CN101475787B - 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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- CN101475787B CN101475787B CN2009100291256A CN200910029125A CN101475787B CN 101475787 B CN101475787 B CN 101475787B CN 2009100291256 A CN2009100291256 A CN 2009100291256A CN 200910029125 A CN200910029125 A CN 200910029125A CN 101475787 B CN101475787 B CN 101475787B
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- ethylene glycol
- nano silver
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- thermal conductive
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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 miniaturized, 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 the heat-conducting glue at heat radiation and heat transfer position; Can in time loose and remove a large amount of heats that produce in the electronics use, all significant to its safety of densification, miniaturized and raising, precision and the work-ing life of electronic product.
The heat conductive filler that uses in the heat-conducting glue at present mainly comprises following several kinds: a kind of is that nitride and the carbide with good insulation properties and high thermal conductivity coefficient mainly comprises aluminium nitride AlN, SP 1, silicon nitride, silit, norbide and titanium carbide etc.Also having a kind of is that MOX such as beryllium oxide, aluminum oxide, Natural manganese dioxide 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 thomel with high heat-conductivity conducting property; 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 like domestic patent CN1061235, CN1970666, CN1880399 and CN1966597.These heat-conducting glues are owing to receive the restriction of adopting 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 is high, thermal resistance is stable, physical strength is good is badly in need of very much.Monodimension nanometer material is owing to have particular structural and unique thermal property, mechanical property and good chemicalstability and by broad research and application.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 is higher with the emission bit density.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 are by weight calculating: epoxy resin: 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, epoxy resin 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 epoxy resin; 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 of ethylene glycol solution and Vinylpyrrolidone polymer (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 in mixing solutions, to add volume be the acetone of 2～3 times of mixed liquor volumes, and then the mixing solutions that will be mixed with acetone carries out spinning 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 Vinylpyrrolidone polymer is AgNO
34～6 times of concentration of ethylene glycol solution;
With AgNO
3Ethylene glycol solution and the ethylene glycol solution of Vinylpyrrolidone polymer join when mixing in the ethylene glycol solution AgNO
3The adding speed of ethylene glycol solution of ethylene glycol solution and Vinylpyrrolidone polymer 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 Vinylpyrrolidone polymer 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 in the hybrid resin system of epoxy resin, 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; Place the high speed shear mixing machine to carry out combination treatment 20～30s colloid mixture again, 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 mixtinite 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 ESEM (SEM) photo of Nano silver grain mixed powder
Fig. 2 is the nano silver wire of embodiment one preparation and transmission electron microscope (TEM) photo of Nano silver grain mixed powder
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, reaction 12min under the microwave power of 900W.It is liquor capacity 500ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out spinning 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 ESEM 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, reaction 12min under the microwave power of 900W.It is liquor capacity 500ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out spinning 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 following in the concrete prescription of high-performance isotropy heat-conducting glue: epoxy resin: 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.Specifically 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 epoxy resin, 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; Place the high speed shear mixing machine to carry out combination treatment 30s colloid mixture again, packing is preserved.Table 1 is the The performance test results by the isotropy high-performance thermal conductive of embodiment two preparations.Can find out that 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, reaction 10min under the microwave power of 800W.It is liquor capacity 100ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out spinning 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 following in the concrete prescription of high-performance isotropy heat-conducting glue: epoxy resin: 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.Specifically 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 epoxy resin, 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; Place the high speed shear mixing machine to carry out combination treatment 20s colloid mixture again, preserve the packing back.
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, reaction 15min under the microwave power of 1000W.It is liquor capacity 150ml acetone that reaction finishes back adding volume in solution, then mixing solutions is carried out spinning 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 following in the concrete prescription of high-performance isotropy heat-conducting glue: epoxy resin: 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.Specifically 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 epoxy resin, 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; Place the high speed shear mixing machine to carry out combination treatment 30s colloid mixture again, packing is preserved.
Claims (1)
1. isotropy high-performance thermal conductive, component are by weight calculating: epoxy resin: 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; The preparation method of the mixed powder of said nano silver wire and Nano silver grain is: with AgNO
3The ethylene glycol solution of ethylene glycol solution and Vinylpyrrolidone polymer (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 in mixing solutions, to add volume be the acetone of 2 ~ 3 times of mixed liquor volumes, and then the mixing solutions that will be mixed with acetone carries out spinning 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, said AgNO
3The concentration of ethylene glycol solution be 0.1 ~ 0.5mol/l, the concentration of the ethylene glycol solution of Vinylpyrrolidone polymer is AgNO
34 ~ 6 times of concentration of ethylene glycol solution, with AgNO
3Ethylene glycol solution and the ethylene glycol solution of Vinylpyrrolidone polymer join when mixing in the ethylene glycol solution AgNO
3The adding speed of ethylene glycol solution of ethylene glycol solution and Vinylpyrrolidone polymer be 10 droplets/minute, the amount of substance that adds sodium-chlor is AgNO
3One of percentage of amount of substance is to 3 percent.
2. a kind of isotropy high-performance thermal conductive according to claim 1 is characterized in that: epoxy resin is bisphenol A-type E51, E44, EPON828 or EPON826.
3. a kind of isotropy high-performance thermal conductive 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. a kind of isotropy high-performance thermal conductive 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 epoxy resin; 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. a kind of isotropy high-performance thermal conductive according to claim 1 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 Vinylpyrrolidone polymer is 98%;
Sodium-chlor is analytical pure.
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| CN103087665B (en) * | 2013-01-31 | 2015-05-06 | 合肥工业大学 | High-heat-conductivity insulation low-viscosity epoxy resin pouring sealant and preparation method thereof |
| JP6349543B2 (en) * | 2013-12-25 | 2018-07-04 | パナソニックＩｐマネジメント株式会社 | COOLING STRUCTURE AND METHOD FOR MANUFACTURING COOLING STRUCTURE |
| CN104227017B (en) * | 2014-09-28 | 2017-01-11 | 重庆文理学院 | Preparation method of silver nanoparticle with controllable particle size |
| CN104974470B (en) * | 2015-07-14 | 2017-12-05 | 江苏兆鋆新材料股份有限公司 | A kind of high heat-resisting, high strength epoxy resin composite preparation method |
| CN106001601B (en) * | 2016-06-01 | 2018-02-13 | 合肥银派科技有限公司 | Nano silver wire conduction liquid that a kind of surface is modified and preparation method thereof |
| CN106180749B (en) * | 2016-07-23 | 2018-07-17 | 常州大学 | It is a kind of doping big L/D ratio nano-silver thread graphene preparation method and its application in terms of preparing conducting resinl |
| CN106735294A (en) * | 2016-12-11 | 2017-05-31 | 浙江大学 | The preparation method of nano silver wire |
| CN108695438B (en) * | 2017-04-12 | 2019-12-13 | Tcl集团股份有限公司 | QLED device, display device and preparation method thereof |
| CN108157387B (en) * | 2017-11-27 | 2021-01-05 | 东南大学 | Silver nanowire antibacterial aerogel and preparation method and application thereof |
| DE102019211178B3 (en) * | 2019-07-26 | 2020-09-17 | Tesa Se | Process for sheathing elongated goods, sheathed goods and their use |
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| CN1546591A (en) * | 2003-12-09 | 2004-11-17 | 清华大学 | High connecting intensity thermosetting conducting resin |
| CN1948414A (en) * | 2006-11-13 | 2007-04-18 | 浙江理工大学 | Method of preparing high performance conductive glue |
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