CN101475787A - Isotropic high performance heat conducting adhesive and preparation thereof - Google Patents
Isotropic high performance heat conducting adhesive and preparation thereof Download PDFInfo
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- CN101475787A CN101475787A CNA2009100291256A CN200910029125A CN101475787A CN 101475787 A CN101475787 A CN 101475787A CN A2009100291256 A CNA2009100291256 A CN A2009100291256A CN 200910029125 A CN200910029125 A CN 200910029125A CN 101475787 A CN101475787 A CN 101475787A
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Abstract
The invention belongs to the technical field of material preparation, and in particular relates to an isotropic high-performance thermal conductive adhesive and a method for preparing the same. According to proportion, mixed powders of silver nanowire and silver nanoparticles are added to a mixed resin system of epoxy resin, CTBN modified epoxy resin and aerosil, and are subjected to mixing treatment for 20 to 30 seconds in a high-speed shear mixing machine; a mixed colloid is added with an acid anhydride curing agent and a curing accelerant, is placed in the high-speed shear mixing machine for mixing treatment for 20 to 30 seconds to prepare the isotropic high-performance thermal conductive adhesive; and compared with the prior thermal conductive adhesive, the isotropic high-performance thermal conductive adhesive has the advantages of high thermal conductivity, stable mechanical property and performance, and the like. The method for preparing the isotropic high-performance thermal conductive adhesive has low cost and good controllability, is simple, and has good practical value in the development of the electronic encapsulation industry and the high-power LED encapsulation industry.
Description
Technical field
The invention belongs to technical field of material, refer in particular to a kind of isotropy high-performance thermal conductive adhesive and preparation method thereof.
Background technology
Along with Electronic Packaging develops to miniaturization, lightness direction gradually, the assembling of microelectronic device is densification more and more, and its Working environment sharply changes to the high temperature direction.2 ℃ of the every risings of electronic devices and components temperature, its reliability decrease 10%, therefore in time heat radiation becomes the important factor that influences its work-ing life.Need in aerospace, electronics, the field such as electric to be applied to dispel the heat and the heat-conducting glue at heat transfer position, can in time loose and remove a large amount of heats that produce in the electronics use, all significant to its reliability of densification, miniaturization and raising, precision and the work-ing life of electronic product.
The heat conductive filler that uses in the heat-conducting glue mainly comprises following several at present: a kind of is that nitride and the carbide with good insulation properties and high thermal conductivity coefficient mainly comprises aluminium nitride, boron nitride, silicon nitride, silicon carbide, norbide and titanium carbide etc.Also having a kind of is that metal oxide such as beryllium oxide, aluminum oxide, magnesium oxide and silicon oxide etc. have than higher thermal conductivity, is filled into and can gives high thermal conductivity of tackiness agent and good physical and mechanical properties in the resin matrix.The third is to adopt metal-powder or the carbon fiber with high heat-conductivity conducting, because these materials itself have high heat conduction high conduction performance, therefore adopt the heat-conducting glue of these fillers all to have very high thermal conductivity, simultaneously owing to adopt the reduction of filler content in the heat-conducting glue behind these fillers, so the heat-conducting glue of preparation all has very high mechanics mechanical property.The domestic and international at present research about heat-conducting glue just just launches, and all discloses some basic recipe and basic devices about the preparation heat-conducting glue as domestic patent CN1061235, CN1970666, CN1880399 and CN1966597.These heat-conducting glues are owing to be subjected to adopting the restriction of the thermal conductivity of heat conductive filler own, so it is low thermal conductivity to occur, the life-span is short, shortcomings such as bad mechanical property.
For this reason, develop the isotropy heat-conducting glue that a kind of thermal conductivity height, thermal resistance are stable, physical strength is good is badly in need of very much.Monodimension nanometer material is owing to thermal property, mechanical property and good chemical stability with special structure and uniqueness are widely studied and applied.Wherein nano silver wire is owing to radius-of-curvature little suitable " point discharge ", and it is less to have good field emissivity and threshold field, and emission and emission bit density are higher.The one dimension nano silver wire both can have been given full play to the advantage of the fibrous texture of nano wire as the heat conductive filler of heat-conducting glue, in the resin matrix of heat-conducting glue, form the heat conduction network better, can bring into play a tunnel conduction effect and an emission conduction effect of nanoparticle again.Adopt nano silver wire and Nano silver grain mixed powder to prepare a kind of high-performance thermal conductive in this patent as the heat conductive filler of heat-conducting glue.This heat-conducting glue that makes has good heat conductivility (thermal conductivity reaches 22W/ (m.K)), and very high shear strength (shear strength when being substrate with Al is 20MPa).
Summary of the invention
The purpose of this invention is to provide a kind of isotropy high-performance thermal conductive and preparation method thereof.
A kind of isotropy high-performance thermal conductive, component is by weight calculating: Resins, epoxy: 3～4 parts; CTBN modified epoxy: 13～15 parts; The mixed powder of nano silver wire and Nano silver grain: 60～70 parts; Aerosil: 0.5～2 part; Silane coupling agent: 0.5～2 part; Anhydride curing agent: 12～14 parts; Curing catalyst: 1～3 part.
Above-mentioned isotropy high-performance thermal conductive, Resins, epoxy are bisphenol A-type E51, E44, EPON828 or EPON826.
Above-mentioned isotropy high-performance thermal conductive, anhydride curing agent are methyl tetrahydro phthalic anhydride or methyl hexahydrophthalic anhydride.
Above-mentioned isotropy high-performance thermal conductive, curing catalyst are DMP-30 or 2-ethyl-4-Methylimidazole.
Above-mentioned isotropy high-performance thermal conductive, except that the mixed powder of nano silver wire and Nano silver grain, other components are technical grade, i.e. technical grade Resins, epoxy; The technical grade anhydride type curing agent; The technical grade curing catalyst; Technical grade CTBN modified epoxy, technical grade aerosil, technical grade silane coupling agent; Above reagent does not all pass through purification process;
In the above-mentioned isotropy high-performance thermal conductive, the preparation method of the mixed powder of nano silver wire and Nano silver grain is:
With AgNO
3The ethylene glycol solution and the ethylene glycol solution of polyvinylpyrrolidone (PVP) join in the ethylene glycol solution and mix, add sodium-chlor then, this mixing solutions is reacted 10～15min under the microwave power of 800～1000W, reaction finishes the back, and to add volume in mixing solutions be the acetone of 2～3 times of mixed liquor volumes, and then the mixing solutions that will be mixed with acetone carries out centrifugation 10～20min under 3000～4000 rev/mins of speed; Remove upper solution, in lower floor's solid, add acetone and wash the back recentrifuge, be the mixed powder of nano silver wire and Nano silver grain after the pressed powder drying that obtains.
AgNO
3The concentration of ethylene glycol solution be 0.1～0.5mol/l, the concentration of the ethylene glycol solution of polyvinylpyrrolidone is AgNO
34～6 times of concentration of ethylene glycol solution;
With AgNO
3Ethylene glycol solution and the ethylene glycol solution of polyvinylpyrrolidone join when mixing in the ethylene glycol solution AgNO
3Ethylene glycol solution and the adding speed of the ethylene glycol solution of polyvinylpyrrolidone be 10 droplets/minute;
The amount of substance that adds sodium-chlor is that one of percentage of AgNO3 amount of substance is to 3 percent.
AgNO
3Be anhydrous nitric acid silver, mass percentage concentration is 99.9%;
C
2H
6O
2Be no water glycol, mass percentage concentration is 99.8%;
The mass percentage concentration of polyvinylpyrrolidone is 98%;
Sodium-chlor is analytical pure.
The preparation method of above-mentioned isotropy high-performance thermal conductive, it is characterized in that: the mixed powder of nano silver wire and Nano silver grain is joined Resins, epoxy in proportion, in the hybrid resin system of CTBN modified epoxy and aerosil, in the high speed shear mixing machine, carry out combination treatment 20～30s, in the colloid that mixes, add acid anhydride type curing agent and curing catalyst then, again colloid mixture is placed the high speed shear mixing machine to carry out combination treatment 20～30s, promptly obtain the isotropy high-performance thermal conductive, the colloid after mixing places refrigerator to preserve.
The beneficial effect that the present invention has is: adopt the nano silver wire and the nanoparticle mixture of the preparation of microwave-assisted oxidation reduction process to prepare a kind of isotropy high-performance thermal conductive as the heat conductive filler filling epoxy resin.This heat-conducting glue has the thermal conductivity height than traditional heat-conducting glue, mechanical property, steady performance.This method cost for preparing the isotropy high-performance thermal conductive adhesive is low, and method is simple, and controllability is good, has very high practical value for the development of Electronic Packaging industry and high-capacity LED Packaging Industry.
Description of drawings
Fig. 1 is by the nano silver wire of embodiment one preparation and scanning electron microscope (SEM) photo of Nano silver grain mixed powder
Fig. 2 transmission electron microscope of mixed powder (TEM) photo that has been the nano silver wire of embodiment one preparation and nano grain of silver
Embodiment
Embodiment 1:
AgNO with 50ml0.3mol/l
3The PVP ethylene glycol solution of ethylene glycol solution and 50ml2mol/l splashes into simultaneously in the ethylene glycol solution of 150ml and mixes, and adds 0.01gNaCl then.This solution is placed industrial microwave oven, under the microwave power of 900W, react 12min.It is liquor capacity 500ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out centrifugation 10min under 4000 rev/mins of speed.Remove upper solution, in lower floor's solid, add 100ml acetone and wash the back recentrifuge, obtain pressed powder 40 ℃ of dry 24h in vacuum drying oven, be the mixed powder of nano silver wire and Nano silver grain.The test of transmission electron microscope observation (TEM) is that dried powder supersound process is dispersed in the toluene, then with drips of solution on the copper mesh that is coated with carbon film, drying at room temperature, TEM model are JEOL200CX.The sample of field emission scanning electron microscope (FESEM) is powdered sample to be dispersed in drop in the ethanol on the sample table, treat ethanol volatilization after, scanning electron microscopic observation, the scanning electron microscope model is FEI SIRION.What Fig. 1 showed is the prepared nano silver wire and the SEM photo of Nano silver grain mixed powder, can see among the figure that nanoparticle and nano wire are dispersed in the sample.What Fig. 2 showed is the TEM photo of preparation nano silver wire and nanoparticle mixed powder.
Embodiment 2:
AgNO with 50ml0.3mol/l
3The PVP ethylene glycol solution of ethylene glycol solution and 50ml1.2mol/l splashes into simultaneously in the ethylene glycol solution of 150ml and mixes, and adds 0.02gNaCl then.This solution is placed industrial microwave oven, under the microwave power of 900W, react 12min.It is liquor capacity 500ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out centrifugation 20min under 3000 rev/mins of speed.Remove upper solution, in lower floor's solid, add 100ml acetone and wash the back recentrifuge, obtain pressed powder 40 ℃ of dry 24h in vacuum drying oven, be the mixed powder of nano silver wire and Nano silver grain.
Each constituent mass proportioning is as follows in the concrete prescription of high-performance isotropy heat-conducting glue: Resins, epoxy: 3.4 parts; CTBN modified epoxy: 14.5 parts; Nano silver wire and Nano silver grain: 67.5 parts; Aerosil: 0.7 part; Silane coupling agent: 0.6 part; Methyl tetrahydro phthalic anhydride: 12.2 parts; DMP-30:1.2 part.The concrete preparation process of colloidal is: the mixed powder of nano silver wire and Nano silver grain is proportionally added in the hybrid resin system of Resins, epoxy, CTBN modified epoxy and aerosil, in the high speed shear mixing machine, carry out combination treatment 30s, in the colloid that mixes, add methyl tetrahydro phthalic anhydride solidifying agent and DMP-30 then, colloid mixture is placed the high speed shear mixing machine to carry out combination treatment 30s, packing is preserved again.Table 1 is the The performance test results by the isotropy high-performance thermal conductive of embodiment two preparations.As can be seen from Table 1, this heat-conducting glue that makes has good heat conductivility (thermal conductivity reaches 22W/ (m.K)), and very high shear strength (shear strength when being substrate with Al is 20MPa).
The The performance test results of table 1 isotropy high-performance thermal conductive
Embodiment 3:
AgNO with 10ml0.1mol/l
3The PVP ethylene glycol solution of ethylene glycol solution and 10ml0.4mol/l splashes into simultaneously in the ethylene glycol solution of 30ml and mixes, and adds 0.002gNaCl then.This solution is placed industrial microwave oven, under the microwave power of 800W, react 10min.It is liquor capacity 100ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out centrifugation 15min under 3500 rev/mins of speed.Remove upper solution, in lower floor's solid, add 100ml acetone and wash the back recentrifuge, obtain pressed powder 40 ℃ of dry 24h in vacuum drying oven, be the mixed powder of nano silver wire and Nano silver grain.
Each constituent mass proportioning is as follows in the concrete prescription of high-performance isotropy heat-conducting glue: Resins, epoxy: 4 parts; CTBN modified epoxy: 14 parts; Nano silver wire and Nano silver grain: 66 parts; Aerosil: 1 part; Silane coupling agent: 1 part; Methyl hexahydrophthalic anhydride solidifying agent: 13 parts; 2-ethyl-4-methylimidazole: 1 part.The concrete preparation process of colloidal is: the mixed powder of nano silver wire and Nano silver grain is proportionally added in the hybrid resin system of Resins, epoxy, CTBN modified epoxy and aerosil, in the high speed shear mixing machine, carry out combination treatment 30s, in the colloid that mixes, add methyl hexahydrophthalic anhydride solidifying agent and curing catalyst 2-ethyl-4-methylimidazole then, colloid mixture is placed the high speed shear mixing machine to carry out combination treatment 20s, preserve the packing back again.
Embodiment 4:
AgNO with 10ml0.5mol/l
3The PVP ethylene glycol solution of ethylene glycol solution and 10ml3.0mol/l splashes into simultaneously in the ethylene glycol solution of 30ml and mixes, and adds 0.01gNaCl then.This solution is placed industrial microwave oven, under the microwave power of 1000W, react 15min.It is liquor capacity 150ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out centrifugation 12min under 4000 rev/mins of speed.Remove upper solution, in lower floor's solid, add 100ml acetone and wash the back recentrifuge, obtain pressed powder 40 ℃ of dry 24h in vacuum drying oven,, be the mixed powder of nano silver wire and Nano silver grain.
Each constituent mass proportioning is as follows in the concrete prescription of high-performance isotropy heat-conducting glue: Resins, epoxy: 3 parts; CTBN modified epoxy: 15 parts; Nano silver wire and Nano silver grain: 67 parts; Aerosil: 0.5 part; Silane coupling agent: 0.5 part; Methyl tetrahydro phthalic anhydride solidifying agent: 12 parts; 2-ethyl-4-methylimidazole: 2 parts.The concrete preparation process of colloidal is: the mixed powder of nano silver wire and Nano silver grain is proportionally added in the hybrid resin system of Resins, epoxy, CTBN modified epoxy and aerosil, in the high speed shear mixing machine, carry out combination treatment 20s, in the colloid that mixes, add methyl tetrahydro phthalic anhydride solidifying agent and 2-ethyl-4-methylimidazole then, colloid mixture is placed the high speed shear mixing machine to carry out combination treatment 30s, packing is preserved again.
Claims (10)
1, a kind of isotropy high-performance thermal conductive, component is by weight calculating: Resins, epoxy: 3～4 parts; CTBN modified epoxy: 13～15 parts; The mixed powder of nano silver wire and Nano silver grain: 60～70 parts; Aerosil: 0.5～2 part; Silane coupling agent: 0.5～2 part; Anhydride curing agent: 12～14 parts; Curing catalyst: 1～3 part.
2, heat-conducting glue according to claim 1 is characterized in that: Resins, epoxy is bisphenol A-type E51, E44, EPON828 or EPON826.
3, heat-conducting glue according to claim 1 is characterized in that: anhydride curing agent is methyl tetrahydro phthalic anhydride or methyl hexahydrophthalic anhydride, and curing catalyst is DMP-30 or 2-ethyl-4-Methylimidazole.
4, heat-conducting glue according to claim 1 is characterized in that: except that the mixed powder of nano silver wire and Nano silver grain, other components are technical grade, i.e. technical grade Resins, epoxy; The technical grade anhydride type curing agent; The technical grade curing catalyst; Technical grade CTBN modified epoxy, technical grade aerosil, technical grade silane coupling agent; Above reagent does not all pass through purification process.
5, heat-conducting glue according to claim 1 is characterized in that: the preparation method of the nano silver wire in the heat-conducting glue and the mixed powder of Nano silver grain is: with AgNO
3The ethylene glycol solution and the ethylene glycol solution of polyvinylpyrrolidone (PVP) join in the ethylene glycol solution and mix, add sodium-chlor then, this mixing solutions is reacted 10～15min under the microwave power of 800～1000W, reaction finishes the back, and to add volume in mixing solutions be the acetone of 2～3 times of mixed liquor volumes, and then the mixing solutions that will be mixed with acetone carries out centrifugation 10～20min under 3000～4000 rev/mins of speed; Remove upper solution, in lower floor's solid, add acetone and wash the back recentrifuge, be the mixed powder of nano silver wire and Nano silver grain after the pressed powder drying that obtains.
6, the preparation method of the mixed powder of nano silver wire according to claim 6 and Nano silver grain is characterized in that: AgNO
3The concentration of ethylene glycol solution be 0.1～0.5mol/l, the concentration of the ethylene glycol solution of polyvinylpyrrolidone is AgNO
34～6 times of concentration of ethylene glycol solution.
7, the preparation method of the mixed powder of nano silver wire according to claim 6 and Nano silver grain is characterized in that: with AgNO
3Ethylene glycol solution and the ethylene glycol solution of polyvinylpyrrolidone join when mixing in the ethylene glycol solution AgNO
3Ethylene glycol solution and the adding speed of the ethylene glycol solution of polyvinylpyrrolidone be 10 droplets/minute.
8, the preparation method of the mixed powder of nano silver wire according to claim 6 and Nano silver grain is characterized in that: the amount of substance that adds sodium-chlor is that one of percentage of AgNO3 amount of substance is to 3 percent.
9, the preparation method of the mixed powder of nano silver wire according to claim 6 and Nano silver grain is characterized in that:
AgNO
3Be anhydrous nitric acid silver, mass percentage concentration is 99.9%;
C
2H
6O
2Be no water glycol, mass percentage concentration is 99.8%;
The mass percentage concentration of polyvinylpyrrolidone is 98%;
Sodium-chlor is analytical pure.
10, the preparation method of the described heat-conducting glue of claim 1, it is characterized in that: the mixed powder of nano silver wire and Nano silver grain is joined in the hybrid resin system of Resins, epoxy, CTBN modified epoxy and aerosil in proportion, in the high speed shear mixing machine, carry out combination treatment 20～30s, in the colloid that mixes, add acid anhydride type curing agent and curing catalyst then, again colloid mixture is placed the high speed shear mixing machine to carry out combination treatment 20～30s, promptly obtain the isotropy high-performance thermal conductive.
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