CN117887394A - High-dispersity anisotropic conductive adhesive film and preparation method thereof - Google Patents
High-dispersity anisotropic conductive adhesive film and preparation method thereof Download PDFInfo
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- 239000002313 adhesive film Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 86
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 13
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000003607 modifier Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000012459 cleaning agent Substances 0.000 claims description 4
- -1 filtering Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 73
- 230000000052 comparative effect Effects 0.000 description 10
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 7
- IYGAMTQMILRCCI-UHFFFAOYSA-N 3-aminopropane-1-thiol Chemical compound NCCCS IYGAMTQMILRCCI-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- SSDNOCNXOSFLRY-UHFFFAOYSA-N 3-methylthiophene-2-thiol Chemical compound CC=1C=CSC=1S SSDNOCNXOSFLRY-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 235000010384 tocopherol Nutrition 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
Abstract
The invention belongs to the technical field of conductive adhesive films, and particularly relates to a highly-dispersible anisotropic conductive adhesive film and a preparation method thereof. The high-dispersibility anisotropic conductive adhesive film comprises the following components in parts by weight: 20-40 parts of epoxy resin, 15-30 parts of nitrile rubber, 20-30 parts of silicon dioxide, 3-10 parts of curing agent and 10 parts of modified Ni powder; the preparation method of the modified Ni powder comprises dispersing the cleaned Ni powder in a modifier for mixing reaction, centrifuging, and drying at normal temperature under reduced pressure. The modified Ni powder is used as conductive particles, which is beneficial to improving the uniformity of the anisotropic conductive adhesive film system, thereby improving the comprehensive performance of the anisotropic conductive adhesive film.
Description
Technical Field
The invention belongs to the technical field of conductive adhesive films, and particularly relates to a highly-dispersible anisotropic conductive adhesive film and a preparation method thereof.
Background
Anisotropic Conductive Film (ACF) is a mainstream electronic packaging material at present, and generally refers to a polymer film including metal particles (nickel (Ni), copper (Cu), gold (Au), etc.) or metal-coated polymer particles as conductive particles, and is widely used for electrical connection of LCD panels, printed Circuit Boards (PCBs), and tape carrier packages (tape carrierpackages, TCPs).
The anisotropic conductive adhesive film is positioned between the circuits, and after being heated and pressurized under specific conditions, the circuit terminals are electrically connected through conductive particles, and the electrodes between the IC chip and the substrate are connected by the conductive particles to form vertical conduction, and meanwhile, the conduction between the adjacent two electrodes (in the horizontal direction) can be avoided, so that the purpose of conducting only in the vertical direction is achieved.
The conductive particles are the core of the ACF for conducting, and the conducting property mainly depends on the resistivity, filling rate and distribution of the conductive particles. As a conductive filler which is inexpensive and excellent in comprehensive properties, ni powder is widely used in ACF industry. However, ni powder is relatively hydrophilic as a whole and has a large surface area, which increases the difficulty of dispersion in ACF matrix resin (organic phase) to some extent.
Disclosure of Invention
The invention aims at solving the technical problems and provides a highly-dispersible anisotropic conductive adhesive film, which improves the dispersibility of Ni powder in an anisotropic conductive adhesive film system by modifying Ni powder through forming coordination compound bonds on the surface of the Ni powder.
The high-dispersity anisotropic conductive adhesive film in the technical scheme of the invention comprises the following components in parts by weight: 20-40 parts of epoxy resin, 15-30 parts of nitrile rubber, 20-30 parts of silicon dioxide, 3-10 parts of curing agent and 10 parts of modified Ni powder.
Further, the particle size of the silica is 50 to 500nm.
Preferably, the curing agent includes, but is not limited to, one or more of imidazole, isocyanate, amine, amide, phenolic, anhydride curing agents.
Further, the preparation method of the modified Ni powder comprises the steps of dispersing the cleaned Ni powder in a modifier for mixing reaction, centrifuging, and drying at normal temperature under reduced pressure.
Covalent bonds and action-coordination bonds are formed on the surface of the micron-sized Ni powder with larger surface area through the organic modifier, so as to carry out surface modification on the Ni powder. Compared with the traditional simple modification means that Ni powder is simply blended in an organic reagent and then centrifugally separated, or Ni powder and a modifier are coated together in a dry/wet way, the coordination bond is a special covalent bond formed by sharing an empty orbit based on metal and an electron pair of an organic molecule, and the bond energy is larger than the secondary valence bond such as Van der Waals force. Therefore, the organic molecules combined on the surface of the Ni powder through coordination bonds are more stable and efficient than those combined by blending/physical coating, so that the dispersing capability of the Ni powder in the anisotropic conductive adhesive film system can be greatly improved, and the uniformity of the anisotropic conductive adhesive film system is further improved.
Further, the Ni powder has a particle diameter of 10 to 100 μm.
Further, during the cleaning of the Ni powder, the Ni powder is dispersed in the cleaning agent and stirred and cleaned for 20 to 60 minutes.
Further, the rotational speed during stirring and cleaning is 300-500 rpm/min.
Further, the cleaning agent is one or more of water, ethanol, ethyl acetate, dilute hydrochloric acid, phosphoric acid, acetone, butanone, toluene and ethylene glycol butyl ether.
Further, the Ni powder is centrifuged for 10 to 30 minutes at 8000 to 10000rpm/min after being cleaned.
Further, the modifier structure contains one or more of mercapto, carboxyl and amino. The modifier may be one or more of 3-mercapto-1-propylamine, 3-methylthiophene-2-thiol, dodecanoic acid, octadecanoic acid, oleic acid, and 1, 12-dodecylamine.
The mercapto group, the oxygen atom in the carboxyl and the nitrogen atom in the amino can form good coordination with the surface of Ni powder, and the organic group is introduced into the surface of Ni powder to promote the Ni powder to be uniformly dispersed in the anisotropic conductive adhesive film system, so that the ACF with excellent performance is obtained.
Further, the raw material components of the high-dispersity anisotropic conductive adhesive film also comprise 5-15 parts of solvent.
Further, the solvent includes, but is not limited to, one or more of ethanol, acetone, dimethylsulfoxide, N-methylpyrrolidone, N-dimethylformamide.
Further, the temperature of the mixing reaction is 20-50 ℃ and the time is 1-12 h.
Further, the rotational speed is 8000-10000 rpm/min and the time is 10-30 min during centrifugation.
Further, the thickness of the highly-dispersible anisotropic conductive film is 20-50 μm.
The invention also provides a preparation method of the high-dispersity anisotropic conductive adhesive film, which comprises the steps of mixing epoxy resin, nitrile rubber, silicon dioxide, a curing agent, modified Ni powder and a solvent, filtering, coating and drying.
Further, the drying temperature is 60-90 ℃ and the drying time is 6-10 h.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) The modified Ni powder is used as conductive particles, which is beneficial to improving the uniformity of the anisotropic conductive adhesive film system, thereby improving the comprehensive performance of the anisotropic conductive adhesive film;
(2) The Ni powder is modified by forming coordination compound bonds on the surface of the Ni powder, so that the dispersing capability of the Ni powder in an anisotropic conductive film system is greatly improved;
(3) The nitrogen atoms in pyridine and amino and the oxygen atoms in carboxyl in the modifier can form good coordination with the surface of Ni powder, and organic groups are introduced into the surface of Ni powder to promote the uniform dispersion of Ni powder in the anisotropic conductive adhesive film system;
(4) The method for improving the uniformity of the anisotropic conductive film system is simple and effective and has low cost.
Detailed Description
The technical scheme of the present invention will be further described by the following specific examples, and it should be understood that the specific examples described herein are only for aiding in understanding the present invention, and are not intended to be limiting. Unless otherwise indicated, all materials used in the examples of the present invention are those commonly used in the art, and all methods used in the examples are those commonly used in the art.
Example 1
The preparation method of the high-dispersity anisotropic conductive film comprises the following steps:
(1) Sequentially dispersing Ni powder in water and ethanol, stirring and cleaning at 300rpm/min for 15min respectively, centrifuging at 8000rpm/min for 10min to obtain cleaned Ni powder, dispersing in 3-mercapto-1-propylamine, mixing and stirring at 30 ℃ for 5h, centrifuging at 8000rpm/min for 10min, and decompressing at normal temperature to obtain modified Ni powder;
(2) Mixing 25 parts of epoxy resin, 25 parts of nitrile rubber, 25 parts of silicon dioxide, 5 parts of diethylenetriamine, 10 parts of modified Ni powder and 10 parts of acetone uniformly, filtering, coating, and baking at 80 ℃ for 8 hours to obtain the high-dispersibility anisotropic conductive adhesive film with the thickness of 30 mu m.
Example 2
The preparation method of the high-dispersity anisotropic conductive film comprises the following steps:
(1) Sequentially dispersing Ni powder in dilute hydrochloric acid and ethanol, stirring and cleaning at 350rpm/min for 15min respectively, centrifuging at 8500rpm/min for 10min to obtain cleaned Ni powder, dispersing in 3-mercapto-1-propylamine, mixing and stirring at 35 ℃ for 5h, centrifuging at 9000rpm/min for 10min, centrifuging at normal temperature, and drying under reduced pressure to obtain modified Ni powder;
(2) Mixing 30 parts of epoxy resin, 20 parts of nitrile rubber, 28 parts of silicon dioxide, 6 parts of diethylenetriamine, 12 parts of modified Ni powder and 12 parts of acetone uniformly, filtering, coating, and baking at 85 ℃ for 8 hours to obtain the high-dispersibility anisotropic conductive adhesive film with the thickness of 30 mu m.
Example 3
The preparation method of the high-dispersity anisotropic conductive film comprises the following steps:
(1) Sequentially dispersing Ni powder in ethyl acetate and acetone, stirring and cleaning at 400rpm/min for 15min respectively, centrifuging at 9000rpm/min for 10min to obtain cleaned Ni powder, dispersing in 3-mercapto-1-propylamine, mixing and stirring at 45 ℃ for 5h, centrifuging at 8500rpm/min for 10min, and drying at normal temperature under reduced pressure to obtain modified Ni powder;
(2) Mixing 35 parts of epoxy resin, 28 parts of nitrile rubber, 20 parts of silicon dioxide, 8 parts of maleic anhydride, 8 parts of modified Ni powder and 15 parts of acetone uniformly, filtering, coating, and baking at 90 ℃ for 8 hours to obtain the high-dispersibility anisotropic conductive adhesive film with the thickness of 30 mu m.
Example 4
The difference between this example and example 1 is only that in step (1), ni powder is firstly dispersed in water and ethanol in sequence, and is respectively stirred and washed at 300rpm/min for 15min, and is centrifuged at 8000rpm/min for 10min to obtain washed Ni powder, and then dispersed in 1, 12-dodecylamine, and mixed and stirred at 30 ℃ for 5h, and centrifuged at 8000rpm/min for 10min, and then dried under reduced pressure at normal temperature to obtain modified Ni powder.
Example 5
The difference between this example and example 1 is only that in step (1), ni powder is firstly dispersed in water and ethanol in sequence, and is respectively stirred and washed at 300rpm/min for 15min, and is centrifuged at 8000rpm/min for 10min to obtain washed Ni powder, and then dispersed in dodecanoic acid, mixed and stirred at 30 ℃ for 5h, and centrifuged at 8000rpm/min for 10min, and then dried under reduced pressure at normal temperature to obtain modified Ni powder.
Example 6
The difference between this example and example 1 is only that in step (1), ni powder is firstly dispersed in water and ethanol in sequence, and is respectively stirred and washed at 300rpm/min for 15min, and is centrifuged at 8000rpm/min for 10min to obtain washed Ni powder, and then dispersed in sodium dodecyl benzene sulfonate, and mixed and stirred at 30 ℃ for 5h, and is centrifuged at 8000rpm/min for 10min, and then dried under reduced pressure at normal temperature to obtain modified Ni powder.
Example 7
The difference between this example and example 1 is only that in step (1), ni powder is first dispersed in water and ethanol in sequence, and is washed by stirring at 300rpm/min for 15min, and washed Ni powder is obtained by centrifugation at 8000rpm/min for 10min, and then dispersed in aromatic alkyl oxy ether, mixed and stirred at 30 ℃ for 5h, and centrifuged at 8000rpm/min for 10min, and then dried under reduced pressure at room temperature to obtain modified Ni powder.
Example 8
The difference between this example and example 1 is that in the step (2), 25 parts of epoxy resin, 25 parts of nitrile rubber, 25 parts of silicon dioxide, 5 parts of diethylenetriamine, 10 parts of modified Ni powder and 10 parts of acetone are uniformly mixed, filtered, coated and baked at 80 ℃ for 8 hours to obtain the highly-dispersible anisotropic conductive adhesive film with the thickness of 40 μm.
Example 9
The difference between this example and example 1 is that in the step (2), 25 parts of epoxy resin, 25 parts of nitrile rubber, 25 parts of silicon dioxide, 5 parts of diethylenetriamine, 10 parts of modified Ni powder and 10 parts of acetone are uniformly mixed, filtered, coated and baked at 80 ℃ for 8 hours to obtain the highly-dispersible anisotropic conductive adhesive film with the thickness of 50 μm.
Comparative example 1
The preparation method of the anisotropic conductive adhesive film of the comparative example comprises the following steps:
(1) Dispersing Ni powder in water and ethanol in turn, stirring and cleaning for 15min at 300rpm/min respectively, and centrifuging for 10min at 8000rpm/min to obtain cleaned Ni powder;
(2) Mixing 25 parts of epoxy resin, 25 parts of nitrile rubber, 25 parts of silicon dioxide, 5 parts of diethylenetriamine, 10 parts of Ni powder and 10 parts of acetone uniformly, filtering, coating, and baking at 80 ℃ for 8 hours to obtain the anisotropic conductive adhesive film with the thickness of 30 mu m.
Comparative example 2
The preparation method of the anisotropic conductive adhesive film of the comparative example comprises the following steps:
(1) Sequentially dispersing Ni powder in water and ethanol, stirring and cleaning at 300rpm/min for 15min respectively, centrifuging at 8000rpm/min for 10min to obtain cleaned Ni powder, dispersing in 3-mercapto-1-propylamine, mixing and stirring at 30 ℃ for 5h, centrifuging at 8000rpm/min for 10min, and decompressing at normal temperature to obtain modified Ni powder;
(2) Mixing 25 parts of epoxy resin, 25 parts of nitrile rubber, 25 parts of silicon dioxide, 5 parts of diethylenetriamine, 2 parts of modified Ni powder and 10 parts of acetone uniformly, filtering, coating, and baking at 80 ℃ for 8 hours to obtain the anisotropic conductive adhesive film with the thickness of 30 mu m.
Comparative example 3
The preparation method of the anisotropic conductive adhesive film of the comparative example comprises the following steps:
(1) Sequentially dispersing Ni powder in water and ethanol, stirring and cleaning at 300rpm/min for 15min respectively, centrifuging at 8000rpm/min for 10min to obtain cleaned Ni powder, dispersing in 3-mercapto-1-propylamine, mixing and stirring at 30 ℃ for 5h, centrifuging at 8000rpm/min for 10min, and decompressing at normal temperature to obtain modified Ni powder;
(2) Mixing 25 parts of epoxy resin, 25 parts of nitrile rubber, 25 parts of silicon dioxide, 5 parts of diethylenetriamine, 20 parts of modified Ni powder and 10 parts of acetone uniformly, filtering, coating, and baking at 80 ℃ for 8 hours to obtain the anisotropic conductive adhesive film with the thickness of 30 mu m.
The anisotropic conductive film prepared in the above examples and comparative examples was characterized in that the difficulty in dispersing Ni powder was represented by the apparent dispersion time of Ni powder (the time for which Ni powder was uniformly dispersed by stirring in the system), the dispersion of modified Ni powder was represented by aggregation of conductive balls (the maximum diameter of agglomerated particles in one view was observed with a stereomicroscope, 10 points were randomly tested in each sample, the maximum value was taken to represent the aggregation of conductive balls), and the performance test was performed after manual striping, and the test results were shown in table 1.
TABLE 1 Performance data sheet for anisotropic conductive films
The anisotropic conductive film systems obtained in examples 1 to 5 and examples 8 to 9 were uniform and exhibited excellent overall properties; examples 6-7 use conventional surfactants to modify Ni powder, and have no strong interaction force between organics and Ni powder, so Ni powder has strong hydrophilicity, weak lipophilicity, long apparent dispersion time, serious aggregation and larger volume resistivity; the Ni powder in comparative example 1 is not modified, is difficult to disperse, has high system resistivity, and belongs to a defective product; the modified Ni powder in the anisotropic conductive adhesive film of comparative example 2 is too small in dosage and easy to disperse, but is insufficient in conductivity, so that the usability of the ACF is affected; the modified Ni powder in the anisotropic conductive film of comparative example 3 is too much in amount, which does not affect dispersion, but the short circuit of the device is easily caused due to the too much amount of conductive filler; in addition, the cost is obviously increased, and the actual production is not facilitated.
Finally, it should be noted that the specific embodiments described herein are merely illustrative of the spirit of the invention and are not limiting of the invention's embodiments. Those skilled in the art to which the invention pertains may make various modifications or additions to the described embodiments or may be substituted in a similar manner, without and without all of the embodiments herein being fully understood. While these obvious variations and modifications, which come within the spirit of the invention, are within the scope of the invention, they are to be construed as being without departing from the spirit of the invention.
Claims (10)
1. The high-dispersibility anisotropic conductive adhesive film is characterized by comprising the following components in parts by weight: 20-40 parts of epoxy resin, 15-30 parts of nitrile rubber, 20-30 parts of silicon dioxide, 3-10 parts of curing agent and 5-15 parts of modified Ni powder.
2. The highly dispersible anisotropic conductive film according to claim 1, wherein the silica has a particle size of 50 to 500nm.
3. The highly dispersible anisotropic conductive film according to claim 1, wherein the preparation method of the modified Ni powder comprises dispersing the washed Ni powder in a modifier, mixing and reacting, centrifuging, and drying under reduced pressure at room temperature.
4. The highly dispersible anisotropic conductive film as claimed in claim 3, wherein the Ni powder has a particle size of 10 to 100. Mu.m.
5. The highly dispersible anisotropic conductive film as claimed in claim 3, wherein the Ni powder is dispersed in the cleaning agent during the cleaning, and the cleaning is performed for 20 to 60 minutes with stirring.
6. The highly dispersible anisotropic conductive film according to claim 5, wherein the cleaning agent is one or more of water, ethanol, ethyl acetate, dilute hydrochloric acid, phosphoric acid, acetone, butanone, toluene, and ethylene glycol butyl ether.
7. The anisotropic conductive film of claim 3, wherein the modifier structure contains one or more of mercapto groups, carboxyl groups, and amino groups.
8. The highly dispersible anisotropic conductive film according to claim 3, wherein the temperature of the mixing reaction is 20 to 50 ℃ for 1 to 12 hours.
9. The highly dispersible anisotropic conductive film according to claim 1, wherein the thickness of the highly dispersible anisotropic conductive film is 20 to 50 μm.
10. The method for preparing the highly dispersible anisotropic conductive film according to claim 1, wherein the method comprises mixing epoxy resin, nitrile rubber, silica, curing agent and modified Ni powder, filtering, coating and drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311591462.0A CN117887394A (en) | 2023-11-27 | 2023-11-27 | High-dispersity anisotropic conductive adhesive film and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311591462.0A CN117887394A (en) | 2023-11-27 | 2023-11-27 | High-dispersity anisotropic conductive adhesive film and preparation method thereof |
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