CN114752012A - Polyacrylate resin for positive conductive silver paste and preparation method thereof - Google Patents
Polyacrylate resin for positive conductive silver paste and preparation method thereof Download PDFInfo
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- CN114752012A CN114752012A CN202210493566.7A CN202210493566A CN114752012A CN 114752012 A CN114752012 A CN 114752012A CN 202210493566 A CN202210493566 A CN 202210493566A CN 114752012 A CN114752012 A CN 114752012A
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- silver paste
- conductive silver
- polyacrylate resin
- positive conductive
- emulsifier
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000004925 Acrylic resin Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 30
- 239000000178 monomer Substances 0.000 claims abstract description 26
- 239000003999 initiator Substances 0.000 claims abstract description 24
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- QRIMLDXJAPZHJE-UHFFFAOYSA-N 2,3-dihydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(O)CO QRIMLDXJAPZHJE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 239000000839 emulsion Substances 0.000 claims description 33
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 25
- 229920000058 polyacrylate Polymers 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000011780 sodium chloride Substances 0.000 claims description 13
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 8
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 7
- 238000000465 moulding Methods 0.000 abstract description 6
- 239000002002 slurry Substances 0.000 abstract description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 8
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000013008 thixotropic agent Substances 0.000 description 2
- JHPBZFOKBAGZBL-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylprop-2-enoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)=C JHPBZFOKBAGZBL-UHFFFAOYSA-N 0.000 description 1
- -1 acrylic ester Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012874 anionic emulsifier Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012875 nonionic emulsifier Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sustainable Energy (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Conductive Materials (AREA)
Abstract
The invention relates to the technical field of solar cell materials, in particular to polyacrylate resin for positive conductive silver paste and a preparation method thereof. The polyacrylate resin for the positive conductive silver paste comprises the following raw materials: acrylate monomer, glycerol methacrylate, deionized water, initiator and emulsifier. The polyacrylate resin for the positive conductive silver paste is used in the positive conductive silver paste, can improve the viscosity and rheological property of the conductive silver paste, achieves excellent printing effect and molding effect while enabling a fine grid circuit to have higher aspect ratio, ensures the printing property of slurry, and solves the problems that the existing slurry with high aspect ratio has poor material return and more broken grids in the printing process; the preparation method for preparing the polyacrylate resin for the positive conductive silver paste is simple in preparation process and convenient to prepare.
Description
Technical Field
The invention relates to the technical field of solar cell materials, in particular to polyacrylate resin for positive conductive silver paste and a preparation method thereof.
Background
Polyacrylate resin is a generic name of polymers of acrylic ester, methacrylic ester and derivatives thereof, and can achieve different physical properties and chemical properties according to the collocation of different monomers. And resins can be classified into thermoplastic resins and thermosetting resins according to the linear structure or network-like crosslinked structure of polyacrylic resins. Due to the excellent performance of the acrylic resin and abundant and diversified molecular designs, the acrylic resin is widely applied to various fields such as coatings, adhesives, printing ink and the like, and is also applied to conductive silver paste.
The main components of the conductive silver paste comprise silver powder, glass powder and an organic carrier, wherein the organic carrier is a dispersion medium of the silver powder and the glass powder, influences the viscosity and rheological property of the paste and plays the most important role in the printing effect of the paste. The organic vehicle is composed of a solvent, a resin and an auxiliary agent, wherein the resin plays a key role in the performance of the organic vehicle. With the continuous breakthrough of the conversion rate of the solar cell, the requirement on the aspect ratio of the ultrafine grid lines is higher and higher, but the paste with the high aspect ratio has the problems of poor material return and more broken grids in the printing process.
Disclosure of Invention
The invention aims to provide polyacrylate resin for positive conductive silver paste, which is used for the positive conductive silver paste, can improve the viscosity and rheological property of the conductive silver paste, achieves excellent printing effect and molding effect while enabling a fine grid circuit to have higher height-width ratio, ensures the printing property of slurry, and solves the problems of poor material return and more broken grids in the printing process of the current slurry with the high height-width ratio.
The invention also aims to provide a preparation method of the polyacrylate resin for preparing the positive conductive silver paste, which is simple in preparation process and convenient to prepare, and the prepared polyacrylate resin can improve the viscosity and rheological property of the conductive silver paste, so that a fine grid circuit has a higher aspect ratio and achieves excellent printing effect and molding effect.
In order to achieve the purpose, the invention adopts the following technical scheme:
the polyacrylate resin for the positive conductive silver paste comprises the following raw materials: acrylate monomer, glycerol methacrylate, deionized water, initiator and emulsifier.
Further, the raw materials comprise the following components in parts by weight: 80-90 parts of acrylate monomer, 10-20 parts of glycerol methacrylate, 100-150 parts of deionized water, 0.8-2 parts of initiator and 2-3.5 parts of emulsifier.
Still further, the acrylate monomer is selected from the group consisting of two or more of methyl methacrylate, butyl acrylate and methyl acrylate.
More specifically, the initiator is azobisisobutyronitrile.
Further, the emulsifier is any one of sodium dodecyl sulfate or sodium dodecyl sulfate.
A preparation method of polyacrylate resin for positive conductive silver paste is used for preparing the polyacrylate resin for positive conductive silver paste, and comprises the following steps:
(1) mixing deionized water and an emulsifier, and stirring and dispersing at high speed for 10-20 min at room temperature to dissolve the emulsifier;
(2) adding an initiator, an acrylate monomer and glyceryl methacrylate, and stirring at high speed for 20-30 min at room temperature to obtain a pre-emulsion;
(3) heating the pre-emulsion to 70-90 ℃ in a nitrogen atmosphere, and stirring for reacting for 6-10 h to obtain a polyacrylate emulsion;
(4) and after the reaction is finished, cooling to room temperature, adding methanol and sodium chloride, filtering to obtain a white solid, washing, and drying to obtain the polyacrylate resin for the positive conductive silver paste.
More specifically, in the step (4), the amount of the added methanol is 5 wt% of the total weight of the polyacrylate emulsion, and the amount of the added sodium chloride is 10 wt% of the total weight of the polyacrylate emulsion.
Further, the stirring speed in the step (1), the step (2) and the step (3) is 180-220 r/min respectively.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
the polyacrylate resin for the positive conductive silver paste is prepared by using an acrylate monomer, glyceryl methacrylate, deionized water, an initiator and an emulsifier as raw materials and used in the positive conductive silver paste of the solar cell, the polyacrylate resin is in the positive conductive silver paste of the solar cell, so that the paste has proper viscoelasticity, the paste has better balance between a printing effect and a fine grid height-width ratio, the acting force between resins can be improved by a 1, 2-dihydroxy structure in the glyceryl methacrylate, and the polyacrylate resin is better combined and dispersed with inorganic particles at the same time, the polyacrylate resin is used in the positive conductive silver paste, the viscosity and rheological property of the conductive silver paste can be improved, a fine grid circuit has a higher height-width ratio, an excellent printing effect and a molding effect are achieved, and the printing property of the paste is ensured, the problems that the existing paste with high aspect ratio has poor material return and more broken grids in the printing process are solved;
the preparation method of the polyacrylate resin for the positive conductive silver paste is further provided, deionized water and an emulsifier are mixed, the emulsifier is dissolved, an initiator, an acrylate monomer and glyceryl methacrylate are added, a pre-emulsion is obtained through stirring, the pre-emulsion is stirred and reacts for 6-10 hours at 70-90 ℃ to obtain a polyacrylate emulsion, methanol and sodium chloride are added for demulsification, white solid is obtained through filtration, the white solid is washed repeatedly by deionized water and then dried, and the polyacrylate resin for the positive conductive silver paste is obtained.
Detailed Description
The polyacrylate resin for the conductive silver paste of the positive electrode comprises the following raw materials: acrylate monomer, glycerol methacrylate, deionized water, initiator and emulsifier.
The polyacrylate resin for the positive conductive silver paste is prepared by using an acrylate monomer, glyceryl methacrylate, deionized water, an initiator and an emulsifier as raw materials and is used in the positive conductive silver paste of the solar cell, the polyacrylate resin is in the positive conductive silver paste of the solar cell, so that the paste has proper viscoelasticity, the paste has better balance between the printing effect and the aspect ratio of a fine grid, the acting force between resins can be improved by the structure of 1, 2-dihydroxy in the glyceryl methacrylate, and the polyacrylate resin is better combined and dispersed with inorganic particles at the same time, the polyacrylate resin is used in the positive conductive silver paste, the viscosity and rheological property of the conductive silver paste can be improved, the fine grid circuit has higher aspect ratio, excellent printing effect and molding effect are achieved, and the printing property of the paste is ensured, the problems that the existing paste with high aspect ratio has poor material return and more broken grids in the printing process are solved.
Specifically, glycerol methacrylate has a CAS number of 201594-54-9.
Further, the raw materials comprise the following components in parts by weight: 80-90 parts of acrylate monomer, 10-20 parts of glycerol methacrylate, 100-150 parts of deionized water, 0.8-2 parts of initiator and 2-3.5 parts of emulsifier.
By limiting the addition amount of each raw material in the formula, the prepared polyacrylate resin has proper viscoelasticity, the viscosity and rheological property of the conductive silver paste can be better improved, the printing effect of the solar cell positive conductive silver paste is ensured, and the problem that the current high aspect ratio is contradictory to the good printing property is solved.
Still further, the acrylate monomer is selected from the group consisting of two or more of methyl methacrylate, butyl acrylate and methyl acrylate.
The acrylate monomer is universally used, the methyl methacrylate, the butyl acrylate and the methyl acrylate are selected, the raw materials are low in cost and easy to obtain, and the hard monomer and the soft monomer form a block copolymer, so that the prepared polyacrylate resin is excellent in performance and has proper viscoelasticity, and the viscosity and rheological property of the conductive silver paste can be well improved.
More specifically, the initiator is azobisisobutyronitrile.
By using azodiisobutyronitrile as an initiator, the azo initiator has stable reaction, no side reaction and better control, can initiate polymerization reaction, and ensures the preparation effect of the polyacrylate resin for the positive conductive silver paste.
Further, the emulsifier is any one of sodium dodecyl sulfate or sodium dodecyl sulfate.
The emulsifier is used to play a role in emulsification, and the commonly used anionic emulsifier sodium dodecyl sulfate or sodium dodecyl sulfate is used, so that the raw materials are low in cost and easy to obtain, the emulsification effect is good, and no cloud point exists in the nonionic emulsifier.
A preparation method of polyacrylate resin for positive conductive silver paste is used for preparing the polyacrylate resin for positive conductive silver paste, and comprises the following steps:
(1) mixing deionized water and an emulsifier, and stirring and dispersing at high speed for 10-20 min at room temperature to dissolve the emulsifier;
(2) adding an initiator, an acrylate monomer and glyceryl methacrylate, and stirring at high speed for 20-30 min at room temperature to obtain a pre-emulsion;
(3) heating the pre-emulsion to 70-90 ℃ in a nitrogen atmosphere, and stirring for reacting for 6-10 h to obtain a polyacrylate emulsion;
(4) and after the reaction is finished, cooling to room temperature, adding methanol and sodium chloride, filtering to obtain a white solid, washing, and drying to obtain the polyacrylate resin for the positive conductive silver paste.
The preparation method comprises the steps of mixing deionized water and an emulsifier, dissolving the emulsifier, adding an initiator, an acrylate monomer and glyceryl methacrylate, stirring to obtain a pre-emulsion, stirring at 70-90 ℃ for 6-10 hours to obtain a polyacrylate emulsion, adding methanol and sodium chloride to perform emulsion breaking, filtering to obtain a white solid, repeatedly washing the white solid with deionized water, and drying to obtain the polyacrylate resin for the positive conductive silver paste.
Further, by defining the reaction temperature and the reaction time in the step (3), if the reaction temperature is too low, the reaction is slow, and if the reaction temperature is too high, the reaction is not controlled, which affects the preparation effect of the polyacrylate resin for the positive electrode conductive silver paste.
More specifically, in the step (4), the amount of the added methanol is 5 wt% of the total weight of the polyacrylate emulsion, and the amount of the added sodium chloride is 10 wt% of the total weight of the polyacrylate emulsion.
After the reaction to obtain the polyacrylate emulsion, cooling the polyacrylate emulsion to room temperature, then adding a certain amount of methanol and sodium chloride to demulsify the polyacrylate emulsion, filtering to obtain a white solid, repeatedly washing the white solid with deionized water, and drying to obtain the polyacrylate resin for the positive conductive silver paste.
Preferably, the stirring speed in the step (1), the step (2) and the step (3) is 180-220 r/min respectively.
Preferably, the stirring speed in the step (1), the step (2) and the step (3) is 200r/min respectively.
Through limiting the stirring speed in the step (1), the step (2) and the step (3), the emulsifier in the step (1) can be fully dissolved through high-speed stirring, so that the initiator, the acrylate monomer and the glyceryl methacrylate in the step (2) are fully mixed, the reaction in the step (3) is fully ensured, and the preparation effect of the prepared polyacrylate resin for the positive conductive silver paste is ensured.
In order to facilitate an understanding of the present invention, a more complete description of the present invention is provided below. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
A preparation method of polyacrylate resin for positive conductive silver paste comprises the following steps:
(1) adding 150 parts of deionized water and 3 parts of emulsifier into a three-neck flask, mixing, stirring at high speed at room temperature for 15min, and dissolving the emulsifier, wherein the emulsifier is sodium dodecyl sulfate;
(2) adding 1.2 parts of initiator, 90 parts of acrylate monomer and 10 parts of glycerol methacrylate according to the mass parts, and stirring at high speed for 30min at room temperature to obtain pre-emulsion, wherein the acrylate monomer is formed by mixing methyl methacrylate and butyl methacrylate, and the mass ratio of the methyl methacrylate to the butyl methacrylate is 2: 1, the initiator is azobisisobutyronitrile;
(3) heating the pre-emulsion to 80 ℃ in a nitrogen atmosphere, keeping the stirring speed of 200r/min, and stirring for reacting for 8 hours to obtain polyacrylate emulsion;
(4) and cooling to room temperature after the reaction is finished, adding methanol and sodium chloride, wherein the addition amount of the methanol is 5 wt% of the total weight of the polyacrylate emulsion, the addition amount of the sodium chloride is 10 wt% of the total weight of the polyacrylate emulsion, filtering to obtain a white solid, repeatedly washing with deionized water, and drying to obtain the polyacrylate resin for the positive conductive silver paste.
Example 2
A preparation method of polyacrylate resin for positive conductive silver paste comprises the following steps:
(1) adding 150 parts of deionized water and 3 parts of an emulsifier into a three-neck flask, mixing, stirring at high speed at room temperature for 15min, and dissolving the emulsifier, wherein the emulsifier is sodium dodecyl sulfate;
(2) adding 1.2 parts of initiator, 80 parts of acrylate monomer and 20 parts of glycerol methacrylate according to the mass parts, and stirring at high speed for 30min at room temperature to obtain a pre-emulsion, wherein the acrylate monomer is formed by mixing methyl methacrylate and butyl methacrylate, and the mass ratio of the methyl methacrylate to the butyl methacrylate is 2: 1, the initiator is azobisisobutyronitrile;
(3) heating the pre-emulsion to 80 ℃ in the nitrogen atmosphere, keeping the stirring speed of 200r/min, and stirring for reacting for 8 hours to obtain polyacrylate emulsion;
(4) and cooling to room temperature after the reaction is finished, adding methanol and sodium chloride, wherein the addition amount of the methanol is 5 wt% of the total weight of the polyacrylate emulsion, the addition amount of the sodium chloride is 10 wt% of the total weight of the polyacrylate emulsion, filtering to obtain a white solid, repeatedly washing with deionized water, and drying to obtain the polyacrylate resin for the positive conductive silver paste.
The polyacrylate resin for the positive conductive silver paste prepared in the above embodiments 1 and 2 and other raw materials are prepared into a conductive silver paste, the raw material ratio of the conductive silver paste is calculated according to the mass parts of 0.8 part of polyacrylate resin, 6 parts of solvent, 1 part of silicone oil, 0.45 part of dispersant, 0.25 part of thixotropic agent, 2 parts of glass powder and 89.5 parts of silver powder, the other raw materials except the polyacrylate resin are conventional raw materials, and after the raw materials are uniformly dispersed, the paste is printed and sintered according to the conventional process, and the performance is tested.
Comparative example 1
The conductive silver paste is prepared by mixing imported polyacrylic resin D and other raw materials, wherein the raw material ratio of the conductive silver paste is calculated according to the mass parts of 0.8 part of polyacrylate resin, 6 parts of solvent, 1 part of silicone oil, 0.45 part of dispersing agent, 0.25 part of thixotropic agent, 2 parts of glass powder and 89.5 parts of silver powder, the polyacrylate resin and the other raw materials are conventional raw materials, the raw materials are uniformly dispersed, and then the paste is printed and sintered according to the conventional process, and the performance is tested.
The results of the performance tests are shown in table 1 below:
table 1 results of performance test of examples and comparative examples
Test items | Example 1 | Example 2 | Comparative example 1 |
Feed back | Superior food | Superior food | Superior food |
Number of broken grids | 3 | 3 | 3 |
Thin grid line height (mum) | 19.15 | 19.38 | 18.13 |
Fine grid line width (mum) | 49.65 | 46.62 | 53.66 |
Aspect ratio | 0.38 | 0.41 | 0.33 |
Cell efficiency (%) | 20.247 | 20.301 | 20.180 |
The test results show that the aspect ratio of the embodiment 1 and the embodiment 2 is better than that of the comparative example 1, the efficiency of the battery piece of the embodiment 1 and the embodiment 2 is also better than that of the comparative example 1, and meanwhile, the printing performance of the embodiment 1 and the embodiment 2 is not reduced, so that the polyacrylic resin for the positive conductive silver paste prepared by the invention can improve the viscosity and rheological property of the conductive silver paste, can ensure the printing property of the paste while ensuring the high aspect ratio of the fine grid circuit, and achieves excellent printing effect and molding effect.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. The polyacrylate resin for the positive conductive silver paste is characterized by comprising the following raw materials: acrylate monomer, glycerol methacrylate, deionized water, initiator and emulsifier.
2. The polyacrylate resin for the positive conductive silver paste according to claim 1, wherein the polyacrylate resin comprises the following raw materials in parts by mass: 80-90 parts of acrylate monomer, 10-20 parts of glycerol methacrylate, 100-150 parts of deionized water, 0.8-2 parts of initiator and 2-3.5 parts of emulsifier.
3. The polyacrylate resin for positive conductive silver paste according to claim 1, wherein the acrylate monomer is selected from the group consisting of two or more of methyl methacrylate, butyl acrylate and methyl acrylate.
4. The polyacrylate resin for the positive electrode conductive silver paste according to claim 1, wherein the initiator is azobisisobutyronitrile.
5. The polyacrylate resin for the positive conductive silver paste of claim 1, wherein the emulsifier is any one of sodium dodecyl sulfate or sodium dodecyl sulfate.
6. The preparation method of the polyacrylate resin for the positive conductive silver paste is characterized by comprising the following steps of:
(1) mixing deionized water and an emulsifier, and stirring and dispersing at high speed for 10-20 min at room temperature to dissolve the emulsifier;
(2) adding an initiator, an acrylate monomer and glyceryl methacrylate, and stirring at high speed for 20-30 min at room temperature to obtain a pre-emulsion;
(3) heating the pre-emulsion to 70-90 ℃ in a nitrogen atmosphere, and stirring for reacting for 6-10 h to obtain a polyacrylate emulsion;
(4) and after the reaction is finished, cooling to room temperature, adding methanol and sodium chloride, filtering to obtain a white solid, washing, and drying to obtain the polyacrylate resin for the positive conductive silver paste.
7. The method for preparing polyacrylate resin for positive electrode conductive silver paste according to claim 6, wherein in the step (4), methanol is added in an amount of 5 wt% and sodium chloride is added in an amount of 10 wt% based on the total weight of the polyacrylate emulsion.
8. The method for preparing the polyacrylate resin for the positive conductive silver paste according to claim 6, wherein the stirring speed in the step (1), the step (2) and the step (3) is 180-220 r/min.
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Citations (9)
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