CN102408858A - Stable type conductive adhesive and preparation method thereof - Google Patents
Stable type conductive adhesive and preparation method thereof Download PDFInfo
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- CN102408858A CN102408858A CN2011103247197A CN201110324719A CN102408858A CN 102408858 A CN102408858 A CN 102408858A CN 2011103247197 A CN2011103247197 A CN 2011103247197A CN 201110324719 A CN201110324719 A CN 201110324719A CN 102408858 A CN102408858 A CN 102408858A
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Abstract
The invention discloses a high-heat-conductivity stable type conductive adhesive for electronic component bonding and surface packaging, which is prepared from the following raw materials in percentage by weight: 10-25% of conductive adhesive matrix, 60-80% of micron laminar silver powder, 5-20% of micron spherical silver powder and 0.03-0.15% of single-wall carbon nanotube. The conductive adhesive matrix is prepared from the following components in percentage by weight: 70-80% of modified epoxy resin, 2-10% of imidazole curing agent, 10-20% of reactive diluent and 0.5-2% of organosilicon coupling agent. Under the combined action of the micro laminar silver powder and the micro spherical silver powder, the conductivity of the high-heat-conductivity stable type conductive adhesive is enhanced; the acidized single-wall carbon nanotubes are added to enhance the heat conductivity and the contact resistance stability of the high-heat-conductivity stable type conductive adhesive; and the performance indexes of the high-heat-conductivity stable type conductive adhesive are obviously higher than working properties of the conductive adhesive in the prior art, thereby solving the problems of low heat conductivity, instable contact resistance and the like in the conductive adhesive in the prior art. The invention is especially applicable to the field of high-power electronic packaging in micro-electronic industry.
Description
Technical field
The present invention relates to a kind of high heat conduction stable form conductive resin that is used for electronic component bonding and surface encapsulation.Its advantage is: thermal conductivity is big, electric conductivity is high, the working hour is long, contact resistance is stable; LV makes its volatile matter with good dispersiveness, curing oven, extremely low amount, with metal advantages of good caking property is arranged.Be particularly suitable for needing heat conduction simultaneously, conduction and bonding to share, have very high practical value for the development of Electronic Packaging industry and high-capacity LED Packaging Industry.
Background technology
Conductive resin is the tackiness agent that has certain conductivity after a kind of curing or the drying; It is that conducting particles is main moity with matrix resin and conductive filler material usually; Bonding effect through matrix resin combines conducting particles; Matrix resin shrinks and compresses conducting particles formation conductive path in the solidification process, realizes being connected by the conduction of sticking material.Because the matrix resin of conductive resin is a kind of tackiness agent; Usually can be in room temperature to 150 ℃ curing; Connect the welding temperature more than 200 ℃ far below the tin lead welding, material deformation, the thermal damage of electron device and the formation of internal stress that this has just been avoided welding high temperature to cause.Conductive resin is compared with scolder, and technology is simple, and easy handling can be enhanced productivity, and has avoided also simultaneously that heavy metal lead causes environmental pollution in the wiping solder, so conductive resin is to substitute the tin lead welding to connect the ideal material of realizing that conduction connects.
At present conductive resin has been widely used in the encapsulation of electronic component such as liquid crystal display, photodiode, IC chip, pcb component, smart card and assembly and bonding, and the trend that progressively replaces traditional soldering welding is arranged.Conductive resin has wide application prospect as the substitute products of wiping solder, still exists a lot of deficiencies but compare with the tin lead welding at present, and is on the low side such as electric conductivity and thermal conductivity, and conductive stability and weather resistance still await raising.Many electronic components begin microminiaturization, make that the material of therefore seeking high heat conduction stable form becomes necessary to the thermotolerance of electron device and the further strict harshness of requirement of thermal diffusivity.The thermal conductivity of domestic and international most of sliver-powder conducting glue products is lower at present, is generally 0.5-2.5W/ (mK), far can not satisfy the requirement of high power device.The present invention is exactly that the conductive resin thermal conductivity and the contact resistance stability that are directed against in the market are not high, and can not satisfy performance demands and invent, and improve the thermal conductivity of conductive resin and the stability of contact resistance, also be the important topic of industry research always.
Summary of the invention
The epoxide resin conductive adhesive that the purpose of this invention is to provide good, the high heat conduction of a kind of consistency, stable form to solve present electro-conductive adhesive in deficiency not high aspect the heat conductivility, utilizes the combination of different fillers to reach favorable conductive and heat conductivility simultaneously.
The technical solution adopted for the present invention to solve the technical problems is: in the conductive resin resin matrix, add micron flake silver powder and the spherical silver powder of micron; Spherical silver powder is used for filling the gap of flake silver powder; Form more conduction and thermal conducting path between the metallic particles thereby make, thereby play the purpose that increases electric conductivity and thermal conductivity.The combination of different-grain diameter silver powder is used, and can reduce the consumption of silver powder, thereby reduce the viscosity of conductive resin, practices thrift cost.SWCN is a kind of nano material of high heat conductance, through adding SWNT, the thermal conductivity of conductive resin is significantly improved, and is specially adapted to the Electronic Packaging technology in the microelectronics industry.
A kind of stable form high-thermal-conductivity epoxy resin conductive resin is characterized in that the composition of this conductive resin is counted with weight fraction:
10 ~ 25 parts of conductive resin matrixes
60 ~ 80 parts of micron flake silver powders
5 ~ 20 parts in the spherical silver powder of micron
0.03 ~ 0.15 part of SWCN
The matrix of this conductive resin is made up of epoxy resin, thinner, silicone based coupling agent and imidazole curing agent four parts.This four part shared proportion in the conductive resin matrix, count with weight fraction:
70 ~ 80 parts of modified epoxies
10 ~ 20 parts of reactive thinners
0.5 ~ 2 part of silicone based coupling agent
2 ~ 10 parts of imidazole curing agents
Described modified epoxy is a kind of in modifying epoxy resin by organosilicon, organic titanium modified epoxy and the organic boron modified epoxy.
Described silicone based coupling agent is a kind of in vinyl silanes, aminosilane, the epoxy radicals silicone hydride organic coupling agent.
Described imidazole curing agent is a kind of in glyoxal ethyline, 2-ethyl-4-methylimidazole and the 1 cyanic acid 2-ethyl 4-methylimidazole.
Said micron flake silver powder is of a size of 6 ~ 8 μ m, and the spherical silver powder of micron is of a size of 1.5 ~ 2 μ m, and the diameter of SWCN is 1 ~ 2 nm.
The present invention solves the concrete steps that its technical problem adopts:
In order to remove the catalyzer and the decolorizing carbon on SWCN surface, improve the purity of carbon nanotube, improve SWNT simultaneously owing to have very big specific surface area, the agglomeration that is produced carries out acidification with SWCN earlier.The step of the acidification of described SWCN is: SWCN is added in the mixing solutions of the vitriol oil and concentrated nitric acid (volume ratio 3:1); Ultra-sonic dispersion 3-5 hour; Then on the sand mold funnel with deionized water repeatedly filtration washing up to pH=7; Then the SWCN of acidification is placed in the vacuum drying oven and under 100 ℃, is dried to constant weight, ground 5-10 minute with agate mortar then, obtain the SWCN of acidification.Preparation heat-conductivity conducting glue step is: earlier with the SWCN after the acidifying in acetone soln ultra-sonic dispersion 1-3 hour; SWCN is evenly spread in the acetone; Then this mixture is joined in the resin, be put into behind the thorough mixing in 80 ℃ the air dry oven acetone is evaporated totally fully, add solidifying agent, thinner and coupling agent then; Add two kinds of silver powder after mixing again, can be made into stable form high heat-conductivity conducting glue in 10 minutes with the planetary mixer high-speed stirring at last.
The invention has the advantages that and select high temperature material, mix the different conductivity filler, not only greatly improved the thermotolerance problem of electro-conductive adhesive, and improved the conduction and the heat conductivility of electro-conductive adhesive as base material.Utilize micro-silver powder excellent conduction and thermal conductivity, be aided with the synergy of micron spherical silver particles and CNT, improved the heat conductivility of conductive resin, also improved the contact resistance stability of conductive resin simultaneously.
Description of drawings
Fig. 1 is for adding the viscosity of conductive resin under different rotating speeds of different mass mark SWNT.
Fig. 2 for the conductive resin that adds different mass mark SWNT under 85 ℃/85%RH condition with the comparison of gold surface contact resistance stability.
Embodiment
Embodiment 1
In the present embodiment, the gross weight of stable form conductive resin is 10g, and its composition is counted with weight fraction:
25 parts of conductive resin matrixes
66.97 parts of micron flake silver powders
8 parts in the spherical silver powder of micron
0.03 part of the single wall carbon CNT of acidification
Wherein the conductive resin matrix is formed, and counts with weight fraction:
70 ~ 80 parts of modified epoxies
10 ~ 20 parts of reactive thinners
0.5 ~ 2 part of silicone based coupling agent
2 ~ 10 parts of imidazole curing agents
Wherein said micron flake silver powder is of a size of 6 ~ 8 μ m, and the spherical silver powder of micron is of a size of 1.5 ~ 2 μ m, and the diameter of SWCN is 1 ~ 2 nm.The step of the acidification of described SWCN is: SWCN is added in the mixing solutions of the vitriol oil and concentrated nitric acid (volume ratio 3:1); Ultra-sonic dispersion 3-5 hour; Use the deionized water repetitive scrubbing up to pH=7 then; Filter with the sand mold funnel, in vacuum oven, be dried to constant weight after, grind subsequent use.
The concrete grammar of conductive resin preparation is: earlier with the SWCN after the acidifying in acetone soln ultra-sonic dispersion 1-3 hour; SWCN is evenly spread in the acetone, this mixture is joined in the resin matrix mix then, be put in 80 ℃ the loft drier acetone soln evaporation is clean; And then adding solidifying agent, thinner and coupling agent; Mix, add silver powder at last and mix, be made into conductive resin.
After above-mentioned conductive resin thorough mixing stirring, constant temperature made its completely solidified in 30 minutes in 150 ℃ baking oven.Under 25 ℃, recording its volume specific resistance is 4.89 * 10
-4Ω cm, the viscosity when rotor is 5rpm is 9366.37CP, and thixotropy index is 5.25, and thermal conductivity is 9.804 W/ (mK).
Embodiment 2
In the present embodiment, the gross weight of stable form conductive resin is 10g, and its composition is counted with weight fraction:
25 parts of conductive resin matrixes
66.94 parts of micron flake silver powders
8 parts in the spherical silver powder of micron
0.06 part of the single wall carbon CNT of acidifying aftertreatment
Wherein the compound method of the treatment process of the size of the composition of conductive resin matrix, silver powder, SWCN and conductive resin thereof is all identical with instance 1.
After above-mentioned conductive resin thorough mixing stirring, constant temperature made its completely solidified in 30 minutes in 150 ℃ baking oven.Under 25 ℃, recording its volume specific resistance is 5.42 * 10
-4Ω cm, the viscosity when rotor is 5rpm is 9683.87CP, and thixotropy index is 5.25, and thermal conductivity is 4.132 W/ (mK).
Embodiment 3
In the present embodiment, the gross weight of stable form conductive resin is 10g, and its composition is counted with weight fraction:
25 parts of conductive resin matrixes
66.85 parts of micron flake silver powders
8 parts in the spherical silver powder of micron
0.15 part of single wall carbon CNT
Wherein the compound method of the treatment process of the size of the composition of conductive resin matrix, silver powder, SWCN and conductive resin thereof is all identical with instance 1.
After above-mentioned conductive resin thorough mixing stirring, constant temperature made its completely solidified in 30 minutes in 150 ℃ baking oven.Under 25 ℃, recording its volume specific resistance is 3.43 * 10
-4Ω cm, the viscosity when rotor is 5rpm is 12858.91CP, and thixotropy index is 5.68, and thermal conductivity is 5.236 W/ (mK).
As shown in Figure 1, the thixotropy index of the conductive resin of interpolation SWCN is highly suitable for the gluing process of conductive resin between 5.25 to 5.68.The viscosity of conductive resin increases with the increase of SWCN addition, and the user can select the conductive resin of suitable viscosity according to different needs.
As shown in Figure 2, the conductive resin of interpolation carbon nanotube and the contact resistivity of gold surface meet the application standard of conductive resin all less than 20%.Because the adding of carbon nanotube, the heat conductivility of conductive resin and the stability of contact resistance are improved really.
Claims (4)
1. stable form conductive resin is characterized in that the composition of this conductive resin is counted with weight fraction:
Conductive resin matrix 10-25 part
60～80 parts of micron flake silver powders
5～20 parts in the spherical silver powder of micron
0.03～0.15 part of SWNT
Wherein the composition of conductive resin matrix is counted with weight fraction:
70～80 parts of modified epoxies
0.5～2 part of silicone based coupling agent
2～10 parts of imidazole curing agents
10～20 parts of reactive thinners.
2. like claims 1 described stable form conductive resin, it is characterized in that described micron flake silver powder is of a size of 6 ~ 8 μ m, the spherical silver powder of micron is of a size of 1.5 ~ 2 μ m, and the diameter of SWCN is 1 ~ 2 nm.
3. stable form conductive resin as claimed in claim 1; It is characterized in that described SWCN through acidification, the step of acidification is: SWCN is added the vitriol oil and the concentrated nitric acid volume ratio is in the mixing solutions of 3:1, ultra-sonic dispersion 3 ~ 5 hours; Use the deionized water repetitive scrubbing up to pH=7 then; Filter with the sand mold funnel, in vacuum oven, be dried to constant weight after, grind.
4. the preparation method of the described stable form conductive resin of claim 1 is characterized in that this method has following process step:
A. earlier SWCN is carried out acidification according to the described acidification step of claim 3;
B. according to the prescription of claim 1, with the ultra-sonic dispersion 1 ~ 3 hour in acetone soln of the SWCN after the acidifying, SWCN is evenly spread in the acetone earlier; Then this mixture is joined in the resin matrix and mix; Be put in 80 ℃ the loft drier acetone soln evaporation is clean, and then add solidifying agent, thinner and coupling agent, mix; Add silver powder at last and mix, be made into conductive resin.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838958A (en) * | 2012-09-17 | 2012-12-26 | 北京宇极科技发展有限公司 | Preparation method of silver colloid for LED (Light Emitting Diode) with high thermal conductivity |
| CN102925090A (en) * | 2012-11-28 | 2013-02-13 | 上海材料研究所 | Preparation method of conductive silver adhesive for electromagnetic shielding |
| CN103317148A (en) * | 2013-06-07 | 2013-09-25 | 惠州市富济电子材料有限公司 | Silver powder and silver colloid prepared with silver powder |
| CN103820055A (en) * | 2013-12-11 | 2014-05-28 | 青岛海洋新材料科技有限公司 | Conductive adhesive for ocean engineering |
| CN104240842A (en) * | 2013-06-21 | 2014-12-24 | 中国钢铁股份有限公司 | Method for preparing modified silver powder and glass powder-free sintered silver colloid |
| CN104356970A (en) * | 2014-10-28 | 2015-02-18 | 成都纳硕科技有限公司 | High-conductivity ultraviolet light curing conductive adhesive |
| CN106349992A (en) * | 2016-08-31 | 2017-01-25 | 强新正品（苏州）环保材料科技有限公司 | Flexible conductive adhesive for electronic component adhesion and surface encapsulation |
| CN107686713A (en) * | 2017-09-25 | 2018-02-13 | 常州市沃兰特电子有限公司 | A kind of epoxide resin conductive adhesive for Electronic Packaging |
| CN108018013A (en) * | 2017-12-30 | 2018-05-11 | 孙祎 | A kind of preparation method of quick-drying stable type conductive adhesive material |
| CN109705803A (en) * | 2019-01-11 | 2019-05-03 | 镇江博慎新材料有限公司 | A kind of single-component organic silicon conducting resinl and its preparation method and application |
| CN112513797A (en) * | 2018-07-17 | 2021-03-16 | 深圳市柔宇科技股份有限公司 | Conductive film, preparation method thereof, touch panel and display device |
| CN112552852A (en) * | 2020-12-18 | 2021-03-26 | 中国振华集团云科电子有限公司 | High-thermal-conductivity silver paste for bonding high-power components and preparation method thereof |
| CN112574703A (en) * | 2019-09-30 | 2021-03-30 | 广州昊毅化工科技有限公司 | Solvent-free conductive adhesive and preparation method thereof |
| CN112745788A (en) * | 2019-10-30 | 2021-05-04 | 深圳市聚飞光电股份有限公司 | Conductive silver adhesive, preparation method thereof and light-emitting device |
| CN113004844A (en) * | 2019-12-19 | 2021-06-22 | 上海市塑料研究所有限公司 | High-heat-dissipation conductive adhesive and preparation method thereof |
| CN114133891A (en) * | 2021-12-23 | 2022-03-04 | 长春永固科技有限公司 | Ultrathin flaky silver powder conductive adhesive and preparation method and application thereof |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102838958A (en) * | 2012-09-17 | 2012-12-26 | 北京宇极科技发展有限公司 | Preparation method of silver colloid for LED (Light Emitting Diode) with high thermal conductivity |
| CN102838958B (en) * | 2012-09-17 | 2013-12-11 | 北京宇极科技发展有限公司 | Preparation method of silver colloid for LED (Light Emitting Diode) with high thermal conductivity |
| CN102925090A (en) * | 2012-11-28 | 2013-02-13 | 上海材料研究所 | Preparation method of conductive silver adhesive for electromagnetic shielding |
| CN102925090B (en) * | 2012-11-28 | 2014-07-02 | 上海材料研究所 | Preparation method of conductive silver adhesive for electromagnetic shielding |
| CN103317148A (en) * | 2013-06-07 | 2013-09-25 | 惠州市富济电子材料有限公司 | Silver powder and silver colloid prepared with silver powder |
| CN103317148B (en) * | 2013-06-07 | 2015-11-25 | 惠州市富济电子材料有限公司 | A kind of silver powder and gained elargol |
| CN104240842A (en) * | 2013-06-21 | 2014-12-24 | 中国钢铁股份有限公司 | Method for preparing modified silver powder and glass powder-free sintered silver colloid |
| CN103820055A (en) * | 2013-12-11 | 2014-05-28 | 青岛海洋新材料科技有限公司 | Conductive adhesive for ocean engineering |
| CN104356970A (en) * | 2014-10-28 | 2015-02-18 | 成都纳硕科技有限公司 | High-conductivity ultraviolet light curing conductive adhesive |
| CN106349992A (en) * | 2016-08-31 | 2017-01-25 | 强新正品（苏州）环保材料科技有限公司 | Flexible conductive adhesive for electronic component adhesion and surface encapsulation |
| CN107686713A (en) * | 2017-09-25 | 2018-02-13 | 常州市沃兰特电子有限公司 | A kind of epoxide resin conductive adhesive for Electronic Packaging |
| CN108018013A (en) * | 2017-12-30 | 2018-05-11 | 孙祎 | A kind of preparation method of quick-drying stable type conductive adhesive material |
| CN112513797A (en) * | 2018-07-17 | 2021-03-16 | 深圳市柔宇科技股份有限公司 | Conductive film, preparation method thereof, touch panel and display device |
| CN109705803A (en) * | 2019-01-11 | 2019-05-03 | 镇江博慎新材料有限公司 | A kind of single-component organic silicon conducting resinl and its preparation method and application |
| CN109705803B (en) * | 2019-01-11 | 2021-02-26 | 镇江博慎新材料有限公司 | Single-component organic silicon conductive adhesive and preparation method and application thereof |
| CN112574703A (en) * | 2019-09-30 | 2021-03-30 | 广州昊毅化工科技有限公司 | Solvent-free conductive adhesive and preparation method thereof |
| CN112745788A (en) * | 2019-10-30 | 2021-05-04 | 深圳市聚飞光电股份有限公司 | Conductive silver adhesive, preparation method thereof and light-emitting device |
| CN113004844A (en) * | 2019-12-19 | 2021-06-22 | 上海市塑料研究所有限公司 | High-heat-dissipation conductive adhesive and preparation method thereof |
| CN112552852A (en) * | 2020-12-18 | 2021-03-26 | 中国振华集团云科电子有限公司 | High-thermal-conductivity silver paste for bonding high-power components and preparation method thereof |
| CN114133891A (en) * | 2021-12-23 | 2022-03-04 | 长春永固科技有限公司 | Ultrathin flaky silver powder conductive adhesive and preparation method and application thereof |
| CN114133891B (en) * | 2021-12-23 | 2023-11-03 | 长春永固科技有限公司 | Ultrathin flake silver powder conductive adhesive and preparation method and application thereof |
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Application publication date: 20120411 |