CN103881611A - Normal temperature conductive adhesive and preparation method thereof - Google Patents
Normal temperature conductive adhesive and preparation method thereof Download PDFInfo
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- CN103881611A CN103881611A CN201410085621.4A CN201410085621A CN103881611A CN 103881611 A CN103881611 A CN 103881611A CN 201410085621 A CN201410085621 A CN 201410085621A CN 103881611 A CN103881611 A CN 103881611A
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Abstract
The invention discloses a normal temperature conductive adhesive and a preparation method thereof. The normal temperature conductive adhesive comprises the following components in parts by weight: 12-16 parts of epoxy resin, 20-30 parts of silver powder, 0.2-0.8 part of carboxyl nitrile rubber, 0.8-2 parts of tricresyl phosphate, 1-5 parts of phenolic resin, 0.5-1 part of polyethylene glycol 20000, 3-8 parts of a diluent, 0.1-0.6 part of hydroxyethyl cellulose, 0.5-1 part of 2-ethyl-4 methylimidazole and 5-10 parts of ethyl acetate. The preparation method comprises the following steps: adding the epoxy resin, the carboxyl nitrile rubber, the tricresyl phosphate, the phenolic resin, the diluent and 2-ethyl-4 methylimidazole into a mixer, stirring to be uniformly mixed, adding ethyl acetate, uniformly mixing, adding other components into the container, uniformly stirring at 60-70 DEG C, cooling to be the room temperature, moving the mixture into a three-roller machine and rolling for three times continuously so as to prepare the normal temperature conductive adhesive.
Description
Technical field
The invention belongs to chemical industry sizing agent preparing technical field, particularly a kind of normal temperature conductive resin and preparation method thereof.
Background technology
Conductive resin be a kind of solidify or dry after there is the sizing agent of certain conductivity, it is that conducting particles is as chief component composition take matrix resin and conductive filler material conventionally, bonding effect by matrix resin combines conducting particles, form conductive path, realize by the conduction of sticky material and connecting.Because the matrix resin of conductive resin is a kind of sizing agent, can select suitable solidification value to carry out bonding, simultaneously, due to the densification of miniaturization, microminiaturization and printed circuit board (PCB) and the developing rapidly of Highgrade integration of electronic component, and conductive resin can be made slurry, realize very high linear resolution.And conductive resin technique is simple, easy handling, can enhance productivity, so conductive resin is to substitute slicker solder welding, realizes the ideal chose that conduction connects.
Can be divided into self-vulcanizing conductive resin, intermediate temperature setting conductive resin, hot setting conductive resin, UV-Curing Electric Conductive Adhesives etc. according to curing system conductive resin.Self-vulcanizing conductive resin is more unstable, and when room temperature storage, volume specific resistance easily changes.When high-temperature electric conduction glue hot setting, metallics is oxidizable, and requirement set time must the shorter requirement that could meet conductive resin.What domestic and international application was more at present is intermediate temperature setting conductive resin (lower than 150 ℃), and its solidification value is moderate, matches with temperature resistant capability and the use temperature of electronic devices and components, and mechanical property is also more excellent, so application is more extensive.UV-Curing Electric Conductive Adhesives combines UV-curing technology and conductive resin, given the performance that conductive resin is new and expanded the range of application of conductive resin.
Normal temperature conductive resin used at present, under normal temperature condition, need the curing time longer, generally more than 5 hours, after solidifying, cohesive strength and shearing resistance are not high enough simultaneously, affect the use range of product, therefore need to develop a kind of can solidifying at short notice and the normal temperature conductive resin of excellent property, meet daily needs.
Summary of the invention
The object of the invention is to provides a kind of normal temperature conductive resin and preparation method thereof in order to overcome above the deficiencies in the prior art.
The present invention realizes by following technique means:
A kind of normal temperature conductive resin, comprise in components by weight percent: epoxy resin 12-16 part, silver powder 20-30 part, carboxy nitrile rubber 0.2-0.8 part, tritolyl phosphate 0.8-2 part, resol 1-5 part, PEG 20000 0.5-1 part, thinner 3-8 part, Natvosol 0.1-0.6 part, 2-ethyl-4 Methylimidazole 0.5-1 part, ethyl acetate 5-10 part.
Described normal temperature conductive resin, be preferably in components by weight percent and comprise: epoxy resin 13-15 part, silver powder 22-26 part, carboxy nitrile rubber 0.4-0.7 part, tritolyl phosphate 1-1.5 part, resol 2-4 part, PEG 20000 0.6-1 part, thinner 4-6 part, Natvosol 0.3-0.5 part, 2-ethyl-4 Methylimidazole 0.6-0.8 part, ethyl acetate 7-9 part.
Above-described normal temperature conductive resin, silver powder is preferably electrolytic silver powder, and particle diameter is 500 orders.
Above-described normal temperature conductive resin, thinner is preferably epoxide diluent No. 600.
The preparation method of the normal temperature conductive resin described in more than one any one, is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 100-120 rev/min, stir 10-20 minute;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 60-70 ℃, stir 15-30 minute, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, rolls continuously roller three times, makes normal temperature conductive resin.
The preparation method of above-described normal temperature conductive resin, in step (5), the roller gap of three-roller is preferably 0.5-1mm.
The preparation method of above-described normal temperature conductive resin, in step (5), the intermediate roll speed of three-roller is preferably 90-100 rev/min.
The preparation method of above-described normal temperature conductive resin, in step (5), the velocity ratio of rear roller, central roll and the preliminary roller of three-roller is preferably 1:2:5.
Normal temperature conductive resin provided by the invention shows that through the performance test results its surface drying time has reached in 2min, when coating bed thickness 1cm, reached in 3h complete set time, resistivity has reached below 60 Ω/cm, more than shearing resistance has reached 20MPa, more than cohesive strength has reached 23MPa.
Embodiment:
Embodiment 1
A kind of normal temperature conductive resin, comprise in components by weight percent: 12 parts of epoxy resin, 500 20 parts of order electrolytic silver powders, 0.2 part of carboxy nitrile rubber, 0.8 part of tritolyl phosphate, 1 part, resol, 0.5 part of PEG 20000,3 parts of No. 600 epoxide diluents, 0.1 part of Natvosol, 0.5 part of 2-ethyl-4 Methylimidazole, 5 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 100 revs/min, stir 10 minutes;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 60 ℃, stir 15 minutes, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, roller gap 0.5mm, intermediate roll speed is preferably 90 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, roll continuously roller three times, make normal temperature conductive resin.
Embodiment 2
A kind of normal temperature conductive resin, comprise in components by weight percent: 13 parts of epoxy resin, 500 22 parts of order electrolytic silver powders, 0.4 part of carboxy nitrile rubber, 1 part of tritolyl phosphate, 2 parts, resol, 0.6 part of PEG 20000,4 parts of No. 600 epoxide diluents, 0.3 part of Natvosol, 0.6 part of 2-ethyl-4 Methylimidazole, 7 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 110 revs/min, stir 15 minutes;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 65 ℃, stir 20 minutes, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, roller gap 0.6mm, intermediate roll speed is preferably 95 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, roll continuously roller three times, make normal temperature conductive resin.
Embodiment 3
A kind of normal temperature conductive resin, comprise in components by weight percent: 14 parts of epoxy resin, 500 25 parts of order electrolytic silver powders, 0.5 part of carboxy nitrile rubber, 1.2 parts of tritolyl phosphates, 3 parts, resol, 0.8 part of PEG 20000,5 parts of No. 600 epoxide diluents, 0.4 part of Natvosol, 0.7 part of 2-ethyl-4 Methylimidazole, 8 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 110 revs/min, stir 20 minutes;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 68 ℃, stir 18 minutes, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, roller gap 0.7mm, intermediate roll speed is preferably 98 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, roll continuously roller three times, make normal temperature conductive resin.
Embodiment 4
A kind of normal temperature conductive resin, comprise in components by weight percent: 15 parts of epoxy resin, 500 26 parts of order electrolytic silver powders, 0.7 part of carboxy nitrile rubber, 1.5 parts of tritolyl phosphates, 4 parts, resol, 1 part of PEG 20000,6 parts of No. 600 epoxide diluents, 0.5 part of Natvosol, 0.8 part of 2-ethyl-4 Methylimidazole, 9 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 120 revs/min, stir 20 minutes;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 70 ℃, stir 25 minutes, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, roller gap 0.6mm, intermediate roll speed is preferably 95 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, roll continuously roller three times, make normal temperature conductive resin.
Embodiment 5
A kind of normal temperature conductive resin, comprise in components by weight percent: 16 parts of epoxy resin, 500 28 parts of order electrolytic silver powders, 0.7 part of carboxy nitrile rubber, 1.8 parts of tritolyl phosphates, 5 parts, resol, 1 part of PEG 20000,7 parts of No. 600 epoxide diluents, 0.5 part of Natvosol, 0.8 part of 2-ethyl-4 Methylimidazole, 9 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 120 revs/min, stir 18 minutes;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 70 ℃, stir 30 minutes, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, roller gap 0.8mm, intermediate roll speed is preferably 100 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, roll continuously roller three times, make normal temperature conductive resin.
Embodiment 6
A kind of normal temperature conductive resin, comprise in components by weight percent: 16 parts of epoxy resin, 500 30 parts of order electrolytic silver powders, 0.8 part of carboxy nitrile rubber, 2 parts of tritolyl phosphates, 5 parts, resol, 1 part of PEG 20000,8 parts of No. 600 epoxide diluents, 0.6 part of Natvosol, 1 part of 2-ethyl-4 Methylimidazole, 10 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 120 revs/min, stir 20 minutes;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 70 ℃, stir 30 minutes, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, roller gap 1mm, intermediate roll speed is preferably 100 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, roll continuously roller three times, make normal temperature conductive resin.
Comparative example 1
A kind of normal temperature conductive resin, comprise in components by weight percent: 15 parts of epoxy resin, 26 parts, silver powder, 0.7 part of carboxy nitrile rubber, 1.5 parts of tritolyl phosphates, 4 parts, resol, 1 part of PEG 20000,6 parts of No. 600 epoxide diluents, 0.5 part of Natvosol, 0.8 part of 2-ethyl-4 Methylimidazole, 9 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 120 revs/min, stir 20 minutes;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 70 ℃, stir 25 minutes, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, roller gap 0.6mm, intermediate roll speed is preferably 95 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, roll continuously roller three times, make normal temperature conductive resin.
Comparative example 2
A kind of normal temperature conductive resin, comprise in components by weight percent: 15 parts of epoxy resin, 500 26 parts of order electrolytic silver powders, 0.7 part of carboxy nitrile rubber, 1.5 parts of tritolyl phosphates, 4 parts, resol, 1 part of PEG 20000,6 parts of No. 600 epoxide diluents, 0.5 part of Natvosol, 0.8 part of 2-ethyl-4 Methylimidazole, 9 parts of ethyl acetate.
Above-described normal temperature conductive resin is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 120 revs/min, stir 20 minutes;
(3) ethyl acetate, PEG 20000, Natvosol and silver powder are joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) mixture step (3) being obtained moves in three-roller, roller gap 0.6mm, and intermediate roll speed is preferably 95 revs/min, and the velocity ratio of rear roller, central roll and preliminary roller is preferably 1:2:5, rolls continuously roller three times, makes normal temperature conductive resin.
The normal temperature conductive resin that above embodiment and comparative example are prepared carries out performance test at 25 ℃ of room temperatures, and result is as follows:
Project | Surface drying time min | Completely set time h(bed thickness 1cm) | Resistivity (Ω/cm) | Shearing resistance MPa | Cohesive strength MPa |
Embodiment 1 | 2 | 3 | 60 | 20 | 23 |
Embodiment 2 | 2 | 3 | 55 | 22 | 23 |
Embodiment 3 | 1 | 2 | 50 | 25 | 25 |
Embodiment 4 | 1 | 1.5 | 50 | 23 | 26 |
Embodiment 5 | 1 | 1 | 50 | 22 | 25 |
Embodiment 6 | 1 | 1.5 | 55 | 21 | 24 |
Comparative example 1 | 1 | 5 | 110 | 23 | 20 |
Comparative example 2 | 2 | 7 | 90 | 15 | 17 |
As can be seen from the above data, add the conductive resin resistivity preparing after 500 order electrolytic silver powders and be significantly less than the conductive resin that general silver powder obtains, the data that obtain from comparative example 2 can be found out simultaneously, by PEG 20000, the conductive resin that Natvosol and silver powder obtain after being directly uniformly mixed is far longer than PEG 20000 under the same conditions completely set time, Natvosol and silver powder are heated to the conductive resin obtaining after 70 ℃ of stir process, electric conductivity is also greater than the latter simultaneously, its reason may be that silver powder has obtained activation after heat treated, can bring into play better electric action, PEG 20000 simultaneously, Natvosol and silver powder have formed mixture, mixture is at the cooling rear loose cavernous structure that produced, the normal temperature conductive resin finally obtaining is more easily solidified, after solidifying, form very strong gluing body, strengthen gluing performance.
Claims (8)
1. a normal temperature conductive resin, it is characterized in that, comprise in components by weight percent: epoxy resin 12-16 part, silver powder 20-30 part, carboxy nitrile rubber 0.2-0.8 part, tritolyl phosphate 0.8-2 part, resol 1-5 part, PEG 20000 0.5-1 part, thinner 3-8 part, Natvosol 0.1-0.6 part, 2-ethyl-4 Methylimidazole 0.5-1 part, ethyl acetate 5-10 part.
2. normal temperature conductive resin according to claim 1, it is characterized in that, comprise in components by weight percent: epoxy resin 13-15 part, silver powder 22-26 part, carboxy nitrile rubber 0.4-0.7 part, tritolyl phosphate 1-1.5 part, resol 2-4 part, PEG 20000 0.6-1 part, thinner 4-6 part, Natvosol 0.3-0.5 part, 2-ethyl-4 Methylimidazole 0.6-0.8 part, ethyl acetate 7-9 part.
3. normal temperature conductive resin according to claim 1 and 2, is characterized in that, silver powder is electrolytic silver powder, and particle diameter is 500 orders.
4. normal temperature conductive resin according to claim 1 and 2, is characterized in that, thinner is No. 600 epoxide diluents.
5. a preparation method for the normal temperature conductive resin described in claim 1-4 any one, is characterized in that, is prepared according to following steps:
(1) take each component according to weight part;
(2) epoxy resin, carboxy nitrile rubber, tritolyl phosphate, resol, thinner, 2-ethyl-4 Methylimidazole are joined in mixing tank, under the condition of 100-120 rev/min, stir 10-20 minute;
(3) ethyl acetate is joined in the mixture after step (2) stirs, continue to be uniformly mixed;
(4) PEG 20000, Natvosol and silver powder are joined in container, be heated to 60-70 ℃, stir 15-30 minute, be down to room temperature;
(5) mixture step (4) being obtained joins in step (3), is uniformly mixed, and moves in three-roller, rolls continuously roller three times, makes normal temperature conductive resin.
6. the preparation method of normal temperature conductive resin according to claim 5, is characterized in that, in step (5), the roller gap of three-roller is 0.5-1mm.
7. the preparation method of normal temperature conductive resin according to claim 5, is characterized in that, in step (5), the intermediate roll speed of three-roller is 90-100 rev/min.
8. the preparation method of normal temperature conductive resin according to claim 5, is characterized in that, in step (5), the velocity ratio of rear roller, central roll and the preliminary roller of three-roller is 1:2:5.
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CN104531028A (en) * | 2015-01-24 | 2015-04-22 | 李�杰 | Preparation method of modified epoxy resin adhesive for adhesion of silicon rubber and metal |
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CN105405487A (en) * | 2014-08-29 | 2016-03-16 | 比亚迪股份有限公司 | Conductive silver paste, preparation method therefor, conductive circuit, and preparation method for conductive circuit |
CN105694161A (en) * | 2016-03-22 | 2016-06-22 | 苏州捷德瑞精密机械有限公司 | Metal particle conductive composite material and preparation method of metal particle conductive composite material |
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