CN101875831A - Novel nano-copper conductive adhesive and preparation method thereof - Google Patents
Novel nano-copper conductive adhesive and preparation method thereof Download PDFInfo
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- CN101875831A CN101875831A CN2009100501396A CN200910050139A CN101875831A CN 101875831 A CN101875831 A CN 101875831A CN 2009100501396 A CN2009100501396 A CN 2009100501396A CN 200910050139 A CN200910050139 A CN 200910050139A CN 101875831 A CN101875831 A CN 101875831A
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Abstract
The invention relates to a novel nano-copper conductive adhesive and a preparation method thereof. The conductive adhesive comprises the following components in epoxy resin in percentage by weight: 30 to 80 percent of nano-copper, 0.5 to 20 percent of curing agent, 1 to 7 percent of photo-initiator, 0.5 to 2 percent of photo-sensitizer, 0.1 to 2 percent of antioxidant and 5 to 10 percent of protective agent. The preparation method comprises the following steps of: firstly, preparing the nano-copper into slurry according to a formula, and simultaneously, adding the curing agent into the epoxy resin to increase the fluidity of the epoxy resin; secondly, adding the photo-initiator, the photo-sensitizer and the antioxidant together with the thick slurry of the nano-copper into the epoxy resin according to the formula; and finally, performing ultraviolet light polymerization to obtain the nano-copper conductive adhesive. The epoxy group nano-copper conductive adhesive prepared by the method has high electric conductivity, has the advantages of low curing temperature, simple process, adjustable fluidity, low cost and the like, and is suitable for mass production.
Description
Technical field
The invention belongs to adhesive area, particularly cold curing adhesive and preparation method thereof.
Background technology
Along with development of electronic technology, the use face of polymeric substrate is more and more wider.Inorganic Sn-Pb welding material shortcoming is obvious: tie point resolving power is low, and spacing is not suitable for the needs of high density packing greater than 0.65mm, and generally welding temperature is higher than 200 ℃, is much higher than the second-order transition temperature of baseplate material, thus the destructible substrate.Inorganic rigid connects simultaneously, and device work heating is tired easily, reduces the reliability of device; Pb is a heavy metal element, easily contaminate environment.Development of new conductive solder material, particularly conductive resin becomes inexorable trend.
Conductive resin is the matrix material that superpolymer and conductive component are formed, and polymkeric substance provides basic mechanical performance for conductive resin, comprises brute force, toughness, and conductive component improves conductive resin with conductive path, gives the conducting function of conductive resin.Conductive resin has two kinds of curing modes: thermofixation and radiation curing, and general heat curing temperature is at 150 to 180 ℃, and the time is about 30min.Radiation curing utilizes electron beam or UV-light to cause to solidify, and speed is fast, and temperature is low, but consider harmful, so reduce irradiation time as far as possible.
The marketization of at present existing many conductive resin products, but price is extremely expensive, and mostly be elevated temperature heat solidity conductive resin.Domestic few at this area research.Patent 02104074 has been reported a kind of conductive resin of anisotropic, but has been ground owing to electroconductibility derives from powder, so there is skewness in its electroconductibility, and the unsteady shortcoming of performance.
Summary of the invention
The present invention is directed to the problem that exists in the background technology, it is low to have proposed a kind of solidification value, and energy-conserving and environment-protective are cheap, nano-copper conductive adhesive of high conductive suitable high-density microelectronics Packaging and preparation method thereof.This kind novel epoxy base nano-copper conductive adhesive is characterized in that: this kind conductive resin is matrix with Resins, epoxy, contains conductive component nanometer copper and solidifying agent simultaneously, light trigger, photosensitizers, oxidation inhibitor, protective material;
This kind novel epoxy base conductive resin is characterized in that: the viscosity of used Resins, epoxy is 8-200pas, and its content is 20wt%-60wt%;
This kind novel epoxy base nano-copper conductive adhesive is characterized in that: the particle diameter of nanometer copper is 1-500nm, and its content is 40wt%-80wt%;
This kind novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed solidifying agent is the dihydroxy ethyl diethylenetriamine, the methylol diethyl triamine, the hydroxyethyl hexanediamine, the contract low viscosity amine self-vulcanizing agent of its modification of amine (benzene dimethylamine condenses), its content is the 0.5wt%-10wt% of Resins, epoxy;
This kind novel epoxy base nano-copper conductive adhesive is characterized in that: employed light trigger is that thio-phenyl-at least a to oxygen azo-cycle-acetone, rice Chi copper clock of oxygen azo-cycle acetone, two methylamine-4-, its content is the 1wt%-7wt% of Resins, epoxy;
This kind novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed photosensitizer is: at least a in hexichol first copper, the fluorescein, its content is Resins, epoxy 0.5%-2wt%.
This kind novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed oxidation inhibitor is triphenylphosphate, diphenyl phosphate, triphenyl phosphite, the phosphorous acid diphenyl ester, ammonium phosphite, primary ammonium phosphate, triethyl phosphate, oxidation inhibitor 168 (three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester), oxidation inhibitor 618 phosphite antioxidants such as (two (octadecyl) pentaerythritol diphosphites), perhaps four 2[3-(3,5-di-t-butyl 2, the 4-hydroxy phenyl) propionic acid] pentaerythritol ester and β-(3,5-di-t-butyl 2, the 4-hydroxy phenyl) hindered phenol antioxygen such as propionic acid octadecanol ester, perhaps one or more in antioxygen 900 compound antioxidants such as grade
This kind novel epoxy base nano-copper conductive adhesive is characterized in that: employed protective material is an ethylene glycol, a condensed ethandiol ether, and Macrogol 200, at least a in 400,600, its content is the 2wt%-8wt% of Resins, epoxy.
Described novel nano-copper conductive adhesive and preparation method thereof is characterized in that, this method may further comprise the steps:
Nanometer copper is dissolved in the protective material, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 80-90wt%;
By proportioning the low viscosity acid anhydride type curing agent being added low viscosity epoxy resin stirs;
With nanometer copper underflow material, together with oxidation inhibitor, light trigger and photosensitizers join in the Resins, epoxy, are warming up to Procuring below 60 degrees centigrade;
The resin of Procuring is carried out ultra-violet curing to get final product.
Perhaps
Nanometer copper is dissolved in the protective material, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 80-90wt%.
With amine curing agent, together with oxidation inhibitor, light trigger and photosensitizers add low viscosity epoxy resin and stir by proportioning;
With nanometer copper underflow material, join in the Resins, epoxy, be warming up to Procuring below 60 degrees centigrade;
The resin of Procuring is carried out ultra-violet curing to get final product.
Beneficial effect
(1) conductive resin conductivity of the present invention is good, and stable performance can effectively reduce energy consumption, and cheap;
(2) preparation technology of the present invention is simple, is easy to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
30g nanometer copper is dissolved in the protective material 7.5g ethylene glycol, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 80wt%.With stirring in the solidifying agent 6g dihydroxy ethyl diethylenetriamine adding 100g Resins, epoxy, form colourless transparent solution; With nanometer copper underflow material, together with oxidation inhibitor triphenyl phosphite 2g, the two methylamine-4-of light trigger join in the Resins, epoxy oxygen azo-cycle-acetone 1g and photosensitizers 0.25g benzophenone, are warming up to 60 ℃ of Procuring 1.5 hours then;
Then the resin of Procuring being carried out uv irradiating 1min gets final product.
Embodiment 2
40g nanometer copper is dissolved in the protective material 10g ethylene glycol, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 80wt%.With stirring in the solidifying agent 4g dihydroxy ethyl diethylenetriamine adding 100g Resins, epoxy, form colourless transparent solution; With nanometer copper underflow material, together with oxidation inhibitor triphenyl phosphite 2g, the two methylamine-4-of light trigger join in the Resins, epoxy oxygen azo-cycle-acetone 1g and photosensitizers 0.25g benzophenone, are warming up to 50 ℃ of Procuring 2 hours then; Then the resin of Procuring being carried out uv irradiating 1min gets final product.
Embodiment 3
60g nanometer copper is dissolved in the protective material 15g ethylene glycol, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 80wt%.With stirring in the two cyanoethyl diethylenetriamines adding of the solidifying agent 0.4g 100g Resins, epoxy, form colourless transparent solution; With nanometer copper underflow material, together with oxidation inhibitor triphenyl phosphite 2g, the two methylamine-4-of light trigger join in the Resins, epoxy oxygen azo-cycle-acetone 1g and photosensitizers 0.5g benzophenone, are warming up to 50 ℃ of Procuring 3 hours then; Then the resin of Procuring being carried out uv irradiating 1min gets final product.
Embodiment 4
60g nanometer copper is dissolved among the protective material ethylene glycol 15g, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 90wt%.With the two cyanoethyl diethylenetriamines of solidifying agent 0.4g, together with oxidation inhibitor triphenyl phosphite 1.2g, the two methylamine-4-of light trigger form colourless transparent solution to stirring in oxygen azo-cycle-acetone 1g and the photosensitizers 0.5g benzophenone adding 100g Resins, epoxy; With nanometer copper underflow material, join in the Resins, epoxy then, be warming up to 50 ℃ of Procuring 3 hours; Then the resin of Procuring being carried out uv irradiating 1min gets final product.
Embodiment product electroconductibility sees Table 1
Table 1: embodiment product performance table
| Nanometer copper content | Volume specific resistance Ω m | Toughness | |
| Embodiment 1 | ????30％ | ????1.5*10-3 | Fine |
| Embodiment 2 | ????40％ | ????1.0*10-3 | Better |
| Embodiment 3 | ????60％ | ????0.8*10-3 | Generally |
| Embodiment 4 | ????60％ | ????0.7*10-3 | Generally |
Claims (10)
1. novel nano-copper conductive adhesive, it is characterized in that: this kind conductive resin is matrix with Resins, epoxy, contains conductive component nanometer copper and solidifying agent simultaneously, light trigger, photosensitizers, oxidation inhibitor, protective material.
2. according to claim item 1 described a kind of novel epoxy base conductive resin, it is characterized in that: the viscosity of used Resins, epoxy is 8-100pas.
3. according to claim item 1 described a kind of novel epoxy base nano-copper conductive adhesive, it is characterized in that: the particle diameter of nanometer copper is 1-500nm, and its content is the 30wt%-80wt% of Resins, epoxy.
4. according to claim item 1 described a kind of novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed solidifying agent is the dihydroxy ethyl diethylenetriamine, the methylol diethyl triamine, the hydroxyethyl hexanediamine, the contract low viscosity amine self-vulcanizing agent of its modification of amine (benzene dimethylamine condenses), its content is the 0.5wt%-20wt% of Resins, epoxy.
5. according to claim item 1 described a kind of novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed light trigger is a thio-phenyl-at least a to oxygen azo-cycle-acetone, Michler's keton to oxygen azo-cycle acetone, two methylamine-4-, and its content is the 1wt%-7wt% of Resins, epoxy.
6. according to claim item 1 described a kind of novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed photosensitizer is: at least a in two first copper, the fluorescein, its content is 0.5wt%-2wt%.
7. according to claim item 1 described a kind of novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed oxidation inhibitor is triphenylphosphate, diphenyl phosphate, triphenyl phosphite, the phosphorous acid diphenyl ester, ammonium phosphite, primary ammonium phosphate, triethyl phosphate, oxidation inhibitor 168 (three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester), oxidation inhibitor 618 phosphite antioxidants such as (two (octadecyl) pentaerythritol diphosphites), perhaps four 2[3-(3,5-di-t-butyl 2, the 4-hydroxy phenyl) propionic acid] pentaerythritol ester and β-(3,5-di-t-butyl 2, the 4-hydroxy phenyl) hindered phenol antioxygen such as propionic acid octadecanol ester, perhaps oxidation inhibitor 900 compound antioxidants such as grade, its content is the 0.1wt%-2wt% of Resins, epoxy.
8. according to claim item 1 described a kind of novel epoxy base nano-copper conductive adhesive, it is characterized in that: employed protective material is an ethylene glycol, a condensed ethandiol ether, and Macrogol 200, at least a in 400,600, its content is 2wt%-8wt%.
9. a preparation method who prepares novel nano-copper conductive adhesive as claimed in claim 1 is characterized in that, this method may further comprise the steps:
Nanometer copper is dissolved in the protective material, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 80wt%-90wt%;
By proportioning amine curing agent being added low viscosity epoxy resin stirs;
With nanometer copper underflow material, together with oxidation inhibitor, light trigger and photosensitizers join in the Resins, epoxy, are warming up to Procuring below 60 degrees centigrade;
The resin of Procuring is carried out ultra-violet curing to get final product.
10. a preparation method who prepares novel nano-copper conductive adhesive as claimed in claim 1 is characterized in that, this method may further comprise the steps:
Nanometer copper is dissolved in the protective material, stirring at room, formation contains the nanometer copper underflow material that nanometer copper content is 80-90wt%;
With amine curing agent, together with oxidation inhibitor, light trigger and photosensitizers add low viscosity epoxy resin and stir by proportioning;
With nanometer copper underflow material, join in the Resins, epoxy, be warming up to Procuring below 60 degrees centigrade;
The resin of Procuring is carried out ultra-violet curing to get final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100501396A CN101875831A (en) | 2009-04-28 | 2009-04-28 | Novel nano-copper conductive adhesive and preparation method thereof |
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|---|---|---|---|
| CN2009100501396A CN101875831A (en) | 2009-04-28 | 2009-04-28 | Novel nano-copper conductive adhesive and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103106964A (en) * | 2011-11-10 | 2013-05-15 | 袁玉君 | Elastic cable |
| CN103881611A (en) * | 2014-03-10 | 2014-06-25 | 苏州捷德瑞精密机械有限公司 | Normal temperature conductive adhesive and preparation method thereof |
| US8994491B2 (en) | 2012-08-17 | 2015-03-31 | Samsung Electro-Mechanics Co., Ltd. | Chip resistor and method of manufacturing the same |
| CN107663438A (en) * | 2016-07-29 | 2018-02-06 | 余琬琴 | High-adhesion conductive copper colloid and screen printing application method thereof |
-
2009
- 2009-04-28 CN CN2009100501396A patent/CN101875831A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103106964A (en) * | 2011-11-10 | 2013-05-15 | 袁玉君 | Elastic cable |
| WO2013067727A1 (en) * | 2011-11-10 | 2013-05-16 | Yuan Yujun | Elastic cable |
| US8994491B2 (en) | 2012-08-17 | 2015-03-31 | Samsung Electro-Mechanics Co., Ltd. | Chip resistor and method of manufacturing the same |
| TWI506653B (en) * | 2012-08-17 | 2015-11-01 | Samsung Electro Mech | Chip resistor and method of manufacturing the same |
| CN103881611A (en) * | 2014-03-10 | 2014-06-25 | 苏州捷德瑞精密机械有限公司 | Normal temperature conductive adhesive and preparation method thereof |
| CN107663438A (en) * | 2016-07-29 | 2018-02-06 | 余琬琴 | High-adhesion conductive copper colloid and screen printing application method thereof |
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Application publication date: 20101103 |