CN114397796A - Electroplating-resistant photoresist for novel C-HJT battery manufacturing process - Google Patents

Electroplating-resistant photoresist for novel C-HJT battery manufacturing process Download PDF

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CN114397796A
CN114397796A CN202210025921.8A CN202210025921A CN114397796A CN 114397796 A CN114397796 A CN 114397796A CN 202210025921 A CN202210025921 A CN 202210025921A CN 114397796 A CN114397796 A CN 114397796A
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acrylate
meth
novel
resin
hjt
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万辉
黄磊
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Zhangjiagang Kesi New Photosensitive Material Co ltd
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Zhangjiagang Kesi New Photosensitive Material Co ltd
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds

Abstract

The invention discloses an electroplating-resistant photoresist for a novel C-HJT battery manufacturing process, which comprises the following raw materials in parts by weight: 10-50 parts of high molecular adhesive, 20-40 parts of photopolymerization monomer and 3-5 parts of photoinitiator, wherein the weight average molecular weight of the high molecular adhesive is more than 2000, and the number average molecular weight of the high molecular adhesive is more than 1000; the photopolymerizable monomer has an ethylenically unsaturated functional group. The electroplating-resistant photoresist disclosed by the invention has high sensitivity, high resolution and excellent developing property, and also has better electroplating-resistant performance and high production rate.

Description

Electroplating-resistant photoresist for novel C-HJT battery manufacturing process
Technical Field
The invention relates to the technical field of photovoltaic C-HJT battery manufacturing processes, in particular to electroplating-resistant photoresist for a novel C-HJT battery manufacturing process.
Background
Compared with the traditional solar cell, the HJT cell adopts a structure of a monocrystalline silicon substrate and an amorphous thin film heterojunction, and the method of depositing the amorphous silicon thin film on the crystalline silicon ensures that the HJT cell has the advantages of both the crystalline silicon and the thin film cell. The HJT battery has many characteristics such as simple structure, high stability, low process temperature, high light conversion efficiency, good temperature characteristics, double-sided power generation, etc., and the HJT battery gradually becomes an ultimate solution for future battery technologies recognized by practitioners in the battery industry.
However, the heterojunction solar cell generally adopts resin type low-temperature cured silver paste as a metal electrode, so that the resistivity is high, the conductivity is poor, and in order to improve the conductivity, the width or the height of the metal electrode needs to be increased, so that the silver paste consumption of the cell is increased. The silver consumption of the single chip is 2.62 times of that of the conventional PERC battery. With the advent of the C-HJT (copper gate heterojunction cell) process, copper gate electrodes are substituted for the traditional silver gate electrodes, thereby achieving the desire to reduce cost. However, in the conventional copper gate electrode, a dry film is used for manufacturing the gate line, and the dry film is subjected to film pressing, exposure, film tearing, development and electroplating to form the electrode gate line. The dry film cost is high, the process automation flow has low production speed, the grid line precision is low, and the industrial manufacturing requirements cannot be completely met, so that the cost is reduced by providing a photoresist to replace the dry film to carry out the C-HJT copper grid electrode manufacturing process, the production speed of the complete automation process flow reaches 6000 pieces/hour, the electrode grid line height is kept fine and reaches 15 mu m of line diameter, the occupied area of the electrode wiring on the surface of the battery is reduced, the light conversion efficiency is improved to the maximum extent, and the efficiency of the C-HJT battery is greatly improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a plating-resistant photoresist for a novel C-HJT battery manufacturing process.
In order to achieve the purpose, the invention adopts the technical scheme that: an electroplating-resistant photoresist for a novel C-HJT battery process comprises the following raw materials in parts by weight: 10-50 parts of high molecular adhesive, 20-40 parts of photopolymerization monomer and 3-5 parts of photoinitiator, wherein the weight average molecular weight of the high molecular adhesive is more than 2000, and the number average molecular weight of the high molecular adhesive is more than 1000; the photopolymerizable monomer has an ethylenically unsaturated functional group.
As a specific embodiment, the weight average molecular weight of the polymer binder is between 3000 and 50000, and the number average molecular weight is between 2000 and 40000.
As a specific embodiment, the polymer binder includes, but is not limited to, at least one of acrylic resin, styrene resin, epoxy resin, amide epoxy resin, polyimide precursor, alkyd resin, phenolic resin, urethane resin, epoxy acrylate resin obtained by reacting epoxy resin with (meth) acrylic acid, and acid-modified epoxy acrylate resin obtained by reacting epoxy acrylate resin with acid anhydride.
As a specific embodiment, the ethylenically unsaturated functional group in the photopolymerizable monomer is an acrylate group, and the photopolymerizable monomer includes, but is not limited to, 1, 4-butanediol di (meth) acrylate, 1, 6-hexanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate adipate, neopentyl glycol di (meth) hydroxypivalate, dicyclopentadienyl di (meth) acrylate, caprolactone-modified dicyclopentadienyl di (meth) acrylate, allylated cyclohexyl di (meth) acrylate, isocyanurate di (meth) acrylate, trimethylolpropane tri (meth) acrylate, trimethyltri (meth) acrylate, tris (acryloxyethyl) isocyanurate, urethane tri (meth) acrylate, and mixtures thereof, At least one of ethoxy modified trimethylolpropane triacrylate, glycerol propoxylate triacrylate, ethoxylated bisphenol A dimethacrylate and aliphatic urethane prepolymer.
As a specific embodiment, one or more of benzoin, benzoin alkyl ethers, acetophenones, anthraquinones, ketals, organic peroxides, thiol compounds, organic halides, benzophenones, thiazolones, and phenylphosphines are used as the photoinitiator.
The photoinitiator selected here is a photopolymerization initiator with an absorption wavelength of about 400nm, and preferably, the photoinitiator may be selected from benzoin and benzoin alkyl ethers such as benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether and the like; acetophenones such as acetophenone, 2-dimethoxy-2-phenylacetophenone, 2-diethoxy-2-phenylacetophenone and 1, 1-dichloroacetophenone; 2-methylmethylthio) phenyl ] -2-morpholinopropanone-1, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone, N-dimethylaminobenzone; anthraquinones such as 2-methylanthraquinone, 2-ethylanthraquinone, 2-tert-butylanthraquinone, and 1-chloroanthraquinone; thiazolones such as 2, 4-dimethylthiazolone, 2, 4-diethylthiazolone, 2-chlorothiazolone and 2, 4-diisopropylthiazolone; ketals such as acetophenone dimethyl ketal and benzyl dimethyl ketal; organic peroxides such as benzoyl peroxide and cumyl peroxide; thiol compounds such as 2,4, 5-triarylimidazole dimer, riboflavin tetrabutyl ester, 2-mercaptobenzimidazole, 2-mercaptobenzoxazole and 2-mercaptobenzothiazole; organic halides such as 2,4, 6-tris-s-triazine, 2,2, 2-tribromoethanol, tribromomethylphenyl ketone, and the like; benzophenones or thiazolones such as benzophenone and 4,4' -bisdiethylaminobenzophenone; 2,4, 6-trimethylbenzoyldiphenylphosphine oxide, and the like. The above-listed photoinitiators may be used singly or in admixture of two or more.
As a specific embodiment, the raw materials are also added with a photoinitiation auxiliary agent, and the photoinitiation auxiliary agent comprises one or more of but not limited to N, N-dimethylamino benzoic acid ethyl ester, N-dimethylamino benzoic acid isoamyl ester, amyl-4-dimethylamino benzoic acid ester, triethylamine and triethanolamine.
As a specific embodiment, the photoinitiator is a photoinitiator 907 manufactured by Qiangli New materials and DETX manufactured by chemical reagents of national drug group.
As a specific embodiment, the raw material further comprises 0.5-1 part of surfactant, and the surfactant is selected from at least one of fluorine-containing surfactant and siloxane surfactant.
The photoresist can also be added with a certain amount of auxiliary agents, such as coloring agents, surfactants, stabilizing agents, polymerization inhibitors or plasticizers and the like.
As the colorant, for example, crystal violet, victoria blue, ethyl violet, phthalocyanine blue, phthalocyanine green and the like are given.
As the surfactant, for example, a fluorine-containing surfactant, a siloxane surfactant, and the like are mentioned.
As the plasticizer, for example, diethyl phthalate, dibutyl phthalate, tributyl phosphate and the like are mentioned.
As the stabilizer, for example, phosphoric acid, phosphorous acid, oxalic acid, malic acid, benzenesulfonic acid and the like are given.
As the polymerization inhibitor, for example, p-cresol, pyrogallol, t-butylcatechol, etc. are mentioned.
As a specific embodiment, the raw material further comprises a solvent, wherein the solvent comprises but is not limited to one or more of methanol, ethanol, propanol, butanol, acetone, butanone, N-methyl-2-pyrrolidone, methyl ethyl ketone, methyl cellosolve, ethyl cellosolve, butyl cellosolve, toluene, N' -dimethylformamide, propylene glycol monomethyl ether, dimethyl sulfoxide, diethyl sulfoxide, phenol, o-cresol, m-cresol, p-cresol, xylenol, halogenated phenol, catechol, tetrahydrofuran, dioxane, dioxolane, trimethylene glycol methyl ether, tetraethylene glycol dimethyl ether, gamma-butyrolactone, hexamethyl o-amide, and propylene glycol methyl ether acetate.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the electroplating-resistant photoresist for the novel C-HJT battery manufacturing process is prepared by adopting a high-molecular adhesive, a photopolymerization monomer and a photoinitiator, has high LDI imaging sensitivity, is resistant to electroplating solution, has fine line diameter reaching 15 mu m, can be used for preparing a high-precision C-HJT battery copper grid electrode, can realize automatic industrial connection, and can reach the production rate of 6000 sheets/hour.
Detailed Description
The technical solution of the present invention is further illustrated below with reference to specific examples.
Preparation of macromolecular adhesive
1. Polymer adhesive A1
Provided is a polymer adhesive A1, which is composed of the following raw materials: 10g of methyl methacrylate, 10g of methacrylic acid, 15g of 2-hydroxyethyl methacrylate, 1g of styrene and 15g of butyl acrylate multipolymer.
The preparation method comprises the following steps:
in a 250ml three-neck flask with a condenser and a stirrer, 10g of methacrylic acid, 10g of methyl methacrylate, 15g of 2-hydroxyethyl methacrylate, 1g of styrene and 15g of butyl acrylate are added, 65gPM solvent is added for stirring and dissolving, the temperature is heated to 40 ℃, 0.5g of AIBN (azobisisobutyronitrile) is added, the temperature is continuously increased to 80 ℃, the temperature is kept for 6 hours, then 0.1g of pyrogallol is added, and the mixture is cooled to the room temperature, so that the high polymer adhesive A1 with the solid content of 40 percent is obtained.
2. Polymer adhesive A2
Provided is a polymer adhesive A2, which is composed of the following raw materials: 100g of polyamic acid prepolymer and 1.5g of diamine monomer binary copolymer.
The preparation method comprises the following steps:
in a 250ml three-necked flask equipped with a condenser and a stirrer, 0.1 mol of pyromellitic dianhydride was added and dissolved in 126g of N-methyl-2-pyrrolidone, and the mixture was heated to 50 ℃ and reacted for 2 hours while maintaining the temperature. Then slowly dripping 0.02 mol of 2-hydroxyethyl acrylic acid, keeping the temperature at 50 ℃ for reaction for 2 hours, then adding 0.09 mol of 4, 4-diaminodiphenyl ether into the reaction system, completely dissolving, and reacting at 50 ℃ for 6 hours to obtain a polyamic acid prepolymer;
diamine monomers were then prepared as follows: adding 0.1g of molar p-phenylenediamine into a toluene solvent, slowly adding 0.2g of trifluoroacetic anhydride under the stirring condition, and reacting at the temperature of 50 ℃ for 1 hour to obtain a diamine monomer;
100g of polyamic acid prepolymer (containing 25% of solid content) and 1.5g of diamine monomer were uniformly mixed to obtain a polymer adhesive A2.
Second, preparation of photoresist
Taking example 1 as an example:
300g of high polymer adhesive A1, 150g of ethoxy modified trimethylolpropane triacrylate (Photomer 4155Cognis7), 50g of trimethylolpropane triacrylate prepolymer (Em 2382; Eternal Materials), 5g of photoinitiator 907 (strong new material), 3.5g of photoinitiator DETX (national reagent), 0.5g of fluorine-based nonionic surfactant (Megafac F-780F Dainippon Ink and Chemicals. Inc.), 1g of polymerization inhibitor MEHQ, 1g of copper phthalocyanine color paste, 400g of solvent MEK and 89g of solvent PM are mixed and stirred uniformly, and then filtered by a 0.5 mu m filter to obtain the corresponding photoresist A. The other examples and comparative examples were prepared in the same manner as in example 1, and the component formulations thereof are shown in Table 1.
TABLE 1
Figure BDA0003464652540000051
Wherein:
the photopolymerizable monomer 1 was ethoxy-modified trimethylolpropane triacrylate (Photomer 4155Cognis 7; manufactured by Miwon Commercial Co., Ltd.); the photopolymerization monomer 2 is trimethylolpropane triacrylate prepolymer (Em 2382; Eternal Materials); the photoinitiator 1 is a photoinitiator 907 (powerful new material); the photoinitiator 2 is a photoinitiator DETX (Chinese medicine reagent); the fluorine-based nonionic surfactant is Megafac F-780F; manufactured by Dainippon Ink and chemicals.inc; the polymerization inhibitor is MEHQ; the solvent A is MEK; the solvent B is a solvent PM; the acid anhydride modified acrylic resin 1 is CCR4959 manufactured by Nippon Kabushiki Kaisha; the acid anhydride-modified acrylic resin 2 was 4060 manufactured by Nippon chemical Co.
The components of example 1, example 2, comparative example 1 and comparative example 2 in table 1 are mixed according to the amount, stirred uniformly and filtered by a 0.5 μm filter, and the corresponding photoresist A, B, C, D is obtained.
The photoresist was fabricated into a C-HJT cell sample A, B, C, D for performance testing as follows.
Manufacturing a battery sample wafer: the photoresist was coated on the C-HJT cell substrate with the copper seed layer by an automatic screen printing machine (Mich. technology), and the coating thickness was controlled to 15 μm. The coated cell piece is dried in an oven at 90 ℃ for 3 minutes, and the dried cell piece substrate A, B, C, D is subjected to the following performance tests respectively:
high sensitivity and developability: placing 21-grade optical gradient ruler on the substrate, exposing with LDI exposure machine (core Acer micro-packaging exposure machine) with 20mJ energy, and developing with conventional method (developing solution is 1% sodium carbonate aqueous solution, developing temperature is 30 deg.C, and spray pressure of developing solution is 1.2 kg/cm)2) Developing for one minute, cleaning the substrate with deionized water, drying with hot air, visually observing the number of the photoresist grids retained by the optical gradient ruler on the substrate, wherein seven grids indicate that the photoresist is completely cured under the energy of 20mJ, and simultaneouslyAnd judging the photoresist developability.
And (4) judging the standard: the number of the photoresist grids is reserved to be seven, which shows that the sensitivity is high; the exposed copper seed layer is clean and excellent; the copper seed layer had a slight white haze which was poor. The results are shown in Table 2.
High resolution: an LDI exposure machine (core Acer micro-packaging exposure machine) is used for making a 15 mu m opening grid line image under the energy of 20mJ, and then the image is developed, and whether the opening grid line is clear or not is observed after the image is developed.
Evaluation criteria: the opening grid line is clear and excellent; the edge of the opening is slightly burred; the open grid line is unclear as poor; the results are shown in Table 2.
Plating resistance: and horizontally electroplating the cell substrate serving as the grid line, wherein the thickness of an electroplated layer on the open grid line is 15-20 mu m, and observing whether the photoresist layer covered on the non-electroplated area is corroded by electroplating solution after electroplating.
In addition, by using the dry film in the prior art, the dry film is hot-pressed on the cell by a laminator, under the energy of 20mJ by an LDI exposure machine (a chip Acer micro-packaging exposure machine), a 15 μm opening grid line image is made, and then the C-HJT cell sample wafer E is obtained by developing and electroplating.
Evaluation criteria: the steel is kept intact and is not corroded; the corrosion was poor and the results are shown in Table 2.
TABLE 2
Figure BDA0003464652540000061
Figure BDA0003464652540000071
As can be seen from Table 2, the battery substrates A and B obtained by the present invention have high sensitivity and excellent developability, and have high resolution and good plating resistance, as compared with the battery substrates C and D. Meanwhile, compared with the battery substrate E prepared by adopting a dry film in the prior art, the battery substrate prepared by adopting the wet film has better developing property and resolution.
In addition, in Table 3, the comparison of various parameters of the C-HJT cell made of the photoresist of the present invention and the C-HJT cell made of the dry film used in the existing market is shown.
TABLE 3
Technical parameters Made of dry films Using the photoresist of the invention
Exposure energy 40-50mJ 15-20mJ
Resolution of 30-50μm 15μm
Automation rate of production line Non-producible line full automation Can be automatically connected
Birth rate 1000-2000 tablets/hour 6000 tablets/hour
From table 3, we can see that the photoresist obtained by the formulation of the present invention has high sensitivity and high resolution, and can realize full-automatic production, and the production speed is high, and can reach 6000 pieces/hour.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (9)

1. An electroplating-resistant photoresist for a novel C-HJT battery manufacturing process is characterized by comprising the following raw materials in parts by weight: 10-50 parts of high molecular adhesive, 20-40 parts of photopolymerization monomer and 3-5 parts of photoinitiator, wherein the weight average molecular weight of the high molecular adhesive is more than 2000, and the number average molecular weight of the high molecular adhesive is more than 1000; the photopolymerizable monomer has an ethylenically unsaturated functional group.
2. The plating resist photoresist for the novel C-HJT battery process as claimed in claim 1, wherein the weight average molecular weight of the polymer binder is 3000-50000 and the number average molecular weight is 2000-40000.
3. The plating resist for the manufacture of novel C-HJT battery as claimed in claim 1 or 2, wherein the polymeric binder includes but is not limited to at least one of acrylic resin, styrene resin, epoxy resin, amide epoxy resin, polyimide precursor, alkyd resin, phenolic resin, urethane resin, epoxy acrylate resin obtained by reacting epoxy resin with (meth) acrylic acid, and acid-modified epoxy acrylate resin obtained by reacting epoxy acrylate resin with acid anhydride.
4. The photoresist of claim 1, wherein the ethylenically unsaturated functional group of the photopolymerizable monomers comprises acrylate group, and the photopolymerizable monomers include but are not limited to 1, 4-butanediol di (meth) acrylate, 1, 6-hexanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate adipate, neopentyl glycol di (meth) acrylate hydroxypivalate, dicyclopentadienyl di (meth) acrylate, caprolactone modified dicyclopentadiene di (meth) acrylate, allylated cyclohexyl di (meth) acrylate, isocyanurate di (meth) acrylate, trimethylolpropane tri (meth) acrylate, and mixtures thereof, At least one of trimethyl tri (methyl) acrylate, tris (propylene oxyethyl) isocyanurate, ethoxy modified trimethylolpropane triacrylate, glycerol propoxylate triacrylate, ethoxylated bisphenol A dimethacrylate and aliphatic urethane prepolymer.
5. The plating-resistant photoresist for the novel C-HJT battery process as claimed in claim 1, wherein the photoinitiator is one or more of benzoin and benzoin alkyl ethers, acetophenones, anthraquinones, ketals, organic peroxides, thiol compounds, organic halides, benzophenones or thiazolones, and phenylphosphines.
6. The plating resist for the manufacture of novel C-HJT cell as claimed in claim 5, wherein photo initiation aids including but not limited to one or more of ethyl N, N-dimethylaminobenzoate, isoamyl N, N-dimethylaminobenzoate, amyl-4-dimethylaminobenzoate, triethylamine, triethanolamine are added to the raw materials.
7. The plating-resistant photoresist for the manufacture of novel C-HJT battery as claimed in claim 5, wherein the photoinitiator is selected from the group consisting of photoinitiator 907 manufactured by Strong New materials GmbH and photoinitiator DETX manufactured by chemical reagents GmbH.
8. The plating resist photoresist for the manufacture of novel C-HJT cell as claimed in claim 1, wherein said raw material further comprises 0.5-1 part of surfactant, wherein said surfactant is at least one selected from the group consisting of fluorinated surfactant and siloxane surfactant.
9. The plating resist for the manufacture of novel C-HJT cell as defined in claim 1 wherein the raw materials further comprise a solvent selected from the group consisting of methanol, ethanol, propanol, butanol, acetone, methyl ethyl ketone, N-methyl 2-pyrrolidone, methyl ethyl ketone, methyl cellosolve, ethyl cellosolve, butyl cellosolve, toluene, N' -dimethylformamide, propylene glycol monomethyl ether, dimethyl sulfoxide, diethyl sulfoxide, phenol, o-cresol, m-cresol, p-cresol, xylenol, halogenated phenols, catechol, tetrahydrofuran, dioxane, dioxolane, trimethylene glycol methyl ether, tetraethylene glycol dimethyl ether, γ -butyrolactone, hexamethyl-o-amide, propylene glycol methyl ether acetate, and mixtures thereof.
CN202210025921.8A 2022-01-11 2022-01-11 Electroplating-resistant photoresist for novel C-HJT battery manufacturing process Pending CN114397796A (en)

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