CN103911006A - Thermal conduction composite material and manufacture method thereof - Google Patents
Thermal conduction composite material and manufacture method thereof Download PDFInfo
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- CN103911006A CN103911006A CN201310001028.2A CN201310001028A CN103911006A CN 103911006 A CN103911006 A CN 103911006A CN 201310001028 A CN201310001028 A CN 201310001028A CN 103911006 A CN103911006 A CN 103911006A
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Abstract
The invention relates to a thermal conduction composite material and a manufacture method, the composite material comprises a high-molecular polymer containing a high-molecular material capable of performing free radical reaction and a peroxide capable of polymerizing the high-molecular material through free radical reaction; a heat conduction filling material which at least contains two heat conduction materials with compatible property; and a silane object which at least contains two different functional groups, wherein, one functional group can participate in a free radical polymerization of a high-molecular polymer, and another functional group is capable of generating a chemical bonding on the surface of the heat conduction filling material. The thermal conduction composite material has the efficacy of reducing contact thermal resistance and material thermal resistance.
Description
Technical field
The present invention is relevant a kind of thermal conduction matrix material and manufacture method, espespecially a kind of design with reduction thermal contact resistance and material thermal resistance effect.
Background technology
The exploitation of electronic product is more and more compact, and the consequent is that the stability of product is more beneficial important, the importance of the heat management aspect that therefore more seems; And no matter be which kind of kenel (for example notebook computer, desktop computer, mobile phone or Other Instruments device), the generation of heat stems from the working at high speed of electronic package, the heat (being called thermal source) of its generation, if do not reduce its temperature within the short period of time, by hot migration low temperature (hot well), electronic package has the possibility of damage, causes the electronic product life-span to reduce or the unsettled problem of quality.
But by heat, by thermal source migration hot well, it has three approach, is respectively radiation, convection current and conduction, and the most effective with conduction; While removing heat, can be the approach of one of them, or two kinds of approach merge, look closely the heat management mode of apparatus and determine.In the situation of electronic package or apparatus inside, in the majority with convection current and pathway, and the effect of pathway is better than convection current approach, this be because of the thermal impedance of solid far below the thermal impedance of gas therefore.Moreover the point that thermal source contacts each other with hot well is more, its thermal impedance is lower, and when thermal source surface is more tending towards smooth with hot well surface, in the time of this two flat surfaces contact, the remaining space not touching is fewer, heat conducting effect is better, and this is because there is low thermal impedance.
Therefore,, when thermal source surface is fewer because contacting produced space with hot well surface, then thermal convection approach is changed into heat conduction path, and this hot well is popular known heat sink material, thermally conductive material or interface thermally conductive material; When this approach changes, its objective is the thermal impedance that is to reduce contact surface, therefore thermal impedance is lower, is to be more conducive to removing of thermal source surface heat; But, except the thermal impedance at thermal source surface and hot well Surface Contact interface, when hot well is manufactured, the contact surface of each stock yard, is also another key that affects thermal impedance.
In addition, the elastic layer of the TWI325752 of tw Taiwan has disclosed thermal radiation sheet metal assembly one graphite thin plate and one deck electrical isolation in its surface, elastic layer is formed by a kind of elasticity constituent, and elasticity constituent comprises a kind of particulate thermal conductivity filler; The TWM412971 of tw Taiwan discloses a kind of heat radiator, comprise a heat radiation main body and a protective layer, heat radiation main body is a graphite substrate, protective layer is coated this graphite substrate at least partly, wherein the material of protective layer is synthetic resins or natural resin, and face is by protective layer being set in graphite substrate to improve the shortcoming of heat radiator dry linting; The TW201024399 of tw Taiwan discloses a kind of carbon containing metal composite and preparation method thereof, and carbon containing metal composite comprises multiple graphite, multiple heat conduction particle and a metal matrix.
Therefore, above taking off patent, as graphite that we know, aluminum oxide, zinc oxide, aluminium nitride, boron nitride, aluminium powder, copper powder etc., is all the heat conductive filler with very good thermal conduction effect; But, if exist with single filler kenel, for example single graphite heat conducting homogeneous layer or graphite substrate, and nothing is that a basic substance forms multiple material with the compound of tool chemical bonded refractory, graphite heat conducting homogeneous layer, graphite substrate or metal composite, mechanical properties can not be better than having the compound of chemical bonded refractory, for example bendability and flexibility or impose small strength outward, and its structure has the anxiety of disintegration; Moreover graphite heat conducting passes homogeneous layer, graphite substrate or carbon containing metal composite, for the contact interface of pyrotoxin, its thermal contact resistance can, higher than the compound with chemical bonded refractory, reduce thermal conduction effect.
In addition, the TWM308849 of tw Taiwan discloses a kind of multilayer materials, comprise one or some heat-conducting layers and one or some electromagnetic wave absorbing layers, and between each layer,, each other with mutual stacked and connect airtight composition, selecting one or both thermal conduction powders collocation between one or both glue materials and 90%～30% between ratio 10%～70% is heat-conducting layer; The heat dissipation film that the TWM390642 of tw Taiwan discloses, formed by a graphite material and a resin material, the weighting material in resin material is zirconium white, cerium oxide, aluminum oxide, carbon nanotube, ferric oxide, magnesium oxide, zinc oxide, titanium oxide and rice oxide compound how; The TW201012910 of tw Taiwan discloses a kind of thermal conduction composite bed, comprise gel heat-conducting layer and release layer, heat-conducting layer weighting material comprises alumina powder, boron nitride powder, aln precipitation powder, magnesium oxide powder, Zinc oxide powder, silicon carbide powder, quartz powder, aluminium-hydroxide powder, carbon fiber powder, diamond powder, powdered graphite, single one or more combinations of aluminium powder; The TWI273118 of tw Taiwan discloses multiple material, by natural graphite, synthetic graphite, expanded graphite, carbon black, carbon fibre, vapor phase process carbon fibre, the carbon nanotubes of boracic, make with phenol resins, unsaturated polyester resin, epoxy resin, vinylester resin, propylene resin; The TW200837083 of tw Taiwan discloses the multiple material of conductivity, is made up of a polyolefin polymer and the graphite expanding; The TWM401536 of tw Taiwan discloses convenient heavily glutinous appropriate composite guide radiator structure, be made up of from stickiness silica gel in thermosetting cement, a metal base and one deck of pottery magnetic powder one deck pottery magnetic powder constituent and filling, pottery magnetic powder constituent can be silicon carbide, aluminium nitride, zinc oxide, aluminum oxide or is replaced by graphite.
So, on take off patent make thermally conductive material, the heat conductive filler and the sizing material that use are well-known skill, but it mixes each other to heat conductive filler and glue material, use one or more heat conductive filler or one or more glue material no matter be, the most important thing is the compatibility of storeroom, thus between different heat conductive fillers or between glue material and heat conductive filler compatibility want high, the thermally conductive material of made just has low thermal impedance; Therefore,, if use two or more heat conductive fillers, select the heat conductive filler that similarity is high, allow the compatibility between heat conductive filler promote, and heat conductive filler is also used to interface modification agent, improve the compatibility between heat conductive filler and glue material, so could make preferably thermally conductive material.
Summary of the invention
Technical problem underlying to be solved by this invention is, overcomes the above-mentioned defect that prior art exists, and a kind of thermal conduction matrix material and manufacture method are provided, and it has the effect that reduces thermal contact resistance and material thermal resistance.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of thermal conduction matrix material, is characterized in that, comprising: high molecular polymer, the macromolecular material that comprises free redical reaction with can be by this macromolecular material the superoxide with free radical reaction polymerization; Heat conductive filler, at least comprises the thermally conductive material of two kinds of character compatibilities; And silane thing, at least comprising two kinds of different functional groups, a kind of functional group can participate in this high molecular polymer Raolical polymerizable, and another kind of functional group can be in this heat conductive filler Surface Creation chemical bonded refractory.
In addition, this macromolecular material is the polydimethylsiloxane that contains at least two vinyl functional group; This heat conductive filler contains tool hole and compressible graphite composite powder and the composite inorganic material that wraps up graphite with nickel; This silane thing contains vinyl and alkoxyl group.Again, this heat conductive filler has compressibility with the composite inorganic material of nickel parcel graphite and the blending of graphite composite powder, reduces thermal impedance to reduce graphite composite powder to form the space after sheet; The characteristic of the acid and absorption moisture content of graphite essence, cause the alkoxyl group of this silane thing that the chemical reaction of hydrolytic condensation occurs with it, and form chemical bond in graphite surface, make graphite surface because thering is vinyl with the combination of this silane thing, and then participate in the polyreaction that this macromolecular material occurs by superoxide, cause graphite and high molecular polymer to form chemical bond, reduce thermal impedance to reduce the space between high molecular polymer and filler.Moreover, further close layer at least one side composite gum of this thermal conduction matrix material, this cementing layer can be glutinous and does not touch with one's hand or do not have tackyness completely, look closely purposes and determine, this cementing layer is made up of add-on type liquid macroimolecule material and the macromolecular material that reacts with this high molecular polymer free redical is all take siloxanes polymer as main chain, and this add-on type liquid macroimolecule material is formed through polyaddition reaction by two kinds of macromolecular materials that at least contain vinyl and hydrogen base.Separately, the temperature of this high molecular polymer polyreaction is 150～200 ℃, and the time is 2～10 minutes.
Thermal conduction method for composite material of the present invention, comprise the following steps: that a. takes the macromolecular material of free redical reaction, and the amount of taking accounts for the more than 50% of macromolecular material aggregate demand; B. add contain can participate in macromolecular material free radical reaction with can be in the silane thing of heat conductive filler Surface Creation chemical bonded refractory, and add-on accounts for silane thing aggregate demand below 50%, and the silane thing adding is mixed with the macromolecular material of taking in step a; C. add the heat conductive filler that at least comprises the compatible thermally conductive material of two kinds of character, and add-on accounts for heat conductive filler aggregate demand below 50%, and the heat conductive filler adding is mixed with the mixture of completing steps b, until mixture outward appearance presents light or occurs without obvious filler; D. add the silane thing identical with step b, and add-on accounts for silane thing aggregate demand below 50%, and the silane thing adding is mixed with the mixture of completing steps c; E. add the heat conductive filler identical with step c, and add-on accounts for heat conductive filler aggregate demand below 50%, and the heat conductive filler adding is mixed with the mixture of completing steps d, until mixture outward appearance presents light or occurs without obvious filler; F. repeating step d and step e, until the aggregate demand of silane thing and heat conductive filler adds completely; G. add and macromolecular material can be mixed with the mixture of completing steps f with the superoxide of free radical reaction polymerization and the mixture of remaining macromolecular material; And h. takes out the mixture of completing steps g, high-pressure and vacuumizing and moulding.
Another person, the macromolecular material amount of taking of step a accounts for macromolecular material aggregate demand 85～95%, the silane thing add-on of step b and steps d accounts for silane thing aggregate demand 25～40%, and the heat conductive filler add-on of step c and step e accounts for heat conductive filler aggregate demand 25～40%.Again, the macromolecular material amount of taking of step a accounts for macromolecular material aggregate demand 90%, and the silane thing add-on of step b and steps d accounts for silane thing aggregate demand 33.3%, and the heat conductive filler add-on of step c and step e accounts for heat conductive filler aggregate demand 33.3%.Moreover step c carries out in decompression and in being warming up to the environment of 100～130 ℃ to step f, the auxiliary effect of puddling; Step g is carried out in the environment of room temperature; Step h carries out in the environment that is warming up to 150～200 ℃.Separately, step c carries out in decompression and in being warming up to the environment of 110 ℃ to step f; Step h carries out in the environment that is warming up to 170 ℃.
The invention has the beneficial effects as follows, it has the effect that reduces thermal contact resistance and material thermal resistance.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is thermal conduction composite structure schematic diagram of the present invention.
Fig. 2 is the process flow chart of thermal conduction method for composite material of the present invention.
Number in the figure explanation:
10 high molecular polymers
20 heat conductive fillers
21 graphite composite powders
22 composite inorganic materials
30 silane things
Embodiment
First, refer to shown in " Fig. 1 ", thermal conduction matrix material of the present invention, is take high molecular polymer 10 as base material mixing heat conductive filler 20 and containing functional group's silane thing 30; The macromolecular material that this high molecular polymer 10 has comprised free redical reaction and can be by this macromolecular material the superoxide with free radical reaction polymerization, and the temperature of polyreaction is preferably 150～200 ℃, time is 2～10 minutes, better temperature is 170 ℃, time is 5 minutes, and then the high molecular polymer of acquisition slaking, this macromolecular material is the polydimethylsiloxane that contains at least two vinyl functional group; This heat conductive filler 20 has at least comprised two kinds of heat conductivity things that character is very compatible, and wherein one is tool hole and compressible graphite composite powder 21, and another kind of is the composite inorganic material 22 take nickel as outer parcel graphite as internal layer; At least contain two kinds of different functional groups containing functional group's silane thing 30, the macromolecular material that wherein a kind of functional group can participate in the reaction of above-mentioned free redical simultaneously carries out Raolical polymerizable, more suitable functional group is vinyl, another kind of functional group can be in graphite packing Surface Creation chemical bonded refractory, and more suitable functional group is alkoxyl group.
Moreover, referring to shown in " Fig. 2 ", thermal conduction method for composite material of the present invention, first, takes the macromolecular material of the free redical reaction of aggregate demand 85%～95%, and more suitable consumption is 90%; Continue, add mixing containing functional group's silane thing of aggregate demand 25～40%, more suitable consumption is 33.3%, and application two cylinders, pug mill type mixer or three cylinders are mixed, and more suitable machine is pug mill type mixer; Continue, add the heat conductive filler (being pre-mixed the thermally conductive material that at least comprises two kinds of character compatibilities) of aggregate demand 25～40% to mix, more suitable consumption is 33.3%, and in reduced pressure atmosphere, carry out simultaneously, until mixture outward appearance presents light, glossy or obviously filler appearance of nothing, now can outside hot water or hot coal wet goods dielectric heating to 100～130 ℃, more suitable temperature is 110 ℃, the auxiliary effect of puddling; Continue, again add mixing containing functional group's silane thing of aggregate demand 25～40%, more suitable consumption is 33.3%, mixes with identical temperature and identical reduced pressure atmosphere with identical mixer; Continue, again add the heat conductive filler of aggregate demand 25～40% to mix, more suitable consumption is 33.3%, mixes, until mixture outward appearance presents light, glossy or occur without obvious filler with identical mixer with identical temperature and identical reduced pressure atmosphere; Continue, add remaining functional group's silane thing that contains to mix, the reduced pressure atmosphere identical with identical temperature skill with identical mixer mixes; Continue, add remaining heat conductive filler to mix, mix with identical temperature and identical reduced pressure atmosphere with identical mixer, until mixture outward appearance presents light, glossy or present without obvious filler; Continue, pass into the medium such as cold water or cold kerosene, outside temperature is down to room temperature; Continue, adding can be by macromolecular material with the superoxide of free radical reaction polymerization and the mixture of remaining macromolecular material, mixes with identical temperature and identical reduced pressure atmosphere with identical mixer; Continue, take out final mixture, relend oil press with high pressure and vacuumize moulding, need Heating temperature to 150～200 ℃ when moulding, the temperature of relatively expecting is 170 ℃; Whereby, go out between the heat conductive filler of two character compatibilities in heat conductive filler the thermal conduction matrix material between closely pressing and filler and macromolecular material with chemical bonded refractory via above program making.
Based on above-mentioned formation, in the heat conductive filler that the present invention uses, composite inorganic material take nickel as outer parcel graphite as internal layer, except having good compatibility with graphite composite powder, tool compressibility when itself and graphite composite powder blending, the space that graphite composite powder can be formed after sheet is filled, and has reduced freeboard in filler, and the solution route that reduces material thermal resistance is provided, in addition, by the characteristic of the acid of graphite essence and absorption moisture content, can there is with it the chemical reaction of hydrolytic condensation containing the alkoxyl group of functional group's silane thing, that is can form chemical bond in graphite surface containing functional group's silane thing, make graphite surface because thering is vinyl with the combination containing functional group's silane thing, when the macromolecular material of free redical reaction is during by superoxide polymerization reaction take place, vinyl can participate in this polyreaction in the lump, cause graphite and high molecular polymer to form chemical bond, except compound rear material surface is smooth and reduced the freeboard between high molecular polymer and filler, the solution route that reduces thermal contact resistance and material thermal resistance is provided.
Be so, the present invention is asymptotic expression and complete at heat conductive filler surface formation chemical bond, that is before adding heat conductive filler for the first time, the mixture of the existing macromolecular material reacting with free redical containing functional group's silane thing, now the solid content of heat conductive filler in this mixture is low, therefore have splendid blending effect, heat conductive filler can be dispersed in mixture, therefore control outside Heating temperature and the moisture content because of heat conductive filler essence acidic nature and absorption, can be hydrolyzed condensation chemical reaction and form chemical bonded refractory containing the alkoxyl group of functional group's silane thing, and then reach the mixture of the low-viscosity of expection, add when continuing and contain for the second time functional group's silane thing in this mixture, except obtaining the mixture that has low-viscosity more, also created and identical for the first time hybird environment, be conducive to add the blending of heat conductive filler for the second time and the hydrolytic condensation chemical reaction of generation expection, continue and add the hydrolytic condensation chemical reaction containing functional group's silane thing and the expection of thermal conductivity filler generation for the third time for the third time, through program like this, but be not limited to three times, it can be divided into four times or five times, consider time cost, more suitable number of times is three times, now can obtain uniform mixture, it is fashionable when superoxide is added, its macromolecular material take free redical reaction, as carrier, contributes to being dispersed in mixture of superoxide, shortens the blending time simultaneously, and the feed way of this gradation asymptotic expression completes the surfaction that generates chemical bonded refractory at filling surface when contributing to blending.
Another person, the present invention still can further provide cementing layer in the one or both sides of thermal conduction matrix material, and this cementing layer is not that the functional for strengthening thermal conduction matrix material is made, this cementing layer can be glutinous and does not touch with one's hand or do not have tackyness completely, look closely purposes and determine, this cementing layer is made up of add-on type liquid macroimolecule material, the macromolecular material that this add-on type liquid macroimolecule material reacts with above-mentioned free redical is same type, be all take siloxanes polymer as main chain, this add-on type liquid macroimolecule material is formed through polyaddition reaction by least two kinds of macromolecular materials, it is respectively and contains vinyl and hydrogen base, it can be via catalyzer, more suitable catalyzer is the catalyzer of platiniferous composition, they can be by vinyl and hydrogen base in the proper ratio in 130～170 ℃, more suitable temperature is 150 ℃, through 1～10 minute, relatively reasonable time is 5 minutes, can obtain cementing layer.But, before not yet generating cementing layer, can prior to the one side of thermal conduction matrix material with the mode of spraying appropriate add delayed-action activator, can add if desired solvent, again with above-mentioned temperature and time, with continous way processing procedure generation polyaddition reaction, can obtain and can generate chemical bonded refractory with the vinyl of thermal conduction matrix material in the one side of thermal conduction matrix material, and then form cementing layer glutinous and that do not touch with one's hand; Again, general make the glutinous of the multiple material of heat conduction and while not touching with one's hand cementing layer, be in mixture base material, to add silicone oil, this kind of mode must have the situation that silicone oil oozes out to occur, and the present invention's application base material itself is adjusted the suitable proportion of vinyl and hydrogen base, do not have the problem generation that silicone oil oozes out.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, any simple modification, equivalent variations and modification that every foundation technical spirit of the present invention is done above embodiment, all still belong in the scope of technical solution of the present invention.
In sum, the present invention is in structure design, use practicality and cost benefit, meet industry development completely required, and the structure disclosing is also to have unprecedented innovative structure, there is novelty, creativeness, practicality, meet the regulation about patent of invention important document, therefore mention application in accordance with the law.
Claims (10)
1. a thermal conduction matrix material, is characterized in that, comprising:
High molecular polymer, the macromolecular material that comprises free redical reaction with can be by this macromolecular material the superoxide with free radical reaction polymerization;
Heat conductive filler, at least comprises the thermally conductive material of two kinds of character compatibilities; And
Silane thing, at least comprises two kinds of different functional groups, and a kind of functional group can participate in this high molecular polymer Raolical polymerizable, and another kind of functional group can be in this heat conductive filler Surface Creation chemical bonded refractory.
2. thermal conduction matrix material according to claim 1, is characterized in that, described macromolecular material is the polydimethylsiloxane that contains at least two vinyl functional group; This heat conductive filler contains tool hole and compressible graphite composite powder and the composite inorganic material that wraps up graphite with nickel; This silane thing contains vinyl and alkoxyl group.
3. thermal conduction matrix material according to claim 2, is characterized in that, described heat conductive filler has compressibility with the composite inorganic material of nickel parcel graphite and the blending of graphite composite powder, reduces thermal impedance to reduce graphite composite powder to form the space after sheet; The characteristic of the acid and absorption moisture content of graphite essence, cause the alkoxyl group of this silane thing that the chemical reaction of hydrolytic condensation occurs with it, and form chemical bond in graphite surface, make graphite surface because thering is vinyl with the combination of this silane thing, and then participate in the polyreaction that this macromolecular material occurs by superoxide, cause graphite and high molecular polymer to form chemical bond, reduce thermal impedance to reduce the space between high molecular polymer and filler.
4. according to the thermal conduction matrix material described in claim 2 or 3, it is characterized in that, further close layer at least one side composite gum of described thermal conduction matrix material, this cementing layer can be glutinous and does not touch with one's hand or do not have tackyness completely, this cementing layer is made up of add-on type liquid macroimolecule material and the macromolecular material that reacts with this high molecular polymer free redical is all take siloxanes polymer as main chain, and this add-on type liquid macroimolecule material is formed through polyaddition reaction by two kinds of macromolecular materials that at least contain vinyl and hydrogen base.
5. thermal conduction matrix material according to claim 4, the temperature that it is characterized in that described high molecular polymer polyreaction is 150～200 ℃, the time is 2～10 minutes.
6. a thermal conduction method for composite material, is characterized in that, comprises the following steps:
A. take the macromolecular material of free redical reaction, and the amount of taking accounts for the more than 50% of macromolecular material aggregate demand;
B. add contain can participate in macromolecular material free radical reaction with can be in the silane thing of heat conductive filler Surface Creation chemical bonded refractory, and add-on accounts for silane thing aggregate demand below 50%, and the silane thing adding is mixed with the macromolecular material of taking in step a;
C. add the heat conductive filler that at least comprises the compatible thermally conductive material of two kinds of character, and add-on accounts for heat conductive filler aggregate demand below 50%, and the heat conductive filler adding is mixed with the mixture of completing steps b, until mixture outward appearance presents light or occurs without obvious filler;
D. add the silane thing identical with step b, and add-on accounts for silane thing aggregate demand below 50%, and the silane thing adding is mixed with the mixture of completing steps c;
E. add the heat conductive filler identical with step c, and add-on accounts for heat conductive filler aggregate demand below 50%, and the heat conductive filler adding is mixed with the mixture of completing steps d, until mixture outward appearance presents light or occurs without obvious filler;
F. repeating step d and step e, until the aggregate demand of silane thing and heat conductive filler adds completely;
G. add and macromolecular material can be mixed with the mixture of completing steps f with the superoxide of free radical reaction polymerization and the mixture of remaining macromolecular material; And
H. take out the mixture of completing steps g, high-pressure and vacuumizing and moulding.
7. thermal conduction method for composite material according to claim 6, it is characterized in that, the macromolecular material amount of taking of described step a accounts for macromolecular material aggregate demand 85～95%, the silane thing add-on of step b and steps d accounts for silane thing aggregate demand 25～40%, and the heat conductive filler add-on of step c and step e accounts for heat conductive filler aggregate demand 25～40%.
8. thermal conduction method for composite material according to claim 7, it is characterized in that, the macromolecular material amount of taking of described step a accounts for macromolecular material aggregate demand 90%, the silane thing add-on of step b and steps d accounts for silane thing aggregate demand 33.3%, and the heat conductive filler add-on of step c and step e accounts for heat conductive filler aggregate demand 33.3%.
9. according to the thermal conduction method for composite material described in claim 6,7 or 8, it is characterized in that, described step c carries out in decompression and in being warming up to the environment of 100～130 ℃ to step f, the auxiliary effect of puddling; Step g is carried out in the environment of room temperature; Step h carries out in the environment that is warming up to 150～200 ℃.
10. thermal conduction method for composite material according to claim 9, is characterized in that, described step c carries out in decompression and in being warming up to the environment of 110 ℃ to step f; Step h carries out in the environment that is warming up to 170 ℃.
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| CN201310001028.2A CN103911006B (en) | 2013-01-04 | 2013-01-04 | Heat transfer composite and manufacture method |
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| CN201310001028.2A CN103911006B (en) | 2013-01-04 | 2013-01-04 | Heat transfer composite and manufacture method |
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| CN103911006B (en) | 2017-07-28 |
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