CN102010685B - Epoxy resin conductive adhesive and preparation method thereof - Google Patents
Epoxy resin conductive adhesive and preparation method thereof Download PDFInfo
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- CN102010685B CN102010685B CN 201010572271 CN201010572271A CN102010685B CN 102010685 B CN102010685 B CN 102010685B CN 201010572271 CN201010572271 CN 201010572271 CN 201010572271 A CN201010572271 A CN 201010572271A CN 102010685 B CN102010685 B CN 102010685B
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Abstract
The invention relates to an epoxy resin conductive adhesive and a preparation method thereof. The epoxy resin conductive adhesive comprises the following raw materials by weight percent: 40%-60% of epoxy resin, 2%-10% of reaction diluent, 3%-7% of curing agent, 1%-3% of accelerant, 0.5%-1.5% of coupling agent and 20%-40% of flake silver powder modified by graphene. Based on high conductive performance of the graphene, the prepared epoxy resin conductive adhesive has high conductive performance under the established process conditions, and is particularly suitable for conductive packaging and adhesion of high-end fine electronic and electrical components.
Description
Technical field
The present invention relates to a kind of tackiness agent and preparation method thereof, relate in particular to a kind of epoxy resin conductive adhesive and preparation method thereof.
Background technology
Along with developing rapidly of semiconductor integrated circuit package industry, occupied the principal status of public economy of domestic IC industry, the problem of How to choose electronic package material seems more important.According to data, most of unicircuit all will use the die bonding material, and epoxy resin conductive adhesive is modal binder materials.
The appearance of Graphene has caused global research boom.It is the outstanding material of present known conductive performance, and this makes it also have huge application potential at microelectronic.Graphene-structured is highly stable, and this stable crystalline network makes carbon atom have outstanding electroconductibility, and wherein the movement velocity of electronics has reached 1/300 of the light velocity, considerably beyond the movement velocity of electronics in general conductor.
Existing epoxy resin conductive adhesive relies on merely filling flake silver powder acquisition conductivity, silver powder easy oxidation in using solidification process causes conductivity to descend.
Summary of the invention
The present invention is directed to existing epoxy resin conductive adhesive and rely on merely filling flake silver powder acquisition conductivity, the silver powder deficiency that easy oxidation causes conductivity to descend in using solidification process, a kind of epoxy resin conductive adhesive and preparation method thereof is provided, in advance flake silver powder is carried out finishing and processing by using mineral carbon alkene in the epoxy resin conductive adhesive of the present invention, utilize the high conduction performance of Graphene, reduced on the one hand the usage quantity of silver powder, most important is to have improved the silver powder technical barrier that easy oxidation causes conductivity to descend in solidification process, thereby obtain extremely stable conductivity, and make conductivity improve nearly 20%.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of epoxy resin conductive adhesive comprises the raw material of following weight percent: Resins, epoxy 40%～60%, reaction diluent 2%～10%, solidifying agent 3%～7%, promotor 1%～3%, coupling agent 0.5%～1.5% and through the flake silver powder 20%～40% of graphene modified.
When epoxy resin conductive adhesive of the present invention uses, in 80 ℃～120 ℃ curing 1 hour～3 hours, carry out polyreaction, get final product.
The invention has the beneficial effects as follows: epoxy resin conductive adhesive of the present invention is based on the high conduction performance of Graphene, under set processing condition, flake silver powder is carried out the Graphene finishing to be processed, again pretreated flake silver powder is dispersed in the epoxy resin-base, thereby significantly improve the specific conductivity of flake silver powder, promote the conductivity of tackiness agent.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described flake silver powder through graphene modified is the coated flake silver powder that Graphene is arranged of surface uniform.
Described grapheme material is the KNG of Xiamen Knano Graphite Technology Corporation Limited
TM-150 Graphene microplates.KNG
TM-150 Graphene microplates be Graphene to pile up the thickness form be the Graphene microplate powder of 5-25nm, have the shape of super large than mechanical property and splendid heat conductivilitys such as wear-resisting, the oilness of (diameter/thickness ratio) and excellence, high strength.
Described flake silver powder is the FS-4A model that Changfeng, Zhejiang precious metal powder company limited produces.
Further, described Resins, epoxy comprises one or both in bisphenol A type epoxy resin and the bisphenol f type epoxy resin.
Further, described reaction diluent is aliphatic glycidyl ether Resins, epoxy, described reaction diluent comprises one or more in glycidyl allyl ether (AGE), butylglycidyl ether (BGE), BDDE and 1, the 6-hexanediol diglycidyl ether.
Further, described solidifying agent comprises one or more in Dyhard RU 100, modified imidazole and derivative thereof and the modified amine curing agent, and its fineness is 5 μ～10 μ.
Further, described promotor comprises one or both in 2,4,6-three (dimethylamino methyl) phenol and the aminoethyl piperazine.
Further, described coupling agent comprises one or both in γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) and γ-(methacryloxypropyl) propyl trimethoxy silicane (KH570).
The present invention also provides a kind of preparation method of epoxy resin conductive adhesive to comprise: at first, use Graphene that flake silver powder is carried out pre-treatment and obtain flake silver powder through graphene modified; Then, 40%～60% Resins, epoxy, 2%～10% reaction diluent, 3%～7% solidifying agent, 1%～3% promotor, 0.5%～1.5% coupling agent and 20%～40% flake silver powder through graphene modified are added in the double-planet dynamic mixing stirrer successively, in vacuum tightness-0.08MPa～-0.1MPa, rotational velocity is 300 rev/mins～1000 rev/mins, revolution speed is mechanical stirring discharging in 1 hour～2 hours under 5 rev/mins～15 rev/mins the condition, and is storing under 0 ℃～8 ℃ cold condition after the discharging.
Further, described use Graphene carries out pretreated process to flake silver powder and comprises: with Graphene: deionized water: flake silver powder mixes in 4～7:80～140:24～42 ratios, mixed solution places on the magnetic stirring apparatus and to stir and heated 0.5 hour～1 hour, heating and temperature control is at 60 ℃～80 ℃, carrying out ultrasonic oscillation processed 1 hour～2 hours again, processing is placed in the vacuum drying oven with 140 ℃～160 ℃ of temperature, toasted 5 hours～7 hours, and removed the moisture content that stays on the surface and get final product.
Embodiment
Below principle of the present invention and feature are described, institute only gives an actual example and to be used for explanation the present invention, is not be used to limiting scope of the present invention.
Embodiment 1
Using Graphene that flake silver powder is carried out pretreated process comprises: with Graphene: deionized water: flake silver powder mixes in the 4:85:24 ratio, mixed solution places on the magnetic stirring apparatus and to stir and heated 0.5 hour, heating and temperature control is at 80 ℃, carrying out ultrasonic oscillation processed 1 hour again, processing is placed in the vacuum drying oven with 140 ℃ of temperature, toasted 5 hours, and removed the moisture content that stays on the surface and get final product.
Accurately take by weighing following various raw material, bisphenol A-type E-51 Resins, epoxy 40%, AGE10%, pretreated flake silver powder 40%, Dyhard RU 100 7%, 2,4,6-three (dimethylamino methyl) phenol 2%, KH560 1%; Add successively in the double-planet dynamic mixing stirrer and mix, in vacuum tightness-0.08MPa, rotational velocity is 300 rev/mins, and revolution speed is that mechanical stirring obtained in 1 hour under 5 rev/mins the condition, after the discharging, stores under 0 ℃ of cold condition.During use, in 80 ℃ of curing 1 hour, carry out polyreaction, get final product.
Embodiment 2
Using Graphene that flake silver powder is carried out pretreated process comprises: with Graphene: deionized water: flake silver powder mixes in the 7:90:40 ratio, mixed solution places on the magnetic stirring apparatus and to stir and heated 0.7 hour, heating and temperature control is at 60 ℃, carrying out ultrasonic oscillation processed 1.5 hours again, processing is placed in the vacuum drying oven with 160 ℃ of temperature, toasted 7 hours, and removed the moisture content that stays on the surface and get final product.
Accurately take by weighing following various raw material, bisphenol A-type E-51 Resins, epoxy 60%, BGE 8%, pretreated flake silver powder 23.5%, modified imidazole solidifying agent 5%, 2,4,6-three (dimethylamino methyl) phenol 3%, KH560 0.5%; Add successively in the double-planet dynamic mixing stirrer and mix, in vacuum tightness-0.1MPa, rotational velocity is 1000 rev/mins, and revolution speed is that mechanical stirring obtained in 1 hour under 15 rev/mins the condition, after the discharging, stores under 0 ℃ of cold condition.During use, in 110 ℃ of curing 3 hours, carry out polyreaction, get final product.
Embodiment 3
Using Graphene that flake silver powder is carried out pretreated process comprises: with Graphene: deionized water: flake silver powder mixes in the 5:100:30 ratio, mixed solution places on the magnetic stirring apparatus and to stir and heated 0.8 hour, heating and temperature control is at 75 ℃, carrying out ultrasonic oscillation processed 2 hours again, processing is placed in the vacuum drying oven with 150 ℃ of temperature, toasted 6 hours, and removed the moisture content that stays on the surface and get final product.
Accurately take by weighing following various raw material, Bisphenol F type 830 Resins, epoxy 50%, BDDE 4.5%, pretreated flake silver powder 40%, modified amine curing agent 3%, aminoethyl piperazine 1%, KH570 coupling agent 1.5%; Add successively in the double-planet dynamic mixing stirrer and mix, in vacuum tightness-0.09MPa, rotational velocity is 800 rev/mins, and revolution speed is that mechanical stirring obtained in 1 hour under 10 rev/mins the condition, after the discharging, stores under 5 ℃ of cold condition.During use, in 100 ℃ of curing 3 hours, carry out polyreaction, get final product.
Embodiment 4
Using Graphene that flake silver powder is carried out pretreated process comprises: with Graphene: deionized water: flake silver powder mixes in the 5:125:40 ratio, mixed solution places on the magnetic stirring apparatus and to stir and heated 0.7 hour, heating and temperature control is at 70 ℃, carrying out ultrasonic oscillation processed 1 hour again, processing is placed in the vacuum drying oven with 150 ℃ of temperature, toasted 5 hours, and removed the moisture content that stays on the surface and get final product.
Accurately take by weighing following various raw material, Bisphenol F type 830 Resins, epoxy 60%, 1,6-hexanediol diglycidyl ether 2%, pre-treatment sheet silver powder 30%, Dyhard RU 100 5%, aminoethyl piperazine 2%, KH570 1%; Above-mentioned each component is added in the double-planet dynamic mixing stirrer successively, and in vacuum tightness-0.1MPa, rotational velocity is 1000 rev/mins, and revolution speed is that mechanical stirring obtained in 1 hour under 15 rev/mins the condition, after the discharging, stores under 8 ℃ of cold condition.During use, in 120 ℃ of curing 1 hour, carry out polyreaction, get final product.
Embodiment 5
Using Graphene that flake silver powder is carried out pretreated process comprises: with Graphene: deionized water: flake silver powder mixes in the 7:80:42 ratio, mixed solution places on the magnetic stirring apparatus and to stir and heated 0.8 hour, heating and temperature control is at 80 ℃, carrying out ultrasonic oscillation processed 1.5 hours again, processing is placed in the vacuum drying oven with 140 ℃ of temperature, toasted 7 hours, and removed the moisture content that stays on the surface and get final product.
Accurately take by weighing following various raw material, Bisphenol F type 830 Resins, epoxy 55%, BGE 4%, pre-treatment sheet silver powder 35%, modified amine curing agent 4%, 2,4,6-three (dimethylamino methyl) phenol 1%, KH570 1%; Above-mentioned each component is added in the double-planet dynamic mixing stirrer successively, and in vacuum tightness-0.08Mpa, rotational velocity is 500 rev/mins, and revolution speed is that mechanical stirring obtained in 2 hours under 10 rev/mins the condition, after the discharging, stores under 8 ℃ of cold condition.During use, in 80 ℃ of curing 3 hours, carry out polyreaction, get final product.
The comparative example 1
Conventional epoxies prescription-the do not add prescription of graphene-based Resins, epoxy, accurately take by weighing following various raw material, bisphenol A-type E-51 Resins, epoxy 50%, AGE 10%, flake silver powder 30%, Dyhard RU 100 5%, 2,4,6-three (dimethylamino methyl) phenol 4%, KH560 1%; Above-mentioned each component is added in the double-planet dynamic mixing stirrer successively, and in vacuum tightness-0.1MPa, rotational velocity is 1000 rev/mins, and revolution speed is that mechanical stirring obtained in 2 hours under 15 rev/mins the condition, after the discharging, stores under 0-8 ℃ of cold condition.During use, in 120 ℃ of curing 2 hours, carry out polyreaction, get final product.
Volume specific resistance by following experimental test epoxy conducting adhesive of the present invention.
Test establishing criteria: GB/T 1410-2006
Use the RT-1000 resistivity tester of Xiang Tan China elegant demeanour device Manufacturing Co., Ltd, in 25 ℃, under the standard environment condition single-component epoxy electro-conductive adhesive curing print of above-described embodiment 1-5 and Comparative Examples acquisition is tested.
Table one test acquired results
| Embodiment | Volume specific resistance m Ω .cm |
| Embodiment 1 | 35.37 |
| Embodiment 2 | 33.46 |
| Embodiment 3 | 38.14 |
| Embodiment 4 | 35.28 |
| Embodiment 5 | 36.52 |
| The comparative example 1 | 8.25 |
Data from table 1 can be found out, compare with conventional epoxies, and epoxy resin conductive adhesive of the present invention, conductivity is better, especially is suitable for conductive adhesive and the encapsulation of the high-end electric components and parts that become more meticulous.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. epoxy resin conductive adhesive, it is characterized in that, comprise the raw material of following weight percent: Resins, epoxy 40%～60%, reaction diluent 2%～10%, solidifying agent 3%～7%, promotor 1%～3%, coupling agent 0.5%～1.5% and through the flake silver powder 20%～40% of graphene modified.
2. epoxy resin conductive adhesive according to claim 1 is characterized in that, described flake silver powder through graphene modified is the coated flake silver powder that Graphene is arranged of surface uniform.
3. epoxy resin conductive adhesive according to claim 1 is characterized in that, described Resins, epoxy comprises one or both in bisphenol A type epoxy resin and the bisphenol f type epoxy resin.
4. epoxy resin conductive adhesive according to claim 1 is characterized in that, described reaction diluent is aliphatic glycidyl ether Resins, epoxy.
5. epoxy resin conductive adhesive according to claim 4, it is characterized in that, described aliphatic glycidyl ether Resins, epoxy comprises one or more in glycidyl allyl ether, butylglycidyl ether, BDDE and 1, the 6-hexanediol diglycidyl ether.
6. epoxy resin conductive adhesive according to claim 1 is characterized in that, described solidifying agent comprises one or more in Dyhard RU 100, modified imidazole and derivative thereof and the modified amine curing agent.
7. epoxy resin conductive adhesive according to claim 1 is characterized in that, described promotor comprises one or both in 2,4,6-three (dimethylamino methyl) phenol and the aminoethyl piperazine.
8. epoxy resin conductive adhesive according to claim 1 is characterized in that, described coupling agent comprises one or both in γ-glycidyl ether oxygen propyl trimethoxy silicane and γ-(methacryloxypropyl) propyl trimethoxy silicane.
9. the preparation method of an epoxy resin conductive adhesive is characterized in that, described preparation method comprises: at first, use Graphene that flake silver powder is carried out pre-treatment and obtain flake silver powder through graphene modified; Then, 40%～60% Resins, epoxy, 2%～10% reaction diluent, 3%～7% solidifying agent, 1%～3% promotor, 0.5%～1.5% coupling agent and 20%～40% flake silver powder through graphene modified are added in the double-planet dynamic mixing stirrer successively, in vacuum tightness-0.08MPa～-0.1MPa, rotational velocity is 300 rev/mins～1000 rev/mins, revolution speed is mechanical stirring discharging in 1 hour～2 hours under 5 rev/mins～15 rev/mins the condition, and is storing under 0 ℃～8 ℃ cold condition after the discharging.
10. the preparation method of epoxy resin conductive adhesive according to claim 9, it is characterized in that, described use Graphene carries out pretreated process to flake silver powder and comprises: with Graphene: deionized water: flake silver powder mixes in 4～7:80～140:24～42 ratios, mixed solution places on the magnetic stirring apparatus and to stir and heated 0.5 hour～1 hour, heating and temperature control is at 60 ℃～80 ℃, carrying out ultrasonic oscillation processed 1 hour～2 hours again, processing is placed in the vacuum drying oven with 140 ℃～160 ℃ of temperature, toasted 5 hours～7 hours, and removed the moisture content that stays on the surface and get final product.
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