Si winding plating manufactured by TOPCon batteries and the cleaning process thereof have the advantages that the additive is used for removing winding plating cleaning in an alkali system, the corrosion of monocrystalline silicon in alkali liquor has the anisotropic characteristic, and the anisotropy can be further amplified under the action of the additive, so that the cleaning of the whole winding plating layer can be completed under the condition of not damaging the normal suede of the middle of a silicon wafer.
Drawings
FIG. 1 is an appearance diagram of example 1 before the lap plating.
FIG. 2 is an appearance diagram of example 1 after the elimination of the lap plating.
Detailed Description
The invention discloses an additive for removing poly-Si plating around made by TOPCon battery and a cleaning process thereof, and the following describes the specific implementation mode of the invention in combination with the preferred embodiment.
Example 1
1. Additive for removing poly-Si winding coating of Topcon battery piece
Taking a 5L PP measuring cup, adding 4.5L deionized water, then adding 2g of fatty alcohol-polyoxyethylene ether sodium sulfate, 1g of lauryl alcohol polyoxyethylene ether (3) carboxylate symmetric succinic acid diester gemini surfactant, 25g of polyvinyl alcohol, 20g of ethylene diamine tetramethylene phosphonic acid, 1.0g of PEG-600 and 0.8g of tartaric acid, adding deionized water to supplement the volume to 5L, stirring uniformly, and preparing the plating removal additive.
The alkali corrodes the winding plating polysilicon, so that the winding plating layer becomes loose, and hydrogen generated by alkali corrosion can be quickly separated from the surface by adding the fatty alcohol-polyoxyethylene ether sodium sulfate, so that the reaction is ensured to be continuously carried out. The lauryl alcohol polyoxyethylene ether (3) carboxylate symmetric succinic acid diester gemini surfactant has strong permeation and wetting effects, can remarkably reduce the tension of a solid-liquid interface, accelerates the mass transfer rate of a cleaning solution on a silicon wafer interface, more remarkably forms a wedge model between monocrystalline silicon and adsorption particles, desorbs the particles from the surface of a silicon wafer and wraps the particles, and forms a compact adsorption layer which is easy to clean on the surface of the silicon wafer. The complexing agent ethylenediamine tetramethylene phosphonic acid can generate complexing action on metal ions adsorbed on the surface of the silicon wafer, so that the metal ions can be more easily dispersed in the cleaning solution. The front protective agent polyvinyl alcohol and PEG-600 can be selectively adsorbed on the surface of the single crystal silicon, and the adsorption effect on the polycrystalline silicon winding coating is very weak, so that a good barrier effect is provided for the normal suede of a non-winding coating area. The addition of the reaction promoter tartaric acid accelerates the corrosion rate of the polycrystalline silicon in the alkali liquor, and can quickly remove the wound coating in a short time. In conclusion, the winding plating removing additive can assist alkali liquor to rapidly remove winding plated polycrystalline silicon, has a good protection effect on a front surface suede while removing a winding plating layer, is small in square resistance improvement amplitude, low in PN junction depth, relatively unobvious in surface concentration change of a boron doped layer, relatively large in adjustment window of a preparation process of a later battery electrode, and easy to realize production stability control.
2. Cleaning process for removing poly-Si winding coating of Topcon battery piece
(1) After double-sided texturing of the silicon wafer is completed, boron doping is carried out on the front side, a tunnel oxide layer is deposited after the back side is polished, and then phosphorus doping is carried out after a layer of polycrystalline silicon grows on the tunnel oxide layer; the boron-doped rear sheet resistance is 110-210 omega/Sq, and the thicknesses of the tunneling oxide layer and the polycrystalline silicon layer are 110-220 nm; the sheet resistance of the silicon chip after phosphorus doping is 15-40 omega/Sq;
(2) on the chain type acid polishing equipment of the original production line, the concentration of hydrofluoric acid in the chain type acid polishing equipment is 20-30%, the time from the single silicon wafer to the moment of just contacting the acid liquid to the moment of completely separating the single silicon wafer from the acid liquid is 50-70S, the temperature is 20-25 ℃, and phosphorus doped layers on the front side and the side surface are removed;
(3) soaking the silicon wafer with the winding coating on the front surface in 10 wt% hydrofluoric acid aqueous solution, controlling the temperature to be 20 ℃, circularly cleaning for 2min to remove the oxide layer on the surface of the silicon wafer, taking out the silicon wafer, and then transferring the silicon wafer to a water tank for cleaning for 2 min;
(4) putting the silicon chip obtained in the step (3) into an alkali tank with the additive of the embodiment for cleaning, controlling the temperature to be 80 ℃, circularly cleaning for 2min, and removing the polycrystalline silicon wound and plated on the front surface; wherein the additive is the prepared additive, the concentration of the sodium hydroxide solution is 45 wt%, and the volume ratio of the additive to the sodium hydroxide solution is 1: 30;
(5) transferring the silicon wafer subjected to alkali washing in the step (4) to a water tank for rinsing for 2min, and then putting H2O2Cleaning in a tank for 150s, controlling the temperature to be 65 ℃, wherein H2O2The content of (a) is 5-8%, the content of H2O2The concentration is 30 wt%;
(6) transferring the silicon wafer obtained in the step (5) to a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HF/HCl for rinsing, controlling the temperature to be 20 ℃, circularly cleaning for 2min, and removing metal ions on the surface of the silicon wafer; wherein the concentration of the HF/HCl mixed acid is 10 wt%, and the mass fraction ratio of HF to HCl is 1: 1.5;
(7) transferring the silicon wafer after acid washing in the step (6) to a water tank for rinsing for 2min, and then putting the silicon wafer with HNO3Soaking the silicon wafer in the acid tank for 300s, controlling the temperature to be 65 ℃, and oxidizing and passivating the surface of the silicon wafer; wherein, HNO3In an amount of6% of HNO3The concentration is 30 wt%;
(8) and (4) transferring the silicon wafer subjected to acid passivation in the step (7) to a water tank for cleaning for 2min, transferring to a slow pulling tank for dehydration, transferring to a drying tank for drying, and controlling the temperature of the drying tank to be 85 ℃ and the time to be 500 s.
Referring to fig. 1 to 2, fig. 1 is an appearance before removal of the spin-plating, and fig. 2 is an appearance after removal of the spin-plating.
Example 2
1. Additive for removing poly-Si winding coating of Topcon battery piece
Taking a 5L PP measuring cup, adding 4.5L deionized water, then adding 2.5g of fatty alcohol-polyoxyethylene ether sodium sulfate, 1.2g of novel amphoteric gemini surfactant of bis-quaternary ammonium carboxymethyl sodium salt, 28g of polyvinyl alcohol, 22g of ethylenediamine tetramethylene phosphonic acid, 1.0g of PEG-400 and 1.0g of gallic acid, adding deionized water to supplement to 5L, stirring uniformly, and preparing the plating removal additive.
The alkali corrodes the winding plating polysilicon, so that the winding plating layer becomes loose, and hydrogen generated by alkali corrosion can be quickly separated from the surface by adding the fatty alcohol-polyoxyethylene ether sodium sulfate, so that the reaction is ensured to be continuously carried out. The novel amphoteric gemini surfactant of the bis-quaternary ammonium carboxymethyl sodium salt has strong permeation and wetting effects, can remarkably reduce the tension of a solid-liquid interface, accelerates the mass transfer rate of a cleaning solution on a silicon wafer interface, more remarkably forms a wedge model between monocrystalline silicon and adsorption particles, desorbs the particles from the surface of the silicon wafer and wraps the particles, and forms a compact adsorption layer which is easy to clean on the surface of the silicon wafer. The complexing agent ethylenediamine tetramethylene phosphonic acid can generate complexing action on metal ions adsorbed on the surface of the silicon wafer, so that the metal ions can be more easily dispersed in the cleaning solution. The front protective agent polyvinyl alcohol and PEG-400 can be selectively adsorbed on the surface of the monocrystalline silicon, and the adsorption effect on the polycrystalline silicon winding plating layer is very weak, so that a good barrier effect is provided for the normal suede of a non-winding plating area. The addition of the reaction accelerator gallic acid accelerates the corrosion rate of the polycrystalline silicon in the alkali liquor, and can quickly remove the surrounding coating in a short time. In conclusion, the winding plating removing additive can assist alkali liquor to rapidly remove winding-plated polycrystalline silicon, has a good protection effect on a front matte surface while removing a winding plating layer, is small in square resistance improvement amplitude, low in PN junction depth, relatively unobvious in surface concentration change of a boron doped layer, relatively large in preparation process adjustment window of a later-stage battery electrode, and is easy to realize production stability control.
2. Cleaning process for removing poly-Si winding coating of Topcon battery piece
(1) After double-sided texturing of the silicon wafer is completed, boron doping is carried out on the front side, a tunnel oxide layer is deposited after the back side is polished, and then phosphorus doping is carried out after a layer of polycrystalline silicon grows on the tunnel oxide layer; the boron-doped rear sheet resistance is 110-210 omega/Sq, and the thicknesses of the tunneling oxide layer and the polycrystalline silicon layer are 110-220 nm; the sheet resistance of the silicon wafer after phosphorus doping is 15-40 omega/Sq;
(2) on the original production line chain type acid polishing equipment, the concentration of hydrofluoric acid in the chain type acid polishing equipment is 20-30%, the time from the single silicon wafer to the moment of being in contact with the acid liquid to the moment of being completely separated from the acid liquid is 50-70S, the temperature is 20-25 ℃, and phosphorus doped layers on the front side and the side surface are removed;
(3) soaking the silicon wafer with the winding coating on the front surface in 10 wt% hydrofluoric acid water solution, controlling the temperature at 20 ℃, circularly cleaning for 2min to remove an oxide layer on the surface of the silicon wafer, taking out the silicon wafer, and then transferring the silicon wafer to a water tank for cleaning for 2 min;
(4) putting the silicon chip obtained in the step (3) into an alkali tank with the additive of the embodiment for cleaning, controlling the temperature to be 80 ℃, circularly cleaning for 2min, and removing the polysilicon wound and plated on the front surface; wherein the additive is the prepared additive, the concentration of the sodium hydroxide solution is 45 wt%, and the volume ratio of the additive to the sodium hydroxide solution is 1: 30;
(5) transferring the silicon wafer subjected to alkali washing in the step (4) to a water tank for rinsing for 2min, and then putting H2O2Cleaning in a tank for 150s, controlling the temperature to be 65 ℃, wherein H2O2The content of (b) is 5-8%, the H2O2The concentration is 30 wt%;
(6) transferring the silicon wafer obtained in the step (5) to a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HF/HCl for rinsing, controlling the temperature to be 20 ℃, circularly cleaning for 2min, and removing metal ions on the surface of the silicon wafer; wherein the concentration of the HF/HCl mixed acid is 10 wt%, and the mass fraction ratio of HF to HCl is 1: 1.5;
(7) transferring the silicon wafer after acid washing in the step (6) to a water tank for rinsing for 2min, and then putting the silicon wafer with HNO3Soaking the silicon wafer in the acid tank for 300s, controlling the temperature to be 65 ℃, and oxidizing and passivating the surface of the silicon wafer; wherein, HNO3The content of (A) is 6%, the HNO3The concentration is 30 wt%;
(8) transferring the silicon wafer subjected to acid passivation in the step (7) into a water tank for cleaning for 2min, transferring the silicon wafer into a slow pulling tank for dehydration, transferring the silicon wafer into a drying tank for drying, and controlling the temperature of the drying tank to be 85 ℃ and the time to be 500 s;
(9) and (4) carrying out a sheet resistance test on the silicon wafer obtained after cleaning, and comparing the sheet resistance value with the sheet resistance value of the winding plating sheet before cleaning to calculate the sheet resistance value.
Through detection, the sheet resistance difference values of the battery cells before and after being cleaned by the additive provided by the embodiment are as follows:
TABLE 1 difference in sheet resistance before and after decoating additive cleaning
Example 3
1. Additive for removing poly-Si winding coating of Topcon battery piece
Taking a 5L PP measuring cup, adding 4.5L deionized water, then adding 1.8g of alpha-olefin sodium sulfonate, 1.2g of novel amphoteric gemini surfactant of bis-quaternary ammonium carboxymethyl sodium salt, 25g of modified starch, 22g of ethylene diamine tetramethylene phosphonic acid, 1.0g of PEG-400 and 1.0g of gallic acid, adding deionized water to supplement the volume to 5L, stirring uniformly, and preparing the plating removal additive.
The alkali corrodes the winding plating layer of the polysilicon to enable the winding plating layer to become loose, and the addition of the alpha-olefin sodium sulfonate can quickly separate hydrogen generated by the alkali corrosion from the surface, so that the reaction is ensured to be continuously carried out. The novel amphoteric gemini surfactant of the bis-quaternary ammonium carboxymethyl sodium salt has strong permeation and wetting effects, can remarkably reduce the tension of a solid-liquid interface, accelerates the mass transfer rate of a cleaning solution on a silicon wafer interface, more remarkably forms a wedge model between monocrystalline silicon and adsorption particles, desorbs the particles from the surface of the silicon wafer and wraps the particles, and forms a compact adsorption layer which is easy to clean on the surface of the silicon wafer. The complexing agent ethylenediamine tetramethylene phosphonic acid can generate complexing action on metal ions adsorbed on the surface of the silicon wafer, so that the metal ions can be more easily dispersed in the cleaning solution. The front-side protective agent modified starch and PEG-400 can be selectively adsorbed on the surface of the single crystal silicon, and the adsorption effect on the polycrystalline silicon winding coating is very weak, so that a good barrier effect is provided for the normal suede of a non-winding coating area. The addition of the reaction accelerator gallic acid accelerates the corrosion rate of the polycrystalline silicon in the alkali liquor, and can quickly remove the wound coating in a short time. In conclusion, the winding plating removing additive can assist alkali liquor to rapidly remove winding plated polycrystalline silicon, has a good protection effect on a front surface suede while removing a winding plating layer, is small in square resistance improvement amplitude, low in PN junction depth, relatively unobvious in surface concentration change of a boron doped layer, relatively large in adjustment window of a preparation process of a later battery electrode, and easy to realize production stability control.
2. Cleaning process for removing poly-Si winding coating of Topcon battery piece
(1) After double-sided texturing of the silicon wafer is completed, boron doping is carried out on the front side, a tunnel oxide layer is deposited after the back side is polished, and then phosphorus doping is carried out after a layer of polycrystalline silicon grows on the tunnel oxide layer; the boron-doped rear sheet resistance is 110-210 omega/Sq, and the thicknesses of the tunneling oxide layer and the polycrystalline silicon layer are 110-220 nm; the sheet resistance of the silicon wafer after phosphorus doping is 15-40 omega/Sq;
(2) on the chain type acid polishing equipment of the original production line, the concentration of hydrofluoric acid in the chain type acid polishing equipment is 20-30%, the time from the single silicon wafer to the moment of just contacting the acid liquid to the moment of completely separating the single silicon wafer from the acid liquid is 50-70S, the temperature is 20-25 ℃, and phosphorus doped layers on the front side and the side surface are removed;
(3) soaking the silicon wafer with the winding coating on the front surface in 10 wt% hydrofluoric acid water solution, controlling the temperature at 20 ℃, circularly cleaning for 2min to remove an oxide layer on the surface of the silicon wafer, taking out the silicon wafer, and then transferring the silicon wafer to a water tank for cleaning for 2 min;
(4) putting the silicon chip obtained in the step (3) into an alkali tank with the additive of the embodiment for cleaning, controlling the temperature to be 80 ℃, circularly cleaning for 2min, and removing the polysilicon wound and plated on the front surface; wherein the additive is the prepared additive, the concentration of the sodium hydroxide solution is 45 wt%, and the volume ratio of the additive to the sodium hydroxide solution is 1: 30;
(5) transferring the silicon wafer subjected to alkali washing in the step (4) to a water tank for rinsing for 2min, and then putting the silicon wafer into an H2O2 tank for cleaning for 150s, wherein the temperature is controlled to be 65 ℃, the content of H2O2 is 5-8%, and the concentration of H2O2 is 30 wt%;
(6) transferring the silicon wafer obtained in the step (5) to a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HF/HCl for rinsing, controlling the temperature to be 20 ℃, circularly cleaning for 2min, and removing metal ions on the surface of the silicon wafer; wherein the concentration of the HF/HCl mixed acid is 10 wt%, and the mass fraction ratio of HF to HCl is 1: 1.5;
(7) transferring the silicon wafer after acid washing in the step (6) to a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HNO3 for soaking for 300s, controlling the temperature to be 65 ℃, and carrying out oxidation passivation on the surface of the silicon wafer; wherein, the content of HNO3 is 6 percent, and the concentration of HNO3 is 30 weight percent;
(8) transferring the silicon wafer subjected to acid passivation in the step (7) to a water tank for cleaning for 2min, transferring to a slow pulling tank for dehydration treatment, transferring to a drying tank for drying, and controlling the temperature of the drying tank to be 85 ℃ and the time to be 500 s;
(9) the silicon wafer obtained after cleaning sequentially comprises the following steps according to the production line cell manufacturing process: removing phosphorosilicate glass by wet etching → passivating Al2Ox → front SiNx → back SiNx → metallization + sintering → annealing → test sorting.
Example 4
1. Additive for removing poly-Si winding coating of Topcon battery piece
Taking a 5L PP measuring cup, adding 4.5L deionized water, then adding 1.8g of alpha-olefin sodium sulfonate, 1.2g of novel amphoteric gemini surfactant of bis-quaternary ammonium carboxymethyl sodium salt, 25g of modified starch, 22g of ethylene diamine tetramethylene phosphonic acid, 1.0g of PEG-400 and 1.0g of gallic acid, adding deionized water to supplement the volume to 5L, stirring uniformly, and preparing the plating removal additive.
The alkali corrodes the winding plating polysilicon to loosen the winding plating layer, and the addition of the alpha-olefin sodium sulfonate can quickly separate hydrogen generated by the alkali corrosion from the surface, so that the reaction is ensured to be continuously carried out. The novel amphoteric gemini surfactant of the bis-quaternary ammonium carboxymethyl sodium salt has strong permeation and wetting effects, can remarkably reduce solid-liquid interfacial tension, accelerates the mass transfer rate of cleaning liquid on a silicon wafer interface, more remarkably forms a wedge model between monocrystalline silicon and adsorption particles, desorbs the particles from the surface of the silicon wafer and wraps the particles, and forms a compact adsorption layer which is easy to clean on the surface of the silicon wafer. The complexing agent ethylenediamine tetramethylene phosphonic acid can generate complexing action on metal ions adsorbed on the surface of the silicon wafer, so that the metal ions can be more easily dispersed in the cleaning solution. The front-side protective agent modified starch and PEG-400 can be selectively adsorbed on the surface of the single crystal silicon, and the adsorption effect on the polycrystalline silicon winding coating is very weak, so that a good barrier effect is provided for the normal suede of a non-winding coating area. The addition of the reaction accelerator gallic acid accelerates the corrosion rate of the polycrystalline silicon in the alkali liquor, and can quickly remove the surrounding coating in a short time. In conclusion, the winding plating removing additive can assist alkali liquor to rapidly remove winding plated polycrystalline silicon, has a good protection effect on a front surface suede while removing a winding plating layer, is small in square resistance improvement amplitude, low in PN junction depth, relatively unobvious in surface concentration change of a boron doped layer, relatively large in adjustment window of a preparation process of a later battery electrode, and easy to realize production stability control.
2. Cleaning process for removing poly-Si winding coating of Topcon battery piece
(1) After double-sided texturing of the silicon wafer is completed, boron doping is carried out on the front side, a tunnel oxide layer is deposited after the back side is polished, and then phosphorus doping is carried out after a layer of polycrystalline silicon grows on the tunnel oxide layer; the boron-doped rear sheet resistance is 110-210 omega/Sq, and the thicknesses of the tunneling oxide layer and the polycrystalline silicon layer are 110-220 nm; the sheet resistance of the silicon wafer after phosphorus doping is 15-40 omega/Sq;
(2) on the original production line chain type acid polishing equipment, the concentration of hydrofluoric acid in the chain type acid polishing equipment is 20-30%, the time from the single silicon wafer to the moment of being in contact with the acid liquid to the moment of being completely separated from the acid liquid is 50-70S, the temperature is 20-25 ℃, and phosphorus doped layers on the front side and the side surface are removed;
(3) soaking the silicon wafer with the winding coating on the front surface in 10 wt% hydrofluoric acid water solution, controlling the temperature at 20 ℃, circularly cleaning for 2min to remove an oxide layer on the surface of the silicon wafer, taking out the silicon wafer, and then transferring the silicon wafer to a water tank for cleaning for 2 min;
(4) putting the silicon chip obtained in the step (3) into an alkali tank with the additive of the embodiment for cleaning, controlling the temperature to be 88 ℃, circularly cleaning for 2min, and removing the polycrystalline silicon wound and plated on the front surface; wherein the additive is the prepared additive, the concentration of the sodium hydroxide solution is 45 wt%, and the volume ratio of the additive to the sodium hydroxide solution is 1: 30;
(5) transferring the silicon wafer subjected to alkali washing in the step (4) into a water tank for rinsing for 2min, then putting the silicon wafer into an H2O2 tank for cleaning for 150s, and controlling the temperature to be 65 ℃, wherein the content of H2O2 is 5-8%, and the concentration of H2O2 is 30 wt%;
(6) transferring the silicon wafer obtained in the step (5) into a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HF/HCl for rinsing, controlling the temperature to be 20 ℃, circularly cleaning for 2min, and removing metal ions on the surface of the silicon wafer; wherein the concentration of the HF/HCl mixed acid is 10 wt%, and the mass fraction ratio of HF to HCl is 1: 1.5;
(7) transferring the silicon wafer after acid washing in the step (6) into a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HNO3 for soaking for 300s, controlling the temperature to be 65 ℃, and carrying out oxidation passivation on the surface of the silicon wafer; wherein, the content of HNO3 is 6 percent, and the concentration of HNO3 is 30 weight percent;
(8) transferring the silicon wafer subjected to acid passivation in the step (7) to a water tank for cleaning for 2min, transferring to a slow pulling tank for dehydration treatment, transferring to a drying tank for drying, and controlling the temperature of the drying tank to be 85 ℃ and the time to be 500 s;
(9) the silicon wafer obtained after cleaning sequentially comprises the following steps according to the production line cell manufacturing process: removing phosphorosilicate glass by wet etching → passivating Al2Ox → front SiNx → back SiNx → metallization + sintering → annealing → test sorting.
Example 5
1. Additive for removing poly-Si winding coating of Topcon battery piece
Taking a 5L PP measuring cup, adding 4.5L deionized water, then adding 1.8g of alpha-olefin sodium sulfonate, 1.2g of novel amphoteric gemini surfactant of bis-quaternary ammonium carboxymethyl sodium salt, 25g of modified starch, 22g of ethylene diamine tetramethylene phosphonic acid, 1.0g of PEG-400 and 1.0g of gallic acid, adding deionized water to supplement to 5L, stirring uniformly, and preparing the plating removal additive.
The winding plating layer becomes loose due to corrosion of alkali on the winding plating layer, and hydrogen generated by alkali corrosion can be quickly separated from the surface due to the addition of the sodium alpha-olefin sulfonate serving as the defoaming agent, so that the reaction is ensured to be continuously carried out. The novel amphoteric gemini surfactant of the bis-quaternary ammonium carboxymethyl sodium salt has strong permeation and wetting effects, can remarkably reduce solid-liquid interfacial tension, accelerates the mass transfer rate of cleaning liquid on a silicon wafer interface, more remarkably forms a wedge model between monocrystalline silicon and adsorption particles, desorbs the particles from the surface of the silicon wafer and wraps the particles, and forms a compact adsorption layer which is easy to clean on the surface of the silicon wafer. The complexing agent ethylenediamine tetramethylene phosphonic acid can generate complexing action on metal ions adsorbed on the surface of the silicon wafer, so that the metal ions can be more easily dispersed in the cleaning solution. The front-side protective agent modified starch and PEG-400 can be selectively adsorbed on the surface of the monocrystalline silicon, but the adsorption effect on the polycrystalline silicon winding plating layer is very weak, so that a good barrier effect is provided for the normal suede of a non-winding plating area. The addition of the reaction accelerator gallic acid accelerates the corrosion rate of the polycrystalline silicon in the alkali liquor, and can quickly remove the surrounding coating in a short time. In conclusion, the winding plating removing additive can assist alkali liquor to rapidly remove winding plated polycrystalline silicon, has a good protection effect on a front surface suede while removing a winding plating layer, is small in square resistance improvement amplitude, low in PN junction depth, relatively unobvious in surface concentration change of a boron doped layer, relatively large in adjustment window of a preparation process of a later battery electrode, and easy to realize production stability control.
2. Cleaning process for removing poly-Si winding coating of Topcon battery piece
(1) After double-sided texturing of the silicon wafer is completed, boron doping is carried out on the front side, a tunnel oxide layer is deposited after the back side is polished, and then phosphorus doping is carried out after a layer of polycrystalline silicon grows on the tunnel oxide layer; the boron-doped rear sheet resistance is 110-210 omega/Sq, and the thicknesses of the tunneling oxide layer and the polycrystalline silicon layer are 110-220 nm; the sheet resistance of the silicon chip after phosphorus doping is 15-40 omega/Sq;
(2) on the original production line chain type acid polishing equipment, the concentration of hydrofluoric acid in the chain type acid polishing equipment is 20-30%, the time from the single silicon wafer to the moment of being in contact with the acid liquid to the moment of being completely separated from the acid liquid is 50-70S, the temperature is 20-25 ℃, and phosphorus doped layers on the front side and the side surface are removed;
(3) soaking the silicon wafer with the winding coating on the front surface in 10 wt% hydrofluoric acid water solution, controlling the temperature at 20 ℃, circularly cleaning for 2min to remove an oxide layer on the surface of the silicon wafer, taking out the silicon wafer, and then transferring the silicon wafer to a water tank for cleaning for 2 min;
(4) putting the silicon chip obtained in the step (3) into an alkali tank with the additive of the embodiment for cleaning, controlling the temperature to be 88 ℃, circularly cleaning for 3min, and removing the polysilicon wound and plated on the front surface; wherein the additive is the prepared additive, the concentration of the sodium hydroxide solution is 45 wt%, and the volume ratio of the additive to the sodium hydroxide solution is 1: 30;
(5) transferring the silicon wafer subjected to alkali washing in the step (4) to a water tank for rinsing for 2min, and then putting the silicon wafer into an H2O2 tank for cleaning for 150s, wherein the temperature is controlled to be 65 ℃, the content of H2O2 is 5-8%, and the concentration of H2O2 is 30 wt%;
(6) transferring the silicon wafer obtained in the step (5) to a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HF/HCl for rinsing, controlling the temperature to be 20 ℃, circularly cleaning for 2min, and removing metal ions on the surface of the silicon wafer; wherein the concentration of the HF/HCl mixed acid is 10 wt%, and the mass fraction ratio of HF to HCl is 1: 1.5;
(7) transferring the silicon wafer after acid washing in the step (6) to a water tank for rinsing for 2min, then putting the silicon wafer into an acid tank with HNO3 for soaking for 300s, controlling the temperature to be 65 ℃, and carrying out oxidation passivation on the surface of the silicon wafer; wherein, the content of HNO3 is 6 percent, and the concentration of HNO3 is 30 weight percent;
(8) transferring the silicon wafer subjected to acid passivation in the step (7) into a water tank for cleaning for 2min, transferring the silicon wafer into a slow pulling tank for dehydration, transferring the silicon wafer into a drying tank for drying, and controlling the temperature of the drying tank to be 85 ℃ and the time to be 500 s;
(9) the silicon wafer obtained after cleaning sequentially comprises the following steps according to the production line cell manufacturing flow: wet etching to remove phosphorosilicate glass → passivated Al2Ox → front SiNx → back SiNx → metallization + sintering → annealing → test sorting.
The measured values of the photoelectric conversion efficiency of the single crystal silicon processed in the above examples 1, 2, 3, 4 and 5 are as follows:
TABLE 2 comparison of values of photoelectric conversion efficiencies of single-crystal silicon after dechlorination in examples 1 to 5
| Examples of the invention | Counting | Eta | Uoc | Isc | FF | Rsh | Rs | IRev2 |
| Example 1 | 5 ten thousand | 23.001 | 0.6841 | 11.329 | 81.35 | 569 | 0.0022 | 0.084 |
| Example 2 | 5 ten thousand | 23.024 | 0.6842 | 11.340 | 81.37 | 619 | 0.0022 | 0.074 |
| Example 3 | 5 ten thousand | 23.060 | 0.6844 | 11.392 | 81.07 | 873 | 0.0018 | 0.046 |
| Example 4 | 5 ten thousand | 23.067 | 0.6916 | 11.373 | 80.39 | 377 | 0.0020 | 0.047 |
| Example 5 | 5 ten thousand | 23.081 | 0.6908 | 11.377 | 80.52 | 378 | 0.0013 | 0.003 |
It should be noted that the above mentioned embodiments are only preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art should be covered by the protection scope of the present invention by making insubstantial changes to the present invention using this idea. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. The additive for removing the poly-Si winding coating of the Topcon battery piece is characterized by mainly comprising the following components in percentage by weight:
the composite surfactant is mainly formed by combining an anionic surfactant and a gemini surfactant, or mainly formed by combining a nonionic surfactant and a gemini surfactant:
the anionic surfactant is one or a composition of more than two of alpha-olefin sodium sulfonate, fatty alcohol polyoxyethylene ether sodium sulfate and cyclohexyl sodium sulfamate; the nonionic surfactant is one or a composition of more than two of sorbate, fatty alcohol-polyoxyethylene ether and octylphenol-polyoxyethylene ether; the gemini surfactant is an anionic gemini surfactant or a nonionic gemini surfactant.
2. The additive for removing poly-Si wraparound coating of a Topcon battery piece according to claim 1, wherein the anionic gemini surfactant is mainly one or a composition of more than two of sulfate ester salt, sulfonate ester, carboxylate and phosphate ester; the nonionic gemini surfactant is mainly one or a composition of more than two of lauryl alcohol polyoxyethylene ether (3) carboxylate symmetrical succinic acid diester gemini surfactants and novel biquaternary ammonium carboxymethyl sodium salt amphoteric gemini surfactants.
3. The additive for removing the poly-Si wraparound coating of the Topcon battery piece according to claim 1, wherein: the defoaming agent is one or a composition of more than two of glucan, xylan, modified starch and polyvinyl alcohol;
the complexing agent is one or more of ethylenediamine tetraacetic acid, ethylenediamine tetramethylenephosphonic acid, diethylenetriamine pentaethylenephosphonic acid and propylenediamine tetramethylenephosphonic acid, and ammonium salt, potassium salt, sodium salt and lithium salt thereof;
the front protective agent is one or a composition of more than two of PEG-400, PEG-600, alkyl glycoside and polyacrylamide;
the reaction promoter is one or more of tannic acid, gallic acid, nicotinic acid and tartaric acid.
4. A cleaning process for removing poly-Si wraparound plating of Topcon cell sheets using the additive of any of claims 1-3, comprising the steps of:
(1) after double-sided texturing of the silicon wafer is completed, boron doping is carried out on the front side, a tunnel oxide layer is deposited after the back side is polished, and then phosphorus doping is carried out after a layer of polycrystalline silicon grows on the tunnel oxide layer;
(2) removing the phosphorus doped layers on the front surface and the side surface on the original production line chain type acid polishing equipment;
(3) soaking the silicon wafer with the winding coating on the front surface obtained in the step (2) in hydrofluoric acid aqueous solution, removing an oxide layer, taking out and then transferring to a water tank for cleaning;
(4) putting the silicon chip obtained in the step (3) into an alkaline tank added with the additive of the invention for cleaning, and removing the polysilicon wound and plated on the front surface;
(5) transferring the silicon wafer subjected to alkali washing in the step (4) to a water tank for rinsing, and then putting the silicon wafer into a water tank with H2O2Rinsing in the tank to remove adsorptionOrganic matter on the surface of the silicon chip;
(6) h in the step (5)2O2Transferring the silicon wafer subjected to the bath cleaning into a water tank for rinsing, and then putting the silicon wafer into an acid tank with HF/HCl for wetting to remove metal ions on the surface of the silicon wafer;
(7) transferring the silicon wafer after acid washing in the step (6) to a water tank for rinsing, and then putting the silicon wafer with HNO3Soaking the silicon wafer in an acid tank, and oxidizing and passivating the surface of the silicon wafer;
(8) and (4) transferring the silicon wafer subjected to acid passivation in the step (7) to a water tank for cleaning, then carrying out slow lifting dehydration treatment, and transferring to a drying tank for drying.
5. The cleaning process for removing the poly-Si coil plating layer of the Topcon battery piece according to claim 4, is characterized in that: in the step (1), the sheet resistance after boron doping is 110-210 omega/Sq, and the thicknesses of the tunneling oxidation layer and the polycrystalline silicon layer are 110-220 nm; the sheet resistance of the silicon wafer after phosphorus doping is 15-40 omega/Sq;
in the step (2), the concentration of hydrofluoric acid in the chain type acid polishing equipment is 20-30%, the time from the single silicon wafer to the moment of just contacting the acid liquor to the moment of completely separating the silicon wafer from the acid liquor is 50-70 s, and the temperature is 20-25 ℃;
in the step (3), the concentration of hydrofluoric acid is 5-15%, the rinsing time is 90-170 s, the temperature is 20-25 ℃, and an oxidized thin layer generated in air is removed, so that subsequent alkali cleaning is facilitated.
6. The cleaning process for removing the poly-Si wraparound coating of the Topcon battery piece according to claim 4, wherein: in the step (4), the volume ratio of the additive to the alkali liquor is 1: 15-20, the alkali liquor is 40-45% of potassium hydroxide or sodium hydroxide solution, the winding coating is cleaned on the premise of not damaging the front suede, the alkali washing time is 120-200 s, and the temperature is 75-88 ℃.
7. The cleaning process for removing the poly-Si coil plating layer of the Topcon battery piece according to claim 4, is characterized in that: in step (5), H2O2The content of (a) is 5-8%, the content of H2O2The concentration is 30 wt%,H2O2the cleaning time of the tank is 120-150 s, and the temperature is 55-65 ℃.
8. The cleaning process for removing the poly-Si coil plating layer of the Topcon battery piece according to claim 4, is characterized in that: in the step (6), the volume ratio of HF to HCl is 1: 1-3; the rinsing time is 90-180 s, and the temperature is 20-25 ℃, so that metal ions on the surface of the silicon wafer can be complexed.
9. The cleaning process for removing the poly-Si coil plating layer of the Topcon battery piece according to claim 4, is characterized in that: in step (7), HNO3The content of (a) is 4-8%, the HNO3The concentration is 30 wt%; the rinsing time is 200-350 s, and the temperature is 50-65 ℃;
in the step (8), the drying time of the drying tank is 300-500 s, and the temperature is 80-90 ℃.
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| CN111785809A (en) * | 2020-07-15 | 2020-10-16 | 常州时创能源股份有限公司 | Method for preparing passivated contact cell |
| CN111900214A (en) * | 2020-08-13 | 2020-11-06 | 晶科能源有限公司 | Method for removing polycrystalline silicon plating, solar cell and preparation method thereof |
| CN112885925A (en) * | 2021-02-05 | 2021-06-01 | 泰州隆基乐叶光伏科技有限公司 | Solar cell and manufacturing method thereof |
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| CN111524983B (en) * | 2020-04-03 | 2021-07-27 | 常州大学 | Efficient crystalline silicon battery with double-sided selective emitter and preparation method thereof |
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| CN111785809A (en) * | 2020-07-15 | 2020-10-16 | 常州时创能源股份有限公司 | Method for preparing passivated contact cell |
| CN111900214A (en) * | 2020-08-13 | 2020-11-06 | 晶科能源有限公司 | Method for removing polycrystalline silicon plating, solar cell and preparation method thereof |
| CN112885925A (en) * | 2021-02-05 | 2021-06-01 | 泰州隆基乐叶光伏科技有限公司 | Solar cell and manufacturing method thereof |
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