CN117887025A - Conductive resin applied to heterojunction battery and preparation method thereof - Google Patents
Conductive resin applied to heterojunction battery and preparation method thereof Download PDFInfo
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- CN117887025A CN117887025A CN202410303961.3A CN202410303961A CN117887025A CN 117887025 A CN117887025 A CN 117887025A CN 202410303961 A CN202410303961 A CN 202410303961A CN 117887025 A CN117887025 A CN 117887025A
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- epoxy resin
- conductive resin
- heterojunction
- vegetable oil
- heating
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- 229920005989 resin Polymers 0.000 title claims abstract description 46
- 239000011347 resin Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003822 epoxy resin Substances 0.000 claims abstract description 77
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 77
- 229920005862 polyol Polymers 0.000 claims abstract description 64
- 150000003077 polyols Chemical class 0.000 claims abstract description 64
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 52
- 239000008158 vegetable oil Substances 0.000 claims abstract description 52
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000001816 cooling Methods 0.000 claims abstract description 39
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 34
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 34
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 33
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 33
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 22
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 claims abstract description 21
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 11
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 3
- 125000002723 alicyclic group Chemical group 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 20
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- 239000002086 nanomaterial Substances 0.000 claims description 10
- 238000009849 vacuum degassing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 30
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 12
- 239000004593 Epoxy Substances 0.000 description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 229920005749 polyurethane resin Polymers 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 238000004321 preservation Methods 0.000 description 8
- 229910021417 amorphous silicon Inorganic materials 0.000 description 7
- 238000013329 compounding Methods 0.000 description 7
- 239000010408 film Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910021419 crystalline silicon Inorganic materials 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000002313 adhesive film Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/6547—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/36 or hydroxylated esters of higher fatty acids of C08G18/38
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/58—Epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
-
- 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
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H13/00—Switches having rectilinearly-movable operating part or parts adapted for pushing or pulling in one direction only, e.g. push-button switch
-
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Dispersion Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a conductive resin applied to a heterojunction battery and a preparation method thereof, comprising the following steps: (1) Mixing hydroxylated carbon nanotubes, diphenylmethane 4,4' -diisocyanate and N, N-dimethylformamide to prepare isocyanated carbon nanotubes; (2) Adding vegetable oil polyol into a reaction vessel, continuously adding xylylene diisocyanate, isocyanated carbon nano tubes and cyclohexanone, heating to 65-75 ℃ under nitrogen atmosphere, preserving heat for 30-40min, adding di-n-butyl tin oxide, heating, and reacting to obtain polyurethane prepolymer; (3) Mixing polyurethane prepolymer, epoxy resin and diethylene glycol, and reacting at 80-85 ℃ for 3-4h; cooling to 40 ℃, adding triethylamine for neutralization, and reacting for 4-5min to obtain the conductive resin. The conductive resin prepared by the method can be applied to the preparation of heterojunction batteries, and has more excellent conductive effect.
Description
Technical Field
The invention belongs to the technical field of conductive resin, and particularly relates to a conductive resin applied to a heterojunction battery and a preparation method thereof.
Background
Along with the rapid development of the photovoltaic industry, the demand for novel products is continuously increased, and in order to adapt to the diversified development of the photovoltaic market, when the power and the voltage required by the market cannot be considered, the solar cell needs to be cut to form a half-cell. Heterojunction (HIT) is a special PN junction formed of amorphous silicon and crystalline silicon material, which is one of N-type batteries in which an amorphous silicon thin film is deposited on crystalline silicon. HIT cells were first successfully developed by the japanese Sanyo company in 1990, and are also called HJT, HDT, or SHJ because HIT has been registered as a trademark by Sanyo. When the heterojunction battery is assembled, glass is usually arranged on one side of the battery piece, and a back plate is arranged on the other side of the battery piece. The cell and the glass and the cell and the back plate are connected through adhesive films, and the transparent conductive films on two sides of the cell are in direct contact with the adhesive films. The heterojunction battery is a high-efficiency crystalline silicon solar battery structure, and is a hybrid solar battery made of crystalline silicon substrates and amorphous silicon films, namely, a layer of undoped (intrinsic) hydrogenated amorphous silicon film heterojunction battery is added between P-type hydrogenated amorphous silicon and N-type silicon substrates, and is fully called as an intrinsic film heterojunction battery.
The heterojunction solar cell has the following specific advantages: 1. no PID phenomenon: because the upper surface of the battery is TCO, the charge can not generate polarization phenomenon on the TCO on the surface of the battery, and PID phenomenon is avoided. This was also confirmed by the measured data. Technical application and prospect of heterojunction solar cells. 2. The low-temperature manufacturing process comprises the following steps: the processing temperature of all the manufacturing processes of HJT batteries is lower than 250, the high-temperature diffusion junction manufacturing process with low production efficiency and high cost is avoided, the optical band gap, the deposition rate, the absorption coefficient and the hydrogen content of the a-Si film are accurately controlled by the low-temperature process, and adverse effects such as thermal stress caused by high temperature can be avoided. 3. High efficiency: HJT batteries have been refreshing world records of battery conversion efficiency for mass production. HJT cells have an efficiency 1-2% higher than P-type single crystal silicon cells and the difference between them is slowly increasing. 4. Technical application and prospect of heterojunction solar cells with high illumination stability: the Staebler-Wronski effect common in amorphous silicon solar cells does not occur in HJT solar cells. Meanwhile, the N-type silicon wafer adopted by HJT battery has no light attenuation phenomenon because the doping agent is phosphorus. 5. Can develop to the thinning: the HJT battery has low processing temperature, symmetrical upper and lower surface structures, no mechanical stress, and smooth thinning, and the thinner the chip, the higher the open-circuit voltage can be obtained for the N-type silicon substrate with higher minority carrier lifetime.
Polyurethane resin is generally added into the existing heterojunction battery silver grid line conductive silver paste, but the conductivity of the polyurethane resin is not ideal, and the conductivity of the conductive silver paste is affected.
Disclosure of Invention
The invention aims to provide a conductive resin applied to a heterojunction battery and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
A method for preparing conductive resin applied to heterojunction cells, comprising the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide according to the mass ratio of 1:1:7-9, heating to 80-100 ℃ for reacting for 25-30h, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction container, heating to 60-70 ℃, stirring under the condition of vacuum degree of 0.07-0.08MPa, vacuum degassing for 30-40min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 65-75 ℃ under nitrogen atmosphere, preserving heat for 30-40min, adding di-n-butyl tin oxide, heating to 100-110 ℃ and reacting for 4-5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 80-85 ℃ and enabling the mass ratio to be 12-14:1: mixing polyurethane prepolymer of 0.2-0.5, epoxy resin and diethylene glycol, and reacting at 80-85 ℃ for 3-4h; cooling to 40 ℃, adding triethylamine for neutralization, and reacting for 4-5min to obtain the conductive resin.
Further, the mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the isocyanated carbon nano tube is 2-3:1: 0.05-0.07.
Further, the mass of the di-n-butyl tin oxide accounts for 0.3-0.7% of the mass of the vegetable oil polyol.
Further, the vegetable oil polyol has a hydroxyl value of 170.+ -.10 mgKOH/g.
Further, the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor City aviation technology Co. The vegetable oil polyol is soybean oil polyol.
Further, the hydroxylated carbon nanotube is a carbon nanotube of XFD02 of Jiangsu Xianfeng nanomaterial science and technology Co.
Further, the epoxy resin is selected from one or more of bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin and alicyclic epoxy resin.
Further, the epoxy resin is a compound of bisphenol A epoxy resin and alicyclic epoxy resin.
Further, the mass ratio of the bisphenol A type epoxy resin to the alicyclic epoxy resin is 1:1.4-1.6.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
The triethylamine in the invention is used in an amount that the conductive resin is neutral.
The invention also provides the conductive resin applied to the heterojunction battery, which is prepared by the preparation method.
Compared with the prior art, the invention has the advantages that: the invention provides a conductive resin applied to a heterojunction battery and a preparation method thereof, wherein the conductive property of the resin is increased by adding conductive filler carbon nano tubes, and the carbon nano tubes have excellent conductive property, and when the carbon nano tubes are uniformly dispersed in polyurethane resin, a conductive network can be formed, so that the overall conductivity is improved. The polyurethane prepolymer prepared by using soybean oil polyol is subjected to epoxy modification, and epoxy groups are introduced into the conductive resin, so that the conductive carbon nanotubes can be more uniformly dispersed in a polyurethane resin system by the epoxy resin to form a conductive network, thereby further improving the conductivity of the polyurethane resin. Meanwhile, the epoxy group is introduced into the polyurethane resin, so that the mechanical strength of the polyurethane resin is enhanced.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a conductive resin applied to a heterojunction battery, and the preparation method comprises the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide in a mass ratio of 1:1:8, heating to 90 ℃ for reaction for 27 hours, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction container, heating to 65 ℃, stirring under the condition of 0.08MPa of vacuum degree, vacuum degassing for 35min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 70 ℃ under nitrogen atmosphere, preserving heat for 35min, adding di-n-butyl tin oxide, heating to 105 ℃ and reacting for 4.5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 82 ℃, wherein the mass ratio is 13:1: mixing polyurethane prepolymer of 0.4, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 3.5h at 82 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 4.5min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the isocyanated carbon nano tube is 2.5:1: 0.06.
The mass of the di-n-butyl tin oxide accounts for 0.5% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g; the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is formed by compounding bisphenol A epoxy resin and alicyclic epoxy resin, and the mass ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 1:1.5.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
Example 2
The embodiment provides a conductive resin applied to a heterojunction battery, and the preparation method comprises the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide in a mass ratio of 1:1:7, heating to 80 ℃ for reaction for 25 hours, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction vessel, heating to 60 ℃, stirring under the condition of vacuum degree of 0.07MPa, vacuum degassing for 30min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 65 ℃ under nitrogen atmosphere, preserving heat for 30min, adding di-n-butyltin oxide, heating to 100 ℃ and reacting for 4h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 80 ℃, and enabling the mass ratio to be 12:1: mixing polyurethane prepolymer of 0.2, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 3h at 80 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 4min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the isocyanated carbon nano tube is 2:1: 0.05.
The mass of the di-n-butyl tin oxide accounts for 0.3% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g; the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is formed by compounding bisphenol A epoxy resin and alicyclic epoxy resin, and the mass ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 1:1.4.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
Example 3
The embodiment provides a conductive resin applied to a heterojunction battery, and the preparation method comprises the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide in a mass ratio of 1:1:9, heating to 100 ℃ for reaction for 30 hours, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction container, heating to 70 ℃, stirring under the condition of 0.08MPa of vacuum degree, vacuum degassing for 40min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 75 ℃ under nitrogen atmosphere, preserving heat for 40min, adding di-n-butyltin oxide, heating to 110 ℃, and reacting for 5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 85 ℃, and mixing the components according to the mass ratio of 14:1: mixing polyurethane prepolymer of 0.5, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 4 hours at 85 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 5min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the isocyanated carbon nano tube is 3:1: 0.07.
The mass of the di-n-butyl tin oxide accounts for 0.7% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g.
The vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is formed by compounding bisphenol A epoxy resin and alicyclic epoxy resin, and the mass ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 1:1.6.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
Comparative example 1
The difference between this comparative example and example 1 is: the carbon nanotubes are directly added.
The method comprises the following steps: a preparation method of conductive resin applied to heterojunction batteries comprises the following steps:
(1) Adding vegetable oil polyol into a reaction container, heating to 65 ℃, stirring under the condition of 0.08MPa of vacuum degree, vacuum degassing for 35min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, hydroxylated carbon nano tube and cyclohexanone, heating to 70 ℃ under nitrogen atmosphere, preserving heat for 35min, adding di-n-butyl tin oxide, heating to 105 ℃ and reacting for 4.5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 82 ℃, wherein the mass ratio is 13:1: mixing polyurethane prepolymer of 0.4, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 3.5h at 82 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 4.5min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the hydroxylated carbon nano tube is 2.5:1: 0.06.
The mass of the di-n-butyl tin oxide accounts for 0.5% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g; the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is formed by compounding bisphenol A epoxy resin and alicyclic epoxy resin, and the mass ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 1:1.5.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
Comparative example 2
This comparative example provides the difference from example 1: the isocyanated carbon nanotubes are replaced with diphenylmethane 4,4' -diisocyanate.
The method comprises the following steps: a preparation method of conductive resin applied to heterojunction batteries comprises the following steps:
(1) Adding vegetable oil polyol into a reaction container, heating to 65 ℃, stirring under the condition of 0.08MPa of vacuum degree, vacuum degassing for 35min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, diphenylmethane 4,4' -diisocyanate and cyclohexanone, heating to 70 ℃ under nitrogen atmosphere, preserving heat for 35min, adding di-n-butyltin oxide, heating to 105 ℃, and reacting for 4.5h to obtain polyurethane prepolymer;
(2) Cooling the polyurethane prepolymer to 82 ℃, wherein the mass ratio is 13:1: mixing polyurethane prepolymer of 0.4, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 3.5h at 82 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 4.5min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the diphenylmethane 4,4' -diisocyanate is 2.5:1: 0.06.
The mass of the di-n-butyl tin oxide accounts for 0.5% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g; the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is formed by compounding bisphenol A epoxy resin and alicyclic epoxy resin, and the mass ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 1:1.5.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
Comparative example 3
The difference between this comparative example and example 1 is: the epoxy resin is bisphenol A type epoxy resin.
The method comprises the following steps: a preparation method of conductive resin applied to heterojunction batteries comprises the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide in a mass ratio of 1:1:8, heating to 90 ℃ for reaction for 27 hours, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction container, heating to 65 ℃, stirring under the condition of 0.08MPa of vacuum degree, vacuum degassing for 35min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 70 ℃ under nitrogen atmosphere, preserving heat for 35min, adding di-n-butyl tin oxide, heating to 105 ℃ and reacting for 4.5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 82 ℃, wherein the mass ratio is 13:1: mixing polyurethane prepolymer of 0.4, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 3.5h at 82 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 4.5min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the isocyanated carbon nano tube is 2.5:1: 0.06.
The mass of the di-n-butyl tin oxide accounts for 0.5% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g; the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is bisphenol A type epoxy resin.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq.
Comparative example 4
The difference between this comparative example and example 1 is: the mass ratio of the bisphenol A type epoxy resin to the alicyclic epoxy resin is 1:0.6.
The method comprises the following steps: a preparation method of conductive resin applied to heterojunction batteries comprises the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide in a mass ratio of 1:1:8, heating to 90 ℃ for reaction for 27 hours, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction container, heating to 65 ℃, stirring under the condition of 0.08MPa of vacuum degree, vacuum degassing for 35min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 70 ℃ under nitrogen atmosphere, preserving heat for 35min, adding di-n-butyl tin oxide, heating to 105 ℃ and reacting for 4.5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 82 ℃, wherein the mass ratio is 13:1: mixing polyurethane prepolymer of 0.4, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 3.5h at 82 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 4.5min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the isocyanated carbon nano tube is 2.5:1: 0.06.
The mass of the di-n-butyl tin oxide accounts for 0.5% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g; the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is formed by compounding bisphenol A epoxy resin and alicyclic epoxy resin, and the mass ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 1:0.6.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
Comparative example 5
The difference between this comparative example and example 1 is: the mass ratio of the bisphenol A type epoxy resin to the alicyclic epoxy resin is 1:3.
The method comprises the following steps: a preparation method of conductive resin applied to heterojunction batteries comprises the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide in a mass ratio of 1:1:8, heating to 90 ℃ for reaction for 27 hours, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction container, heating to 65 ℃, stirring under the condition of 0.08MPa of vacuum degree, vacuum degassing for 35min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 70 ℃ under nitrogen atmosphere, preserving heat for 35min, adding di-n-butyl tin oxide, heating to 105 ℃ and reacting for 4.5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 82 ℃, wherein the mass ratio is 13:1: mixing polyurethane prepolymer of 0.4, epoxy resin and diethylene glycol, and carrying out heat preservation reaction for 3.5h at 82 ℃; cooling to 40 ℃, adding triethylamine to neutralize, and reacting for 4.5min to obtain the conductive resin.
The mass ratio of the vegetable oil polyol to the xylylene diisocyanate to the isocyanated carbon nano tube is 2.5:1: 0.06.
The mass of the di-n-butyl tin oxide accounts for 0.5% of the mass of the vegetable oil polyol.
The hydroxyl value of the vegetable oil polyol is 170+/-10 mgKOH/g; the vegetable oil polyol is FH3170 polyol of the Zhangjiu harbor city of the aviation technology Co.
The hydroxylated carbon nanotube is XFD02 of Jiangsu Xianfeng nano material technology Co.
The epoxy resin is formed by compounding bisphenol A epoxy resin and alicyclic epoxy resin, and the mass ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 1:3.
The bisphenol A type epoxy resin is purchased from Wan Qing chemical technology Co., ltd, and the epoxy equivalent is 180-190g/eq; the alicyclic epoxy resin is Jiangsu Pu Le Si biological technology Co., ltd, and the viscosity is 400-750 mPa.s.
Performance testing
The conductive resin prepared in the examples and the comparative examples is used for preparing the conductive silver paste of the heterojunction battery silver grid line, and the conductive silver paste consists of the following raw materials: 4.5g of conductive resin, 0.40g of coupling agent KH560 0.045g,BYK203 0.01g,4,4-diamine diphenyl sulfone, 0.008g of benzyl dimethylamine, ethanol and acetone 1:1 (weight ratio) mixed solvent 0.5g, carboxyl-terminated liquid nitrile rubber 0.10g, salicylic acid 0.05g, cyclohexanone and ethylene glycol monomethyl ether 1: 0.5 (weight ratio) mixing diluent 8.0g, tributyl phosphate 0.01g, flake silver powder 90g and nano silver powder 5g. The control group was a commercially available polyurethane resin, available from Shanghai shou Xingjingsu, inc., model CR606. Curing the conductive silver paste: curing at 180 deg.c/10 min, and then measuring the adhesive strength and volume resistivity.
TABLE 1 Performance test results
As is clear from examples, the conductive resins prepared in examples 1 to 3 of the present invention prepared conductive silver pastes, which have different volume resistivity, while a lower volume resistivity represents a higher conductivity. The conductive resin prepared by the invention is superior to the polyurethane resin sold in the market, and the performance is reduced to different degrees by changing the preparation raw materials and conditions as shown in comparative examples 1-5.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A method for preparing a conductive resin for a heterojunction battery, comprising the following steps:
(1) Mixing the hydroxylated carbon nano tube, the diphenylmethane 4,4' -diisocyanate and the N, N-dimethylformamide according to the mass ratio of 1:1:7-9, heating to 80-100 ℃ for reacting for 25-30h, cooling, centrifuging, washing and drying to obtain the isocyanated carbon nano tube;
(2) Adding vegetable oil polyol into a reaction container, heating to 60-70 ℃, stirring under the condition of vacuum degree of 0.07-0.08MPa, vacuum degassing for 30-40min, cooling to 45 ℃, stopping stirring and vacuumizing; continuously adding xylylene diisocyanate, isocyanated carbon nano tube and cyclohexanone, heating to 65-75 ℃ under nitrogen atmosphere, preserving heat for 30-40min, adding di-n-butyl tin oxide, heating to 100-110 ℃ and reacting for 4-5h to obtain polyurethane prepolymer;
(3) Cooling the polyurethane prepolymer to 80-85 ℃ and enabling the mass ratio to be 12-14:1: mixing polyurethane prepolymer of 0.2-0.5, epoxy resin and diethylene glycol, and reacting at 80-85 ℃ for 3-4h; cooling to 40 ℃, adding triethylamine for neutralization, and reacting for 4-5min to obtain the conductive resin.
2. The method for preparing the conductive resin applied to the heterojunction cell as claimed in claim 1, wherein the mass ratio of the vegetable oil polyol, the xylylene diisocyanate and the isocyanated carbon nano tube is 2-3:1: 0.05-0.07.
3. The method for preparing a conductive resin for heterojunction cells as claimed in claim 1, wherein the mass of di-n-butyltin oxide is 0.3-0.7% of the mass of the vegetable oil polyol.
4. The method for preparing a conductive resin for heterojunction cells as claimed in claim 1, wherein the hydroxyl value of the vegetable oil polyol is 170±10mgKOH/g.
5. The method for preparing a conductive resin for a heterojunction cell as claimed in claim 4, wherein the vegetable oil polyol is FH3170 polyol of the company of the division of flying technology in Zhangjiu harbor.
6. The method for preparing a conductive resin applied to a heterojunction battery according to claim 1, wherein the hydroxylated carbon nanotube is a carbon nanotube of XFD02 of Jiangsu Xianfeng nanomaterial technology Co.
7. The method for preparing a conductive resin applied to a heterojunction cell as claimed in claim 1, wherein the epoxy resin is selected from one or more of bisphenol a type epoxy resin, alicyclic epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin.
8. The method for preparing a conductive resin applied to a heterojunction cell as claimed in claim 7, wherein the epoxy resin is a bisphenol a type epoxy resin and an alicyclic epoxy resin.
9. The method for preparing a conductive resin applied to a heterojunction cell as claimed in claim 8, wherein the mass ratio of bisphenol a type epoxy resin to alicyclic epoxy resin is 1:1.4-1.6.
10. A conductive resin for heterojunction cells prepared by the preparation method of any one of claims 1 to 9.
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