CN105754535A - Insulating heat-conductive adhesive and preparation method thereof - Google Patents
Insulating heat-conductive adhesive and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K7/16—Solid spheres
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C08K2003/0806—Silver
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/282—Binary compounds of nitrogen with aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C08K2201/00—Specific properties of additives
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Abstract
The invention relates to a heat interface material, in particular to an insulating heat-conductive adhesive. The insulating heat-conductive adhesive is prepared from raw materials in parts by weight as follows: 24-30 parts of an epoxy resin matrix, 16-22 parts of a curing agent, 30-50 parts of an insulating heat-conductive agent and 8-18 parts of an electricity-conductive heat-conductive agent. The characteristic of good electronic heat-conductive interface compatibility is used, the electricity-conductive heat-conductive agent and the insulating heat-conductive agent are compounded, the thermal contact resistance of the heat-conductive agents is reduced, and the overall heat conductivity of the adhesive is improved while the insulation of the adhesive is not affected. The adhesive has the good adhesive property, high heat conductivity coefficient, good manufacturability and high cost performance, and the operation is convenient.
Description
Technical field
The present invention relates to a kind of thermal interfacial material, particularly to a kind of insulating heat-conductive adhesive with conductive and heat-conductive agent and insulating heat-conductive agent mixing filling and preparation method thereof.
Background technology
Along with the fast development of electronic product in recent years, the high-density installation of electronic unit and the radiating requirements brought increases so that thermal conductive adhesive increase in demand in circuit board printing, package semiconductor, heat dissipation design industry.And by the solidfied material of epoxy composite because of its good insulating properties, low-shrinkage, chemical-resistant, glueability is outstanding and obtains large-scale application.It is said that in general, namely the heat conductivity of adhesive can be used for cooling system more than 1W/m K.
It is known that the high-conductive metals such as copper, silver, gold due to have numerous can free migration electronics and show excellence heat conductivility, in like manner electrically conductive graphite also has outstanding electric conductivity, is being generally selected of conductive and heat-conductive agent;The insulated non-metal materials such as bortz powder, Graphene, carborundum, boron nitride completely have outstanding heat conductivility equally because of crystal structure, are being generally selected of insulating heat-conductive agent.In thermal conduction mechanism, insulating heat-conductive agent, because relying on phonon thermal conductance, easily can not form effective hot transmission path because of the impact such as lattice defect, interfacial effect;Conductive and heat-conductive agent relies on electronics heat transfer to have better interface compatibility.
General thermal conductive adhesive is by improving additive level and changing high thermal conductivity thermal conducting agent to improve heat conductivity, and common thermal conducting agent mass content is higher than 70%, and this causes that adhesive viscosity is excessive and is not easy to operate.And existing thermal conductive adhesive it is generally required to below 5 DEG C cold storage environment storage, it is necessary to more than 50 DEG C middle hot setting use.
Summary of the invention
For above-mentioned epoxy resin base adhesive Problems existing, the invention provides a kind of cost performance high, the preparation method of the high-heat-conductivity glue stick of the easy to operate of thermal conducting agent mass content 47%~60%.The technical scheme is that
The insulating heat-conductive adhesive of the present invention, it is characterised in that described insulating heat-conductive adhesive raw material includes following component by weight: epoxy resin-base 24~30 parts, 16~22 parts of firming agent, insulating heat-conductive agent 30~50 parts, conductive and heat-conductive agent 8~18 parts.
Insulating heat-conductive adhesive according to the present invention, wherein, described epoxy resin group includes one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin and polyfunctional group type epoxy resin.
Insulating heat-conductive adhesive according to the present invention, wherein, described firming agent can be firming agent commonly used in the art, for instance, one or more in amine curing agent, acid anhydride type curing agent etc..The present invention reduces interface resistance by the mode that insulating heat-conductive agent and conductive and heat-conductive agent are composite.
Insulating heat-conductive adhesive according to the present invention, wherein, described insulating heat-conductive agent includes one or more in carborundum, boron nitride, aluminium nitride, aluminium oxide, bortz powder and silicon nitride.
Insulating heat-conductive adhesive according to the present invention, wherein, described conductive and heat-conductive agent, including one or more in a nanometer ping-pong ball, micron silver strip, nano-silver thread and electrically conductive graphite powder.
The preparation method of the above-mentioned insulating heat-conductive adhesive of the present invention, comprises the following steps:
1) with 30~50 parts of insulating heat-conductive agent, the conductive and heat-conductive agent of mass fraction 8~18 parts is added appropriate solvent to mix homogeneously, dried prepared mixture A;
2) mixture B will be prepared after 20~30 parts of mixture A and 24~30 part epoxy resin-base mix homogeneously;
3) after 18~30 parts of mixture A and 16~22 part firming agent mix homogeneously, mixture C will after defoaming treatment, be prepared;
4) by mixture B and mixture C example in mass ratio (1~1.5): 1 mix after use, and make its completion of cure, prepare insulating heat-conductive adhesive.
The preparation method of the above-mentioned insulating heat-conductive adhesive according to the present invention, step 1) described solvent can the Conventional solvents of this area, for instance the one in acetone, ethanol or water etc..The addition of described solvent is mass fraction 50~100 parts.
The present invention utilizes the feature that the interface compatibility of electronics heat conduction is good, adopts conductive and heat-conductive agent/insulating heat-conductive agent composite, reduces the thermal contact resistance of thermal conducting agent, and not only having improved adhesive overall thermal conductivity but also can not affect the insulating properties of adhesive;It is good that invention adhesive possesses adhesive property, and heat conductivity is high, and good manufacturability is easy to operate, and cost performance is high.
Detailed description of the invention
By the examples below the present invention being described in further details, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
Embodiment 1
The preparation of insulating heat-conductive adhesive of the present invention is realized: bisphenol A type epoxy resin 25 parts by following steps, aromatic amine curing agent 20 parts, carborundum 40 parts, nano-silver thread 5 parts, nanometer ping-pong ball 5 parts.Its preparation adopts step as follows:
1) by mass fraction carborundum 40 parts, nano-silver thread 5 parts, nanometer ping-pong ball 5 parts, add 50 parts of proper amount of acetone, mechanical agitation is taken out for 2 hours to mix homogeneously, puts into dry 24h in 50 DEG C of vacuum drying ovens, prepares mixture A;
2) by 25 parts of mixture A and 25 part epoxy resin mechanical agitation mixing 1h, taking-up is put into and is prepared mixture B in froth in vacuum case after defoaming treatment;
3) put into defoaming treatment in froth in vacuum case by taking out after mixing 1h in 30 parts of mixture A and 20 part firming agent mechanical agitation, prepare mixture C;
4) use after mixture B, mixture C 1:1 in mass ratio being mixed, and make its completion of cure.
Embodiment 2
The preparation of insulating heat-conductive adhesive of the present invention is realized: bisphenol f type epoxy resin 30 parts by following steps, 22 parts of fatty amines firming agent, carborundum 28 parts, aluminium nitride 7 parts, bortz powder 5 parts, micron silver strip 5 parts, nanometer ping-pong ball 3 parts.Its preparation adopts step as follows:
1) by the carborundum 28 parts of mass fraction, aluminium nitride 7 parts, bortz powder 5 parts, micron silver strip 5 parts, nanometer ping-pong ball 3 parts, add 50 parts of ethanol, mechanical agitation is taken out for 2 hours to mix homogeneously, and after centrifugation, dry 24h in 80 DEG C of vacuum drying ovens, prepares mixture A;
2) 20 parts of mixture A and 30 part epoxy resin are added mixing 1h in vacuum dispersing stirrer, after defoaming treatment, prepare mixture B;
3) 28 parts of mixture A and 22 part firming agent are added mixing 1h in vacuum dispersing stirrer, after defoaming treatment, prepare mixture C;
4) use after mixture B, mixture C 1:1 in mass ratio being mixed, and make its completion of cure.
Embodiment 3
The preparation of insulating heat-conductive adhesive of the present invention is realized: polyfunctional group type epoxy resin 30 parts by following steps, alicyclic ring amine curing agent 20 parts, carborundum 20 parts, silicon nitride 10 parts, aluminium nitride 8 parts, micron silver strip 10 parts.Its preparation adopts step as follows:
1) by mass fraction carborundum 20 parts, silicon nitride 10 parts, aluminium nitride 8 parts, micron silver strip 10 parts, add in 100 parts of distilled water, mechanical agitation is taken out for 2 hours to mix homogeneously, puts into dry 24h in 120 DEG C of vacuum drying ovens, prepare mixture A after centrifugation;
2) by 30 parts of mixture A and 30 part epoxy resin, mechanical agitation 2h, to mix homogeneously, prepares mixture B after defoaming treatment;
3) 18 parts of mixture A and 20 part firming agent are added mixing 1h in vacuum dispersing stirrer, after defoaming treatment, prepare mixture C;
4) use after mixture B, mixture C 1.5:1 in mass ratio being mixed, and make its completion of cure.
Embodiment 4
The preparation of insulating heat-conductive adhesive of the present invention is realized: bisphenol A type epoxy resin 24 parts, fatty amines and 16 parts of polyether amine firming agent (mass ratio 3:1), carborundum 30 parts, boron nitride 20 parts, nanometer ping-pong ball 10 parts by following steps.Its preparation adopts step as follows:
1) by mass fraction carborundum 30 parts, boron nitride 20 parts, nanometer ping-pong ball 10 parts, add in 100 parts of distilled water, 80 DEG C of vacuum stirring 2h, to mix homogeneously, take out and put into dry 24h in 120 DEG C of vacuum drying ovens, prepare mixture A;
2) by 30 parts of mixture A and 24 part epoxy resin, mechanical agitation 2h, to mix homogeneously, prepares mixture B after defoaming treatment;
3) by 30 parts of mixture A and 16 part firming agent, mechanical agitation 2h, to mix homogeneously, prepares mixture C after defoaming treatment;
4) use after mixture B, mixture C 1.2:1 in mass ratio being mixed, and make its completion of cure.
Embodiment 5
The preparation of insulating heat-conductive adhesive of the present invention is realized: bisphenol A type epoxy resin 30 parts, acid anhydride type curing agent and accelerator 20 parts, carborundum 40 parts, 10 parts of electrically conductive graphite powder by following steps.Its preparation adopts step as follows:
1) by mass fraction carborundum 40 parts, electrically conductive graphite 10 parts, add 100 parts of distilled water, mechanical agitation is taken out and is put into dry 24h in 120 DEG C of vacuum drying ovens to mix homogeneously, centrifugation, prepare mixture A for 2 hours;
2) by 30 parts of mixture A and 30 part epoxy resin, mechanical agitation 2h, to mix homogeneously, prepares mixture B after defoaming treatment
3) 20 parts of mixture A and 20 part firming agent are added mixing 1h in vacuum dispersing stirrer, after defoaming treatment, prepare mixture C;
4) use after mixture B, mixture C 1.5:1 in mass ratio being mixed, and make its completion of cure.
Embodiment 6
The preparation of insulating heat-conductive adhesive of the present invention is realized: bisphenol f type epoxy resin 24 parts by following steps, 18 parts of firming agent (fatty amine mixes with aliphatic cyclic amine equal proportion), carborundum 20 parts, aluminium oxide 10 parts, boron nitride 10 parts, micron silver strip 10 parts, nanometer ping-pong ball 8 parts.Its preparation adopts step as follows:
1) by the carborundum 20 parts of mass fraction, aluminium oxide 10 parts, boron nitride 10 parts, micron silver strip 10 parts, nanometer ping-pong ball 8 parts, add 100 parts of ethanol, mechanical agitation is taken out for 2 hours to mix homogeneously, and after centrifugation, dry 24h in 80 DEG C of vacuum drying ovens, prepares mixture A;
2) 30 parts of mixture A and 24 part epoxy resin are added mixing 1h in vacuum dispersing stirrer, after defoaming treatment, prepare mixture B;
3) 28 parts of mixture A and 18 part firming agent are added mixing 1h in vacuum dispersing stirrer, after defoaming treatment, prepare mixture C;
4) use after mixture B, mixture C 1.2:1 in mass ratio being mixed, and make its completion of cure.
Comparative example
The preparation of insulating heat-conductive adhesive of the present invention is realized: bisphenol A type epoxy resin 30 parts by following steps, 20 parts of fatty amines firming agent, carborundum 50 parts.Its preparation adopts step as follows:
1) by 20 parts of carborundums and 30 parts of epoxy resin, mechanical agitation 2h, to mix homogeneously, prepares mixture A after defoaming treatment
2) by 30 parts of carborundums and 20 parts of firming agent, mechanical agitation 2h, to mix homogeneously, prepares mixture B after defoaming treatment;
3) use after mixture A, mixture B 1:1 in mass ratio being mixed, and make its completion of cure.
By following experimental test invention adhesive heat conductivity and adhesive shear strength.
Adhesive shear strength method of testing: GB7124-1986.
Thermal conductivity is tested: use the PPMS-9T type property test system of U.S. QuantumDesign company to test the thermal conductivity of solid after adhesive solidification under 25 DEG C of standard environments.
Resistivity measurement: use Beijing hat to survey EST121 type high resistance tester, the resistivity of solid after test adhesive solidification under 25 DEG C of standard environments.
Acquired results tested by table 1
Embodiment | Thermal conductivity (W/m K) | Resistivity (Ω cm) | Adhesive shear strength (MPa) |
Embodiment 1 | 1.85 | 2×1011 | 7.93 |
Embodiment 2 | 1.41 | 3×1013 | 9.72 |
Embodiment 3 | 1.36 | 9×1013 | 11.38 |
Embodiment 4 | 2.03 | 4×1012 | 7.22 |
Embodiment 5 | 1.68 | 5×1012 | 10.65 |
Embodiment 6 | 1.44 | 5×1012 | 7.86 |
Comparative example | 0.94 | More than 1014 | 8.39 |
Can be seen that according to table 1 acquired results, while the heat conductivility making the composite thermal plastic insulation of introducing conductive and heat-conductive agent and insulating heat-conductive agent is improved significantly, its resistivity declines and inconspicuous, still falls within insulant and (thinks in electrotechnics that resistivity is 109~1022The material of Ω cm is insulant).
Certainly; the present invention can also have various embodiments; when without departing substantially from present invention spirit and essence thereof; those of ordinary skill in the art can make various corresponding change and deformation according to disclosure of the invention, but these change accordingly and deformation all should belong to the scope of the claims appended by the present invention.
Claims (8)
1. an insulating heat-conductive adhesive, it is characterised in that described insulating heat-conductive adhesive raw material includes following component by weight: epoxy resin 24~30 parts, 16~22 parts of firming agent, insulating heat-conductive agent 30~50 parts, conductive and heat-conductive agent 8~18 parts.
2. insulating heat-conductive adhesive according to claim 1, it is characterised in that described epoxy resin includes one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin and polyfunctional group type epoxy resin.
3. insulating heat-conductive adhesive according to claim 1, it is characterised in that described firming agent is one or more in amine curing agent and acid anhydride type curing agent.
4. insulating heat-conductive adhesive according to claim 1, it is characterised in that described insulating heat-conductive agent includes one or more in carborundum, boron nitride, aluminium nitride, aluminium oxide, bortz powder and silicon nitride.
5. insulating heat-conductive adhesive according to claim 1, it is characterised in that described conductive and heat-conductive agent, including one or more in a nanometer ping-pong ball, micron silver strip, nano-silver thread and electrically conductive graphite powder.
6. a preparation method for the arbitrary described insulating heat-conductive adhesive of claim 1-5, comprises the following steps:
1) with 30~50 parts of insulating heat-conductive agent, the conductive and heat-conductive agent of mass fraction 8~18 parts is added appropriate solvent to mix homogeneously, dried prepared mixture A;
2) mixture B will be prepared after 20~30 parts of mixture A and 24~30 part epoxy resin-base mix homogeneously;
3) after 18~30 parts of mixture A and 16~22 part firming agent mix homogeneously, mixture C will after defoaming treatment, be prepared;
4) by mixture B and mixture C (1~1.5) in proportion: 1 mix after use, and make its completion of cure, prepare insulating heat-conductive adhesive.
7. preparation method according to claim 6, it is characterised in that step 1) described solvent is the one in acetone, ethanol or water.
8. the preparation method according to claim 6 or 7, it is characterised in that step 1) addition of described solvent is mass fraction 50~100 parts.
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Cited By (7)
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CN106356112A (en) * | 2016-10-31 | 2017-01-25 | 广东昭信照明科技有限公司 | Conductive silver paste with low silver content and preparation method thereof |
CN106634654A (en) * | 2016-12-16 | 2017-05-10 | 东莞市翔龙能源科技有限公司 | Adhesive film with radiant heat dissipation function for LED (Light Emitting Diode) and preparation method of adhesive film |
CN107641490A (en) * | 2017-09-22 | 2018-01-30 | 北京天山新材料技术有限公司 | A kind of epoxy adhesive |
CN109679280A (en) * | 2018-11-12 | 2019-04-26 | 许文强 | A kind of preparation method of high thermal conductivity electromagnetic shielding material |
CN110350705A (en) * | 2019-07-05 | 2019-10-18 | 张峰铭 | The fire-proof motor and its method of a kind of waterproof and dustproof, Anti-burnout |
CN110890167A (en) * | 2018-09-10 | 2020-03-17 | 昆山工研院新型平板显示技术中心有限公司 | Conductive paste, preparation method and display device comprising conductive paste |
CN115368858A (en) * | 2022-08-31 | 2022-11-22 | 广东合正科技有限公司 | Heat-conducting adhesive for circuit board and preparation method thereof |
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CN104910846A (en) * | 2015-06-15 | 2015-09-16 | 南京工业大学 | Heat-conductive electricity-conductive adhesive and preparation method of adhesive |
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JP2001207033A (en) * | 2000-01-26 | 2001-07-31 | Sumitomo Bakelite Co Ltd | Die attach paste and semiconductor device |
CN102161871A (en) * | 2011-03-09 | 2011-08-24 | 烟台德邦电子材料有限公司 | Heat-conductive insulated adhesive tape for large-power light-emitting diode (LED) and preparation method thereof |
CN104017529A (en) * | 2014-04-14 | 2014-09-03 | 江苏嘉娜泰有机硅有限公司 | Single-component epoxy resin conductive silver adhesive composition and preparation method thereof |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106356112A (en) * | 2016-10-31 | 2017-01-25 | 广东昭信照明科技有限公司 | Conductive silver paste with low silver content and preparation method thereof |
CN106634654A (en) * | 2016-12-16 | 2017-05-10 | 东莞市翔龙能源科技有限公司 | Adhesive film with radiant heat dissipation function for LED (Light Emitting Diode) and preparation method of adhesive film |
CN107641490A (en) * | 2017-09-22 | 2018-01-30 | 北京天山新材料技术有限公司 | A kind of epoxy adhesive |
CN110890167A (en) * | 2018-09-10 | 2020-03-17 | 昆山工研院新型平板显示技术中心有限公司 | Conductive paste, preparation method and display device comprising conductive paste |
CN109679280A (en) * | 2018-11-12 | 2019-04-26 | 许文强 | A kind of preparation method of high thermal conductivity electromagnetic shielding material |
CN109679280B (en) * | 2018-11-12 | 2020-12-15 | 嘉兴华维新能源有限公司 | Preparation method of high-thermal-conductivity electromagnetic shielding material |
CN110350705A (en) * | 2019-07-05 | 2019-10-18 | 张峰铭 | The fire-proof motor and its method of a kind of waterproof and dustproof, Anti-burnout |
CN115368858A (en) * | 2022-08-31 | 2022-11-22 | 广东合正科技有限公司 | Heat-conducting adhesive for circuit board and preparation method thereof |
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