CN114805750A - Bisphenol A-novolac epoxy resin, conductive adhesive for main-gate-free battery component prepared from bisphenol A-novolac epoxy resin and application of conductive adhesive - Google Patents
Bisphenol A-novolac epoxy resin, conductive adhesive for main-gate-free battery component prepared from bisphenol A-novolac epoxy resin and application of conductive adhesive Download PDFInfo
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- CN114805750A CN114805750A CN202210588083.5A CN202210588083A CN114805750A CN 114805750 A CN114805750 A CN 114805750A CN 202210588083 A CN202210588083 A CN 202210588083A CN 114805750 A CN114805750 A CN 114805750A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 60
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 60
- 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 title claims abstract description 50
- 239000004843 novolac epoxy resin Substances 0.000 title claims abstract description 23
- 229930185605 Bisphenol Natural products 0.000 title claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 10
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000007822 coupling agent Substances 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 10
- 239000012745 toughening agent Substances 0.000 claims description 10
- 239000002048 multi walled nanotube Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000012752 auxiliary agent Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 6
- SHKUUQIDMUMQQK-UHFFFAOYSA-N 2-[4-(oxiran-2-ylmethoxy)butoxymethyl]oxirane Chemical compound C1OC1COCCCCOCC1CO1 SHKUUQIDMUMQQK-UHFFFAOYSA-N 0.000 claims description 6
- 229920000459 Nitrile rubber Polymers 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 6
- 229920002647 polyamide Polymers 0.000 claims description 6
- 239000013008 thixotropic agent Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 claims description 3
- 150000008065 acid anhydrides Chemical group 0.000 claims description 2
- 150000001412 amines Chemical group 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- OTARVPUIYXHRRB-UHFFFAOYSA-N diethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](C)(OCC)CCCOCC1CO1 OTARVPUIYXHRRB-UHFFFAOYSA-N 0.000 claims description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical group C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 abstract description 14
- 229920000647 polyepoxide Polymers 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 abstract description 6
- 238000011049 filling Methods 0.000 abstract description 6
- 238000004132 cross linking Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 229920001744 Polyaldehyde Polymers 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000004841 bisphenol A epoxy resin Substances 0.000 abstract description 3
- 238000010030 laminating Methods 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 239000000306 component Substances 0.000 description 19
- 238000001723 curing Methods 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 16
- 238000010992 reflux Methods 0.000 description 16
- 238000003756 stirring Methods 0.000 description 16
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 12
- 229920001568 phenolic resin Polymers 0.000 description 12
- 239000005011 phenolic resin Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 229910000679 solder Inorganic materials 0.000 description 5
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000005194 fractionation Methods 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 4
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- NTXGQCSETZTARF-UHFFFAOYSA-N buta-1,3-diene;prop-2-enenitrile Chemical compound C=CC=C.C=CC#N NTXGQCSETZTARF-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000013035 low temperature curing Methods 0.000 description 2
- 238000012858 packaging process Methods 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910001312 Amalgam (dentistry) Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000013082 photovoltaic technology Methods 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
- C08G59/04—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof
- C08G59/06—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof of polyhydric phenols
- C08G59/08—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof of polyhydric phenols from phenol-aldehyde condensates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- 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
- H01L31/04—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 adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/05—Electrical interconnection means between PV cells inside the PV module, e.g. series connection of PV cells
- H01L31/0504—Electrical interconnection means between PV cells inside the PV module, e.g. series connection of PV cells specially adapted for series or parallel connection of solar cells in a module
- H01L31/0512—Electrical interconnection means between PV cells inside the PV module, e.g. series connection of PV cells specially adapted for series or parallel connection of solar cells in a module made of a particular material or composition of materials
-
- 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
- C08G2170/00—Compositions for adhesives
-
- 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
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
Abstract
The invention discloses bisphenol A-novolac epoxy resin, a conductive adhesive for a main-grid-free battery component prepared from the bisphenol A-novolac epoxy resin and application of the conductive adhesive. The bisphenol A epoxy resin, the straight chain polyaldehyde and the epoxy chloropropane are used for synthesizing a novel modified epoxy resin, namely the bisphenol A-novolac epoxy resin under a certain condition, and a long carbon chain is introduced into a molecule to form a new structure, so that the crosslinking degree of the resin is improved, and the toughness of the resin is increased; after curing, the adhesive has high bonding strength, low shrinkage rate and high mechanical strength. The conductive adhesive prepared from the bisphenol A-novolac epoxy resin has the advantages that the multi-arm carbon nano tubes are introduced, the tensile strength is improved, the silver powder filling amount is reduced, the cost of the conductive adhesive is effectively reduced while the conductivity and the mechanical property are ensured, meanwhile, the assembly laminating process is perfectly adapted, the production process flow is reduced, and the production efficiency is improved.
Description
Technical Field
The invention relates to the technical field of novel materials, in particular to bisphenol A-novolac epoxy resin, a conductive adhesive for a main-grid-free battery component prepared from the bisphenol A-novolac epoxy resin and application of the conductive adhesive.
Background
Photovoltaic is an important clean energy source, and is an important energy field and technical direction in the world; the photovoltaic cell assembly is a core component of photovoltaic power generation, and the crystalline silicon cell assembly accounts for more than 95% of the market. The cost of the crystalline silicon chip and the silver paste occupies a great proportion in the crystalline silicon component, and the reduction of the silver paste amount and the silicon chip amount is very important for reducing the comprehensive cost of the component, the battery power cost and the promotion of the photovoltaic market application. The development of high-efficiency and low-cost solar cells and components is the subject of unchanged photovoltaic industry. With the development of photovoltaic technology, conventional solar cells generally use a tin-lead solder ribbon crimped to the cell's main grid to conduct current. However, the use of solder strips increases the internal resistance of the assembly, resulting in increased electrical losses during the packaging process; moreover, the width of the solder strip is generally consistent with that of the main grid of the battery, and the part of the surface of the battery, which is shielded by the solder strip, cannot receive illumination, so that the optical loss in the packaging process is increased. Therefore, the photovoltaic module prepared by using the conventional solar cell positive electrode design scheme and the solder strip interconnection welding technology has high packaging loss, and cannot fully exert the advantage of high conversion efficiency of the solar cell.
The development of the multi-line serial connection technology of the solar cell without the main grid can reduce the shading area of grid lines on the front surface of the solar cell and improve the conversion efficiency of the solar cell and the power of a component, and meanwhile, the main component of the matrix of the welding strip without the main grid is copper, so that the use amount of silver paste is greatly reduced, and the production cost of the solar cell and the component is reduced; with the development of the technology of the grid-free type solar cell, the cost of conductive adhesive is higher and higher, in order to improve the light utilization rate as much as possible, the width of grid lines is smaller and higher, the requirement on the adhesive force of the conductive adhesive is higher and higher, the high solid content of the conductive adhesive for the conventional HJT cell causes that the bonding strength of the bonded thin grid lines is weaker, and the requirement of the technology of the grid-free type solar cell cannot be met, the prepared conductive adhesive is the high-adhesive-force low-temperature curing conductive silver paste prepared by self-made specific multifunctional epoxy resin, meanwhile, the lamination process of the assembly can be perfectly matched, the curing is completed within 20min at 150 ℃, the production process flow is reduced, the production efficiency of the assembly is improved, and if the technology is industrialized, the technology has better compatibility with the production equipment of the conventional solar cell and the assembly, and the modification cost is low. More particularly, the technology without the main grid can be combined with the technology of a high-efficiency double-sided battery, namely the HJT battery, to prepare the double-sided double-glass assembly, so that the application range is wider, the power generation capacity is higher, and the investment yield is higher, so that the market popularization potential is huge. The research and development of a novel main-grid-free battery assembly becomes a current assembly research and development hot door, and in order to meet the requirements of the novel main-grid-free HJT battery assembly, reduce the cost and develop a low-temperature-curing conductive adhesive with high adhesive force and low silver filling amount, the research and development is urgent.
Disclosure of Invention
Aiming at the defects in the prior art, the invention synthesizes novel modified epoxy resin-bisphenol A-novolac epoxy resin by using bisphenol A resin, straight-chain polyaldehyde and epoxy chloropropane under a certain condition, and introduces a long carbon chain into molecules to form a new structure, thereby improving the crosslinking degree of the resin and increasing the toughness of the resin; after curing, the adhesive has high bonding strength, low shrinkage rate and high mechanical strength. The conductive adhesive prepared from the bisphenol A-novolac epoxy resin has the advantages that the multi-arm carbon nano tubes are introduced, the tensile strength is improved, the silver powder filling amount is reduced, the cost of the conductive adhesive is effectively reduced while the conductivity and the mechanical property are ensured, meanwhile, the assembly laminating process is perfectly adapted, the production process flow is reduced, and the production efficiency is improved.
The invention provides a bisphenol A-novolac epoxy resin in a first aspect, which has a structural formula shown as a general formula I:
（I）
wherein n is an integer of 1 to 20, preferably an integer of 5 to 10. The epoxy resin has a special structure, namely 4 functional groups are contained in the epoxy resin, and a material with high crosslinking density and high adhesive force can be obtained after curing.
The bisphenol A-novolac epoxy resin is prepared by reacting bisphenol A, linear chain polyaldehyde and epichlorohydrin.
The invention provides a preparation method of a novel high-adhesion conductive adhesive for a non-main-gate battery component, which comprises the following steps:
the bisphenol A-novolac epoxy resin with the structural general formula I is taken as a base resin, an auxiliary agent is added, the mixture is uniformly dispersed, dendritic micron-sized flaky silver powder and carbon nano tubes are added, and the conductive adhesive is prepared after uniform mixing; wherein, the content of the bisphenol A-novolac epoxy resin accounts for 10 to 20 weight parts; the silver powder accounts for 50-80 parts by weight; 1-5 parts of carbon nano tube and 2-15 parts of auxiliary agent; wherein the auxiliary agent comprises a curing agent, an accelerator, a coupling agent, a reactive diluent, a thixotropic agent and a toughening agent;
in the above technical solution, it is further preferable that the 2 to 15 parts by weight of the assistant comprises 5 to 13 parts by weight of the curing agent, 0.1 to 3 parts by weight of the accelerator, 0.1 to 3 parts by weight of the coupling agent, 0.5 to 3 parts by weight of the reactive diluent, 0.5 to 3 parts by weight of the thixotropic agent, and 0.5 to 3 parts by weight of the toughening agent.
In the above technical solution, it is further preferable that the curing agent is an acid anhydride or imidazole curing agent; methylhexahydrophthalic anhydride is preferred.
With respect to the above technical solution, it is further preferable that the accelerator is an amine accelerator; DMP-30 is preferred.
In the above technical solution, it is further preferable that the silver powder is a flake silver powder, the particle size is 0.1 to 10 μm, and the loose packed density is 0.5 to 4.5g/cm 3 Specific surface area of 0.5-3m 2 (ii) in terms of/g. More preferably, the silver powder has a particle diameter of 2 to 8 μm, a bulk density of 2 to 4g/cm3, and a specific surface area of 1 to 2m 2 /g。
With respect to the above-mentioned technical solutions, it is further preferred that the reactive diluent is a glycidyl ether, preferably 1, 4-butanediol diglycidyl ether.
For the technical solution mentioned above, it is further preferable that the coupling agent is one or a mixture of several of γ -glycidoxypropyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltriethoxysilane, and γ -glycidoxypropylmethyldiethoxysilane;
for the above technical solution, it is further preferable that the toughening agent is carboxyl-terminated liquid nitrile rubber;
with respect to the above-mentioned technical solution, it is further preferred that the thixotropic agent is hydrogenated castor oil and/or polyamide wax;
for the above technical solution, it is further preferable that the carbon nanotube is a multi-walled carbon nanotube, the diameter of the carbon nanotube is 30-60nm, and the length of the carbon nanotube is 5-15 nm.
The application of the high-adhesion conductive adhesive prepared by the method comprises the application of the conductive adhesive in the aspects of a non-main-gate battery component, the technical field of low-temperature LED die bonding, the technical field of chip capacitor end electrodes and the like.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of a novel high-binding-force conductive adhesive for components, which is characterized in that epoxy resin with a specific structure is synthesized and applied to the conductive adhesive, (1) specific functional bisphenol A-novolac epoxy resin is synthesized through a two-step method, and a long carbon chain is introduced into resin molecules to form a new structure, so that the crosslinking density is improved, the curing strength and toughness of the resin are improved, and the binding force and mechanical properties are increased; the connection reliability is guaranteed; (2) in the conductive adhesive prepared from the bisphenol A-novolac epoxy resin, the tensile strength is improved through selection of proper components and component proportions, the filling amount of the silver powder is reduced, and the cost of the conductive adhesive is effectively reduced while the conductivity and the mechanical property are ensured; (3) the laminating process of the perfectly-matched assembly reduces the production process, improves the production efficiency, improves the efficiency and reduces the cost, and provides powerful support for the popularization and the application of the novel assembly.
Detailed Description
The following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments.
In the present invention, percentages and percentages are by mass unless otherwise specifically indicated. Unless otherwise specified, the experimental methods used are conventional methods, and the materials, reagents and the like used are commercially available.
The multi-walled carbon nanotubes selected in the following examples were carbon tubes having a diameter of 40nm and a length of 10 nm;
the silver powder selected in the following examples is dendritic micron-sized flaky silver powder with the particle size of 5 mu m and the loose density of 4g/cm 3 。
Example 1
A preparation method of a novel high-adhesion conductive adhesive for components comprises the following steps:
(1) weighing 11.4g of bisphenol A resin, adding the bisphenol A resin into 25mL of n-butanol, heating to 65 ℃ in continuous mechanical stirring and high-temperature reflux, adding 20mL of glutaraldehyde and 0.25g of 1wt% sodium hydroxide aqueous solution when the bisphenol A is dissolved to be clear, continuing heating to 100 ℃, stirring and carrying out high-temperature reflux reaction for 6 hours, and carrying out reduced pressure fractionation on the obtained product to obtain synthetic phenolic resin;
(2) weighing 6.5g of the phenolic resin obtained in the step (1), adding the phenolic resin into 30mL of epoxy chloropropane, adding 0.15g of tetrabutylammonium bromide, carrying out nitrogen protection, mechanically stirring and heating to 100 ℃, carrying out reflux reaction for 3 hours, then cooling to 60 ℃, adding 25mL of 10wt% sodium hydroxide aqueous solution, then heating to 70 ℃, continuing stirring and refluxing for 1 hour, and carrying out cleaning and reduced pressure distillation to obtain the epoxy resin with the structural formula shown in I, wherein n is 8;
(3) weighing 14 parts by weight of the epoxy resin with the structural formula shown in the formula I obtained in the step (2), 10 parts by weight of methyl hexahydrophthalic anhydride serving as a curing agent, 1 part by weight of DMP-30 serving as an accelerator, 1 part by weight of 1, 4-butanediol diglycidyl ether serving as a diluent, 1 part by weight of gamma-glycidyl ether oxypropyltrimethoxysilane serving as a coupling agent, 1 part by weight of polyamide wax and 1 part by weight of carboxyl-terminated liquid nitrile butadiene rubber serving as a toughening agent, uniformly mixing at normal temperature, adding 70 parts by weight of silver powder and 1 part by weight of multi-walled carbon nano tubes into the epoxy resin, uniformly stirring and mixing the silver powder and the multi-walled carbon nano tubes by a homogenizer and a three-roll mill, and carrying out vacuum defoaming to obtain the conductive adhesive with the silver powder filling amount of 70 wt%.
(4) The curing condition of the conductive adhesive is that the conductive adhesive is cured for 20min at 150 ℃, and the volume resistivity is 3.4 multiplied by 10 -4 Omega cm, shear strength 22.1 MPa.
Example 2
A preparation method of a novel high-adhesion conductive adhesive for components comprises the following steps:
1) weighing 11.4g of bisphenol A resin, adding the bisphenol A resin into 30mL of n-butanol, heating to 65 ℃ in continuous mechanical stirring and high-temperature reflux, adding 20mL of glutaraldehyde and 0.2g of 1wt% sodium hydroxide aqueous solution when the bisphenol A is dissolved to be clear, continuing heating to 100 ℃, stirring and carrying out high-temperature reflux reaction for 6 hours, and carrying out reduced pressure fractionation on the obtained product to obtain synthetic phenolic resin;
(2) weighing 6.5g of the phenolic resin obtained in the step (1), adding the phenolic resin into 30mL of epoxy chloropropane, adding 0.15g of tetrabutylammonium bromide, carrying out nitrogen protection, mechanically stirring and heating to 100 ℃, carrying out reflux reaction for 3 hours, then cooling to 60 ℃, adding 25mL of 10wt% sodium hydroxide aqueous solution, then heating to 70 ℃, continuing stirring and refluxing for 1 hour, and carrying out cleaning and reduced pressure distillation to obtain the epoxy resin with the structural formula shown in I, wherein n is 6;
(3) weighing 10 parts by weight of the epoxy resin with the structural formula shown in the formula I obtained in the step (2), 7.5 parts by weight of methyl hexahydrophthalic anhydride serving as a curing agent, 1 part by weight of DMP-30 serving as an accelerator, 0.5 part by weight of 1, 4-butanediol diglycidyl ether serving as a diluent, 1 part by weight of 2- (3, 4-epoxycyclohexyl) ethyl triethoxysilane serving as a coupling agent, 1 part by weight of polyamide wax and 1 part by weight of carboxyl-terminated butadiene-acrylonitrile butadiene rubber serving as a toughening agent, uniformly mixing at normal temperature, adding 75 parts by weight of silver powder and 3 parts by weight of multi-walled carbon nano tubes into the mixture, fully stirring and uniformly mixing the silver powder and the multi-walled carbon nano tubes by using a homogenizer and a three-roll mill, and carrying out vacuum defoaming to obtain the conductive adhesive with the filling amount of the silver powder of 75 wt%.
(4) The curing condition of the conductive adhesive is that the conductive adhesive is cured for 20min at 150 ℃, and the volume resistivity is 1.2 multiplied by 10 -4 Omega cm, shear strength 19.8 MPa.
Example 3
A preparation method of a novel high-adhesion conductive adhesive for components comprises the following steps:
1) weighing 11.4g of bisphenol A resin, adding the bisphenol A resin into 25mL of n-butanol, heating to 65 ℃ in continuous mechanical stirring and high-temperature reflux, adding 20mL of glutaraldehyde and 0.25g of 1wt% sodium hydroxide aqueous solution when the bisphenol A is dissolved to be clear, continuing heating to 100 ℃, stirring and carrying out high-temperature reflux reaction for 5 hours, and carrying out reduced pressure fractionation on the obtained product to obtain synthetic phenolic resin;
(2) weighing 6.5g of the phenolic resin obtained in the step (1), adding the phenolic resin into 30mL of epoxy chloropropane, adding 0.10g of tetrabutylammonium bromide, carrying out nitrogen protection, mechanically stirring and heating to 100 ℃, carrying out reflux reaction for 3 hours, then cooling to 50 ℃, adding 25mL of 10wt% sodium hydroxide aqueous solution, then heating to 65 ℃, continuing stirring and refluxing for 1 hour, and carrying out cleaning and reduced pressure distillation to obtain the epoxy resin with the structural formula shown in I, wherein n is 7;
(3) weighing 16 parts by weight of the epoxy resin with the structural formula shown in the formula I obtained in the step (2), 12 parts by weight of methyl hexahydrophthalic anhydride serving as a curing agent, 1 part by weight of DMP-30 serving as an accelerator, 0.75 part by weight of 1, 4-butanediol diglycidyl ether serving as a diluent, 0.5 part by weight of gamma-glycidyl ether oxypropyltrimethoxysilane serving as a coupling agent, 0.75 part by weight of 2- (3, 4-epoxycyclohexane) ethyl triethoxysilane, 1 part by weight of polyamide wax and 1 part by weight of carboxyl-terminated liquid butadiene-acrylonitrile rubber serving as a toughening agent, uniformly mixing at normal temperature, adding 65 parts by weight of silver powder and 2 parts by weight of multi-walled carbon nanotubes into the mixture, fully stirring and uniformly mixing the mixture through a homogenizer and a three-roll mill, and carrying out vacuum defoaming to obtain the conductive adhesive with the silver powder content of 65 wt%.
(4) The curing condition of the conductive adhesive is that the conductive adhesive is cured for 20min at 150 ℃, and the volume resistivity is 8 multiplied by 10 -4 Omega cm, shear strength 25.8 MPa.
Example 4
A preparation method of a novel high-adhesion conductive adhesive for components comprises the following steps:
1) weighing 11.4g of bisphenol A resin, adding the bisphenol A resin into 25mL of n-butanol, heating to 65 ℃ in continuous mechanical stirring and high-temperature reflux, adding 20mL of glutaraldehyde and 0.25g of 1wt% sodium hydroxide aqueous solution when the bisphenol A is dissolved to be clear, continuing heating to 95 ℃, stirring and carrying out high-temperature reflux reaction for 6 hours, and carrying out reduced pressure fractionation on the obtained product to obtain synthetic phenolic resin;
(2) weighing 6.5g of the phenolic resin obtained in the step (1), adding the phenolic resin into 30mL of epoxy chloropropane, adding 0.1g of tetrabutylammonium bromide, carrying out nitrogen protection, mechanically stirring and heating to 100 ℃, carrying out reflux reaction for 3 hours, then cooling to 60 ℃, adding 30mL of 10wt% sodium hydroxide aqueous solution, then heating to 75 ℃, continuously stirring and refluxing for 1 hour, and carrying out cleaning and reduced pressure distillation to obtain the epoxy resin with the structural formula shown in I, wherein n is 10;
(3) weighing 13 parts by weight of epoxy resin with the structural formula shown in the formula I obtained in the step (2), 10 parts by weight of curing agent methylhexahydrophthalic anhydride, 1 part by weight of accelerator DMP-30, 2 parts by weight of diluent 1, 4-butanediol diglycidyl ether, 0.5 part by weight of coupling agent gamma-glycidyl ether oxypropyl trimethoxy silane, 0.5 part by weight of polyamide wax and 1 part by weight of toughening agent carboxyl-terminated liquid nitrile rubber, uniformly mixing at normal temperature, adding 70 parts by weight of silver powder and 2 parts by weight of multi-walled carbon nanotubes into the mixture, fully stirring and uniformly mixing the mixture by a homogenizer and a three-roll mill, and defoaming in vacuum to obtain conductive adhesive with the silver powder filling amount of 70 wt%.
(4) The curing condition of the conductive adhesive is that the conductive adhesive is cured for 20min at 150 ℃, and the volume resistivity is 4.2 multiplied by 10 -4 Omega cm, shear strength 20 MPa.
Comparative example 1
Compared with the example 1, the difference is that the component bisphenol A-novolac epoxy resin is changed into bisphenol A epoxy resin E51, and the effect difference is detected as follows: curing at 150 deg.C for 20min to increase volume resistivity to 1.4 × 10 -2 The shear strength is lower than 2.4 MPa.
Comparative example 2
Compared with the example 1, the difference is that the component bisphenol A-novolac epoxy resin is changed into bisphenol A epoxy resin E44, and the effect difference is detected as follows: curing at 150 deg.C for 20min to reduce volume resistivity to 6 × 10 -2 The shear strength is lower than 2.2 MPa.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and those skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (13)
1. A bisphenol A-novolac epoxy resin is characterized in that the structural formula is shown as a general formula I:
I
wherein n is an integer of 1 to 20, preferably an integer of 5 to 10.
2. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 1, wherein the method comprises the following steps: the preparation method comprises the following steps of taking bisphenol A-novolac epoxy resin as basic resin, adding an auxiliary agent, uniformly mixing and dispersing, then adding dendritic micron-sized flaky silver powder and carbon nano tubes, and uniformly mixing to prepare conductive adhesive; wherein, the content of the bisphenol A-novolac epoxy resin accounts for 10-20 parts by weight; the silver powder accounts for 50-80 parts by weight; 1-5 parts of carbon nano tube and 2-15 parts of auxiliary agent; the auxiliary agent comprises a curing agent, an accelerator, a coupling agent, a reactive diluent, a thixotropic agent and a toughening agent.
3. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 2, wherein the method comprises the following steps: in the 2-15 parts by weight of the auxiliary agent, 5-13 parts by weight of curing agent, 0.1-3 parts by weight of accelerator, 0.1-3 parts by weight of coupling agent, 0.5-3 parts by weight of reactive diluent, 0.5-3 parts by weight of thixotropic agent and 0.5-3 parts by weight of toughening agent.
4. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 2, wherein the method comprises the following steps: the curing agent is selected from acid anhydride or imidazole curing agent; methylhexahydrophthalic anhydride is preferred.
5. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 2, wherein the method comprises the following steps: the accelerator is amine accelerator; DMP-30 is preferred.
6. The method for preparing the high-adhesion conductive adhesive for the novel non-main-gate battery assembly according to claim 2, wherein the method comprises the following steps: the silver powder is flake silver powder, the particle size is 0.1-10 mu m, and the apparent density is 0.5-4.5g/cm 3 Specific surface area of 0.5-3m 2 /g。
7. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 6, wherein the method comprises the following steps: the silver powder has a particle size of 2-8 μm, a bulk density of 2-4g/cm3, and a specific surface area of 1-2m 2 /g。
8. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 2, wherein the method comprises the following steps: the reactive diluent is glycidyl ether, preferably 1, 4-butanediol diglycidyl ether.
9. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 2, wherein the method comprises the following steps: the coupling agent is one or a mixture of more of gamma-glycidoxypropyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltriethoxysilane and gamma-glycidoxypropylmethyldiethoxysilane.
10. The method for preparing the high-adhesion conductive adhesive for the novel non-main-gate battery assembly according to claim 2, wherein the method comprises the following steps: the toughening agent is carboxyl-terminated liquid nitrile rubber.
11. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 2, wherein the method comprises the following steps: the thixotropic agent is hydrogenated castor oil and/or polyamide wax.
12. The method for preparing the high-adhesion conductive adhesive for the novel masterless gate battery component as claimed in claim 2, wherein the method comprises the following steps: the carbon nanotube is multi-walled carbon nanotube with diameter of 30-60nm and length of 5-15 nm.
13. The use of the high adhesion conductive adhesive prepared by the method of claim 2, wherein: the application comprises the application of the high-bonding-force conductive adhesive to the technical field of non-main-gate battery components, low-temperature LED die bonding and chip capacitor end electrodes.
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