CN103589379A - Modified conductive glue and preparation method thereof - Google Patents
Modified conductive glue and preparation method thereof Download PDFInfo
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- CN103589379A CN103589379A CN201310506481.9A CN201310506481A CN103589379A CN 103589379 A CN103589379 A CN 103589379A CN 201310506481 A CN201310506481 A CN 201310506481A CN 103589379 A CN103589379 A CN 103589379A
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- conductive resin
- electromagnetic shielding
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- copper powder
- conductive glue
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Abstract
The invention relates to the technical field of conductive glue, is an improvement aiming at the prior art and particularly relates to modified conductive glue and a preparation method thereof. The modified conductive glue comprises the following components: an electromagnetic shielding enhancer, copper powder and other related materials; the electromagnetic shielding enhancer and the copper powder are premixed by adopting a mechanical ball-milling method. Compared with the prior art, the modified conductive glue has the advantages that the electromagnetic shielding performance of the conductive glue is remarkably improved due to the addition of the electromagnetic shielding enhancer; the electromagnetic shielding enhancer and the copper powder are mixed uniformly due to the application of the mechanical ball-milling method. Therefore, the problem that the electromagnetic shielding property of the conductive glue is poor is effectively solved, so that the conductive glue has relatively great industrial application value.
Description
Technical field
The present invention relates to conductive resin technical field, is improvements over the prior art, is specifically related to a kind of modification conductive resin and preparation method thereof.
Background technology
Hyundai electronics assembling with is connected in industry, conductive resin because connect temperature low, without cleaning, be particularly useful for the advantages such as High Density Packaging or ultra fine-pitch assembling, and enjoy industry high praise.Along with the continuous progress of science and technology and improving constantly of people's living standard, industry is also had higher requirement to conductive resin.But often there is the problems such as electromagnetic wave shielding is not good, cost is higher, conductive filler material dispersion is even not in current conductive resin.In order to make conductive resin have larger industrial application value, the electromagnetic wave shielding of conductive resin in the urgent need to address is not good, cost is high, the dispersed problem such as bad.
Because the electric conductivity of copper and silver approach, but cost is well below silver, so cupric powder conductive adhesive has good application prospect.But also there is the shortcomings such as easy reunion, electromagnetic wave shielding be not good in current cupric powder conductive adhesive.
Summary of the invention
A kind of modification conductive resin that the object of the invention is to avoid above-mentioned weak point of the prior art and provide and preparation method thereof.The interpolation of electromagnetic shielding toughener, makes the present invention than prior art, has significantly improved the capability of electromagnetic shielding of conductive resin; The application of mechanical ball milling method, has realized more uniformly electromagnetic shielding toughener and conductive filler material and mixes, improved copper powder dispersiveness, extended storage time of conductive resin.
Object of the present invention can realize by following measure:
A kind of modification conductive resin of the present invention, its ingredient weight percent (%) is:
Thinner 1 ~ 8%,
Solidifying agent 5 ~ 12%,
Promotor 0.01 ~ 0.3%,
Softening agent 0.2 ~ 0.9%,
Electromagnetic shielding toughener 10 ~ 30%,
Copper powder 15 ~ 40%,
All the other are modified epoxy, and each composition weight sum is 100%.
Described thinner be dibutyl ethylene glycol ether, Virahol, methylethylketone, mixed propyl alcohol, Diethylene Glycol butyl ether, in one or more.Its Main Function is that reduction viscosity is easy to use, and improves work-ing life.
Described solidifying agent is diaminodiphenyl-methane, 4,4 '-diamino-3,3 '-diethyl ditane, N-aminoethyl piperazine, 3-aminomethyl-3,5,5-trimethyl cyclohexylamine, 1, one or more in two (aminomethyl) hexanaphthenes of 3-, trimellitic anhydride, tetrahydrotoluene tetracarboxylic dianhydride.Its Main Function is and prepolymer reaction, and generating three-dimensional reticulated structure improves the mechanical property of product.
Described promotor is one or more in 2,2-dithio-bis-benzothiazole, trolamine.Its Main Function is to accelerate curing reaction.
Described softening agent is trimellitic acid nonyl polyhexamethylene, tri trimellitate (2-ethylhexyl) ester, epoxidized vegetable oil, acetylated monoglyceride, hexanaphthene-1, one or more in 2-dicarboxylic acid dinonyl.Its Main Function is the plasticity and toughness that improve after conductive resin solidifies, and improves the shock resistance after conductive resin solidifies.
Described electromagnetic shielding toughener is one or more in amorphous magnesium yttrium binary alloy, non-crystalline state magnalium binary alloy, amorphous magnesium gadolinium binary alloy.Its Main Function is the capability of electromagnetic shielding improving after conductive resin solidifies.
Described modified epoxy is one or more in acrylic modified epoxy resin, polyester modified epoxy resin and modifying epoxy resin by organosilicon.Its Main Function is to provide the required cohesive strength of conductive resin.
The preparation method of the conductive resin of a kind of modification conductive resin of the present invention, comprises following two steps:
(1) pre-mixing of electromagnetic shielding toughener and copper powder: first 10 ~ 30% electromagnetic shielding tougheners and 15 ~ 40% copper powders are put into the high energy ball mill of applying argon gas protection, ratio of grinding media to material is 6 ~ 10:1, rotating speed is 300 revs/min ± 50 revs/min, Ball-milling Time is 6 hours ± 1 hour, obtains the conductive filler material that electromagnetic wave shielding conductive resin is used;
(2) preparation of conductive resin: successively modified epoxy, 1 ~ 8% thinner, 5 ~ 12% solidifying agent, 0.01 ~ 0.3% promotor and 0.2 ~ 0.9% softening agent are added in vacuum planetary mixer and be stirred to evenly, vacuum tightness is that 0.065 ~ 0.085 MPa, rotating speed are 100 revs/min ± 10 revs/min; Then when stirring, slowly add the premixed conductive filler material of step (1), be stirred to evenly; Obtain a kind of modification conductive resin.
The present invention compared to existing technology tool has the following advantages: the interpolation of electromagnetic shielding toughener, and make the present invention than prior art, significantly improved the capability of electromagnetic shielding of conductive resin; The application of mechanical ball milling method, has realized more uniformly electromagnetic shielding toughener and copper powder and mixes.Therefore, the present invention efficiently solves the not good problem of conductive resin electromagnetic wave shielding, makes conductive resin have larger industrial application value.
Embodiment
Embodiment 1: methylethylketone 1%,
4,4 '-diamino-3,3 '-diethyl ditane 12%,
Trolamine 0.01%,
Trimellitic acid nonyl polyhexamethylene 0.2%,
Amorphous magnesium yttrium binary alloy 10%,
Copper powder 15%,
Modifying epoxy resin by organosilicon 61.79%;
Preparation process: the pre-mixing of (1) electromagnetic shielding toughener and copper powder: first 10% amorphous magnesium yttrium binary alloy and 15% copper powder are put into the high energy ball mill of applying argon gas protection, ratio of grinding media to material is 6:1, rotating speed is 300 revs/min, Ball-milling Time is 6 hours, obtains electromagnetic shielding toughener and copper powder after pre-mixing; (2) preparation of conductive resin: successively by 61.79% modifying epoxy resin by organosilicon, 1% methylethylketone, 12% 4,4 '-diamino-3,3 '-diethyl ditane, 0.01% trolamine and 0.2% trimellitic acid nonyl polyhexamethylene add and in vacuum planetary mixer, are stirred to evenly, and vacuum tightness is that 0.075 MPa, rotating speed are 100 revs/min; Then when stirring, slowly add electromagnetic shielding toughener and the copper powder after the pre-mixing of step (1) institute, be stirred to evenly; Obtain a kind of modification conductive resin.
Embodiment 2:
Methylethylketone 3%,
Diethylene Glycol butyl ether 4%,
N-aminoethyl piperazine 6%,
4,4 '-diamino-3,3 '-diethyl ditane 6%
2,2-dithio-bis-benzothiazole 0.15%,
Acetylated monoglyceride 0.5%,
Non-crystalline state magnalium binary alloy 22%,
Copper powder 25%,
Polyester modified epoxy resin 18%,
Acrylic modified epoxy resin 15.35%;
Preparation process: the pre-mixing of (1) electromagnetic shielding toughener and copper powder: first 22% non-crystalline state magnalium binary alloy and 25% copper powder are put into the high energy ball mill of applying argon gas protection, ratio of grinding media to material is 6:1, rotating speed is 300 revs/min, Ball-milling Time is 6 hours, obtains electromagnetic shielding toughener and copper powder after pre-mixing; (2) preparation of conductive resin: successively by 18% polyester modified epoxy resin, 15.35% acrylic modified epoxy resin, 3% methylethylketone, 4% Diethylene Glycol butyl ether, 6%N-aminoethyl piperazine, 6% 4,4 '-diamino-3,3 '-diethyl ditane, 0.15% 2,2-dithio-bis-benzothiazole and 0.5% acetylated monoglyceride join in vacuum planetary mixer and are stirred to evenly, and vacuum tightness is that 0.075 MPa, rotating speed are 100 revs/min; Then when stirring, slowly add electromagnetic shielding toughener and the copper powder after the pre-mixing of step (1) institute, be stirred to evenly; Obtain a kind of modification conductive resin.
Thinner 1 ~ 8%,
Solidifying agent 5 ~ 12%,
Promotor 0.01 ~ 0.3%,
Softening agent 0.2 ~ 0.9%,
Electromagnetic shielding toughener 10 ~ 30%,
Copper powder 15 ~ 40%,
All the other are modified epoxy, and each composition weight sum is 100%.
Embodiment 3:
Diethylene Glycol butyl ether 8%,
Trimellitic anhydride 12%,
2,2-dithio-bis-benzothiazole 0.3%,
Epoxidized vegetable oil 0.9%,
Amorphous magnesium gadolinium binary alloy 30%,
Copper powder 40%,
Polyester modified epoxy resin 9.8%;
Preparation process: the pre-mixing of (1) electromagnetic shielding toughener and copper powder: first 30% amorphous magnesium gadolinium binary alloy and 40% copper powder are put into the high energy ball mill of applying argon gas protection, ratio of grinding media to material is 6:1, rotating speed is 300 revs/min, Ball-milling Time is 6 hours, obtains electromagnetic shielding toughener and copper powder after pre-mixing; (2) preparation of conductive resin: successively by 9.8% polyester modified epoxy resin, 8% Diethylene Glycol butyl ether, 12% trimellitic anhydride, 0.3% 2,2-dithio-bis-benzothiazole and 0.9% epoxidized vegetable oil join in vacuum planetary mixer and are stirred to evenly, and vacuum tightness is that 0.075 MPa, rotating speed are 100 revs/min; Then when stirring, slowly add electromagnetic shielding toughener and the copper powder after the pre-mixing of step (1) institute, be stirred to evenly; Obtain a kind of modification conductive resin.
Table 1 is the salient features Experimental Comparison data of embodiment of the present invention 1-3 and a commercially available conductive resin.
The salient features comparison of test results data of table 1 embodiment 1-3
Claims (8)
1. a modification conductive resin, its ingredient weight percent (%) is:
Thinner 1 ~ 8%,
Solidifying agent 5 ~ 12%,
Promotor 0.01 ~ 0.3%,
Softening agent 0.2 ~ 0.9%,
Electromagnetic shielding toughener 10 ~ 30%,
Copper powder 15 ~ 40%,
All the other are modified epoxy, and each composition weight sum is 100%.
2. a kind of modification conductive resin according to claim 1, is characterized in that: described electromagnetic shielding toughener is one or more in amorphous magnesium yttrium binary alloy, non-crystalline state magnalium binary alloy, amorphous magnesium gadolinium binary alloy.
3. a kind of modification conductive resin according to claim 1, is characterized in that: described thinner be dibutyl ethylene glycol ether, Virahol, methylethylketone, mixed propyl alcohol, Diethylene Glycol butyl ether, in one or more.
4. a kind of modification conductive resin according to claim 1, it is characterized in that: described solidifying agent is diaminodiphenyl-methane, 4,4 '-diamino-3,3 '-diethyl ditane, N-aminoethyl piperazine, 3-aminomethyl-3,5,5-trimethyl cyclohexylamine, 1, one or more in two (aminomethyl) hexanaphthenes of 3-, trimellitic anhydride, tetrahydrotoluene tetracarboxylic dianhydride.
5. a kind of modification conductive resin according to claim 1, is characterized in that: described promotor is one or more in 2,2-dithio-bis-benzothiazole, trolamine.
6. a kind of modification conductive resin according to claim 1, it is characterized in that: described softening agent is trimellitic acid nonyl polyhexamethylene, tri trimellitate (2-ethylhexyl) ester, epoxidized vegetable oil, acetylated monoglyceride, hexanaphthene-1, one or more in 2-dicarboxylic acid dinonyl.
7. a kind of modification conductive resin according to claim 1, is characterized in that: described modified epoxy is one or more in acrylic modified epoxy resin, polyester modified epoxy resin and modifying epoxy resin by organosilicon.
8. the preparation method of a kind of modification conductive resin according to claim 1, it is characterized in that, comprise the steps: the pre-mixing of (1) electromagnetic shielding toughener and copper powder: first 10 ~ 30% electromagnetic shielding tougheners and 15 ~ 40% copper powders are put into the high energy ball mill of applying argon gas protection, ratio of grinding media to material is 6 ~ 10:1, rotating speed is 300 revs/min ± 50 revs/min, Ball-milling Time is 6 hours ± 1 hour, obtains the conductive filler material that electromagnetic wave shielding conductive resin is used; (2) preparation of conductive resin: successively modified epoxy, 1 ~ 8% thinner, 5 ~ 12% solidifying agent, 0.01 ~ 0.3% promotor and 0.2 ~ 0.9% softening agent are added in vacuum planetary mixer and be stirred to evenly, vacuum tightness is that 0.065 ~ 0.085 MPa, rotating speed are 100 revs/min ± 10 revs/min; Then when stirring, slowly add the premixed conductive filler material of step (1), be stirred to evenly; Obtain a kind of modification conductive resin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310506481.9A CN103589379A (en) | 2013-10-24 | 2013-10-24 | Modified conductive glue and preparation method thereof |
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| CN201310506481.9A CN103589379A (en) | 2013-10-24 | 2013-10-24 | Modified conductive glue and preparation method thereof |
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| CN103589379A true CN103589379A (en) | 2014-02-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418391A (en) * | 2017-06-20 | 2017-12-01 | 湖北睿智新材料有限责任公司 | A kind of new formula of conductive powder paint and preparation method thereof |
| CN110093130A (en) * | 2018-01-31 | 2019-08-06 | 上海宝银电子材料有限公司 | A kind of electromagnetic shielding conductive silver glue and preparation method thereof |
-
2013
- 2013-10-24 CN CN201310506481.9A patent/CN103589379A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418391A (en) * | 2017-06-20 | 2017-12-01 | 湖北睿智新材料有限责任公司 | A kind of new formula of conductive powder paint and preparation method thereof |
| CN110093130A (en) * | 2018-01-31 | 2019-08-06 | 上海宝银电子材料有限公司 | A kind of electromagnetic shielding conductive silver glue and preparation method thereof |
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Application publication date: 20140219 |