CN103627179A - Graphene-containing silicone rubber composite material with high thermal conductivity and preparation method thereof - Google Patents
Graphene-containing silicone rubber composite material with high thermal conductivity and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of a heat conducting polymer-based composite, and particularly relates to a graphene-containing silicone rubber composite material with the high thermal conductivity and a preparation method thereof. The composite material comprises a matrix, a heat conducting filler and a vulcanizing agent. The preparation method comprises the following steps: mixing at a room temperature so as to obtain a mixed rubber material; and carrying out hot press molding and one-stage vulcanization on the mixed rubber material by using a flat vulcanizing machine, and putting in a drying oven, carrying out two-stage vulcanization, thus obtaining the silicone rubber composite material with the high thermal conductivity. As graphene is high in thermal conductivity and has a unique two-dimensional lamellar structure, an interconnected heat conducting network is easy to form in the composite material, and the thermal conductivity of the silicon rubber composite material is obviously increased; and the thermal conductivity of the graphene-containing silicone rubber composite material is 0.3W/m.K-1.5W/m.K, and the hardness of the silicone rubber composite material can be reduced. The graphene-containing silicone rubber composite material with the high thermal conductivity is simple in preparation technology, high in production efficiency and easy for the realization of industrialization mass production, and meanwhile, a direction is pointed out for the batch application of graphene.
Description
Technical field
The invention belongs to heat-conductivity polymer composite field, particularly a kind of high thermal conductive silicon rubber composite that contains Graphene and preparation method thereof.
Background technology
Along with Highgrade integration and the high-power of hyundai electronics chip technology, the Novel hot boundary material that development has high heat conductance has become the key issue that needs urgent solution.
The over-all properties that high temperature resistant, high voltage withstanding, resistance to ozone ageing that silicon rubber has, radiation hardness etc. are excellent is the hot interface body material extensively adopting in industry.Yet silicon rubber heat conductivility lower (thermal conductivity is only 0.15W/mK), is not suitable for being directly used as heat interfacial material, conventionally need to add heat conductive filler to improve its thermal conductivity.At present, conventional heat conductive filler mainly contains: metal-powder, aluminum oxide, boron nitride, silicon carbide etc., and because the thermal conductivity of these heat conductive fillers itself is lower, therefore only just can obtain higher thermal conductivity in the situation that loading level is very high.Yet the processing characteristics of filling in a large number the silicon rubber composite material of heat conductive filler declines, after sulfuration, hardness increases, and has affected to a great extent its usability.
In recent years, in order further to improve the thermal conductivity of silicon rubber composite material, fast-developing nano level high thermal conductivity filler Graphene attracts wide attention.Graphene has the following advantages as heat conductive filler:
(1) grapheme material has unique two-dimension phonon transport property, high theoretical thermal conductivity (up to 5150W/mK), is the highest material of current thermal conductivity;
(2) Graphene has very high radius-thickness ratio (up to more than 5000), very high specific surface area, and theoretical value is up to 2600m
2/ g, Graphene is high specific surface area so, can be conducive to improve itself and the interaction of matrix polymer, and enhancing interface bonding energy is better with the consistency of polymkeric substance;
(3) Graphene is two-dimensional slice structure, than other inorganic heat conductive fillers, is more easy to be scattered in polymeric matrix.
The advantage of comprehensive above Graphene, using Graphene as heat conductive filler, can be so that the thermal conductivity of matrix material be greatly improved.Yet, also few about the research of graphene/silicon rubber heat-conductive composite material, the research that the high-temperature silicon disulfide rubber of especially take is matrix.Chinese invention patent application (publication number CN103087404A) discloses a kind of Graphene filled polymer based composites and preparation method thereof, Graphene microplate is joined in the polymkeric substance such as PET, PS, PVC, can improve the thermal conductivity of matrix material.Chinese invention patent application (CN102827480A) discloses a kind of method of preparing high thermal conductive silicon rubber composite, and by add the thermal conductivity that expanded graphite improves silicon rubber in silicon rubber, but this method is loaded down with trivial details for the treatment process of graphite.
Summary of the invention
In order to overcome the low shortcoming of existing silicon rubber composite material thermal conductivity, the object of this invention is to provide a kind of high thermal conductive silicon rubber composite that contains Graphene and preparation method thereof, utilize the heat conductivility of Graphene excellence, and by optimal preparation technology, obtain that thermal conductivity is high, the high-performance heat-conductive composite material of good heat resistance, mechanical property excellence.
Technical scheme of the present invention is:
A high thermal conductive silicon rubber composite that contains Graphene, counts by weight, and in this matrix material, matrix is 100 parts, and heat conductive filler is 20~70 parts, and vulcanizing agent is 0.5~5.0 part; Described matrix is raw-silastic continuously, and raw-silastic continuously is that molecular weight is 200000~1000000 the polysiloxane that contains vinyl; Described heat conductive filler is inorganic heat conductive filler, and it is Graphene, or the mixture of Graphene and aluminum oxide.
Described vulcanizing agent is benzoyl peroxide, dicumyl peroxide or 2,5-dimethyl-2,5-di-t-butyl hexane peroxide.
When described inorganic heat conductive filler is the mixture of Graphene and aluminum oxide, the part by weight of Graphene and aluminum oxide is 1:(1~5).
Described Graphene is Graphene prepared by intercalation stripping method, graphite oxidation reduction method or additive method.
The preparation method of the described high thermal conductive silicon rubber composite that contains Graphene, comprises the steps:
(1) matrix, heat conductive filler, vulcanizing agent is mixing under 20 ℃~30 ℃ conditions of room temperature, obtain rubber unvulcanizate;
(2) gained rubber unvulcanizate is placed in to vacuum drying oven, at 40 ℃~80 ℃, adopts the method vacuumizing, remove inner bubble;
(3) step (2) gained rubber unvulcanizate is put into mould, be placed in the hot-forming and one step cure of vulcanizing press, then put into loft drier and carry out post vulcanization, obtain high thermal conductive silicon rubber composite.
Hot-forming and one step cure described in step (3) is: step (2) gained rubber unvulcanizate is placed in to mould, at 130 ℃~185 ℃, under the condition of 10MPa~15MPa, vulcanizes 5~25 minutes.
Post vulcanization described in step (3) is: the rubber unvulcanizate of hot-forming and one step cure, in vacuum drying oven, is kept to 1h~3h at 180 ℃~220 ℃, obtain high thermal conductive silicon rubber composite.
Compared with prior art, tool of the present invention has the following advantages:
(1) heat conductive filler that the present invention uses, there is good heat conductivility, the two-dimentional laminated structure of its uniqueness, high specific surface area, make it be easy in silicon rubber matrix, disperse and form heat conduction network, the in the situation that of low loading level, can reach higher heat conductivility.
(2) with the present invention, prepare the technique of graphene/silicon rubber composite simple, production efficiency is high, is easy to realize commercial scale production, does not use other poisonous and hazardous chemical reagent in preparation process, therefore can be to environment.
In a word, the high thermal conductive silicon rubber composite that the present invention contains Graphene is mixing at ambient temperature by matrix, heat conductive filler and vulcanizing agent, obtains glue stuff compounding.Gained glue stuff compounding is hot-forming and carry out one step cure through vulcanizing press, then puts into loft drier post vulcanization, obtains high thermal conductive silicon rubber composite.Because Graphene has high heat conductance and unique two-dimentional laminated structure, be easy to form the heat conduction network being communicated with in matrix material, significantly improved the thermal conductivity of silicon rubber composite material, the thermal conductivity of silicon rubber graphene composite material of the present invention is 0.3W/mK~1.5W/mK, and can reduce the hardness of silastic material.The preparation technology of high thermal conductive silicon rubber composite of the present invention is simple, and production efficiency is high, is easy to realize commercial scale production.Meanwhile, direction has been pointed out in the batch application that the present invention is Graphene.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the Graphene that uses in the embodiment of the present invention.
Fig. 2 is the electron scanning micrograph of the aluminum oxide that uses in the embodiment of the present invention.
Fig. 3 is for Determination of conductive coefficients sample drawing.
The cross section electron scanning micrograph of prepared heat-conducting silicon rubber 1 in Fig. 4 embodiment of the present invention.
The cross section electron scanning micrograph of prepared heat-conducting silicon rubber 2 in Fig. 5 embodiment of the present invention.
Embodiment
High thermal conductive silicon rubber composite provided by the present invention and preparation method thereof, comprises the steps:
(1) by matrix, heat conductive filler, vulcanizing agent at ambient temperature (20 ℃~30 ℃) mixing, obtain rubber unvulcanizate;
(2) gained rubber unvulcanizate is placed in to vacuum drying oven, at a certain temperature, adopts the method vacuumizing, remove inner bubble.
(3) by step (2) gained rubber unvulcanizate through the moulding of vulcanizing press hot-press vulcanization, then in vacuum drying oven, carry out post vulcanization, obtain high thermal conductive silicon rubber composite.
Wherein, described matrix is raw-silastic continuously, and raw-silastic continuously is that molecular weight is 200000~1000000 the polysiloxane that contains vinyl (as: methyl vinyl silicone rubber, methyl silicone rubber, methyl ethylene phenyl siloxane rubber or trifluoropropyl siloxane etc.).Described heat conductive filler is inorganic heat conductive filler, and it is Graphene, or the mixture of Graphene and aluminum oxide.By adding a certain amount of above heat conductive filler, the thermal conductivity of the high thermal conductive silicon rubber composite obtaining is 0.3W/mK~1.5W/mK.
In order to be illustrated more clearly in technical scheme of the present invention, below in conjunction with embodiment and accompanying drawing, be described in further detail.
Embodiment 1
(1) take the methyl vinyl silicone rubber of 100g, drop in two roller mills, processing temperature is 24 ℃, then adds the Graphene (Fig. 1) of 25g, and the vulcanizing agent of 0.7g (2,5-dimethyl-2,5-di-t-butyl hexane peroxide DHBP), mixing evenly after, thin-pass 5 times, lower.
As shown in Figure 1, pattern feature and the technical parameter of Graphene of the present invention are as follows:
As can be seen from Fig. 1, Graphene has good sheet structure, and because it has very large radius-thickness ratio (being greater than 1000), its diameter 0.5~5 μ m, thickness 1~5nm show as the form of curling as shown in the figure in macroscopic view, are rendered as fluffy cluster-shaped.
(2) rubber unvulcanizate is placed in to vacuum drying oven, temperature is 50 ℃, vacuumizes 5 times and removes air entrapment.
(3) rubber unvulcanizate of removing bubble is placed in to suitable mould, add a cover up and down steel plate, be placed in vulcanizing press and carry out high temperature vulcanized being cross-linked with hot-forming, condition is 170 ℃, 10MPa, curing time is 10 minutes, makes silicon rubber composite material sheet material.Above-mentioned gained silicon rubber composite material sheet material is placed in to vacuum drying oven, processes 2 hours for 200 ℃, obtain thermally conductive silicone rubber composite material 1, see Fig. 4.As can be seen from Figure 4, the Graphene on cross section is high-visible, and Graphene forms packing structure closely in silicon rubber matrix, and the heat conduction network of formation is obviously visible.
Embodiment 2
(1) take the methyl vinyl silicone rubber of 100g, drop in two roller mills, processing temperature is 24 ℃, then add the Graphene (Fig. 1) of 25g and the aluminum oxide (Fig. 2) of 44g, and the vulcanizing agent of 0.7g (2,5-dimethyl-2,5-di-t-butyl hexane peroxide), mixing evenly after, thin-pass 8 times, lower.
As shown in Figure 2, pattern feature and the technical parameter of aluminum oxide of the present invention are as follows: as can be seen from Fig. 2, and Al
2o
3for closely knit spheroidal particle, particle size range is 20~100 μ m.
(2) rubber unvulcanizate is placed in to vacuum drying oven, temperature is 50 ℃, vacuumizes 5 times and removes air entrapment.
(3) rubber unvulcanizate of removing bubble is placed in to suitable mould, add a cover up and down steel plate, be placed in vulcanizing press and carry out high temperature vulcanized being cross-linked with hot-forming, condition is 170 ℃, 10MPa, curing time is 10 minutes, makes the silicon rubber composite material sheet material that heat conductive filler is filled.Above-mentioned gained silicon rubber composite material sheet material is placed in to vacuum drying oven, processes 2 hours for 200 ℃, obtain thermally conductive silicone rubber composite material 2, see Fig. 5.As can be seen from Figure 5, Graphene and Al
2o
3filler is shown in mutual parcel and forms evenly continuous hot transport network architecture in silicon rubber inside.
Embodiment 3
Difference from Example 1 is:
(1) take the methyl silicone rubber of 100g, drop in two roller mills, processing temperature is 25 ℃, then adds the Graphene (Fig. 1) of 35g, and the vulcanizing agent of 4.0g (benzoyl peroxide), mixing evenly after, thin-pass 6 times, lower.
(2) rubber unvulcanizate is placed in to vacuum drying oven, temperature is 40 ℃, vacuumizes 6 times and removes air entrapment.
(3) rubber unvulcanizate of removing bubble is placed in to suitable mould, add a cover up and down steel plate, be placed in vulcanizing press and carry out high temperature vulcanized being cross-linked with hot-forming, condition is 130 ℃, 12MPa, curing time is 15 minutes, makes silicon rubber composite material sheet material.Above-mentioned gained silicon rubber composite material sheet material is placed in to vacuum drying oven, processes 2.5 hours, obtain thermally conductive silicone rubber composite material 3 for 180 ℃.
Embodiment 4
Difference from Example 2 is:
(1) take the methyl ethylene phenyl siloxane rubber of 100g, drop in two roller mills, processing temperature is 28 ℃, then add the Graphene (Fig. 1) of 20g and the aluminum oxide (Fig. 2) of 30g, and the vulcanizing agent of 1.0g (dicumyl peroxide), mixing evenly after, thin-pass 3 times, lower.
(2) rubber unvulcanizate is placed in to vacuum drying oven, temperature is 60 ℃, vacuumizes 4 times and removes air entrapment.
(3) rubber unvulcanizate of removing bubble is placed in to suitable mould, add a cover up and down steel plate, be placed in vulcanizing press and carry out high temperature vulcanized being cross-linked with hot-forming, condition is 160 ℃, 15MPa, curing time is 8 minutes, makes the silicon rubber composite material sheet material that heat conductive filler is filled.Above-mentioned gained silicon rubber composite material sheet material is placed in to vacuum drying oven, processes 1 hour, obtain thermally conductive silicone rubber composite material 4 for 220 ℃.
Comparative example 1
(1) take the methyl vinyl silicone rubber of 100g and the vulcanizing agent of 0.7g (2,5-dimethyl-2,5-di-t-butyl hexane peroxide), drop in two roller mills, processing temperature is 24 ℃, mixing evenly after, thin-pass 5 times, lower.
(2) rubber unvulcanizate is placed in to vacuum drying oven, temperature is 50 ℃, vacuumizes 5 times and removes air entrapment.
(3) rubber unvulcanizate of removing bubble is placed in to suitable mould, add a cover up and down steel plate, be placed in vulcanizing press and carry out high temperature vulcanized being cross-linked with hot-forming, condition is 170 ℃, 10MPa, curing time is 10 minutes, makes the silicon rubber composite material sheet material that heat conductive filler is filled.Above-mentioned gained silicon rubber composite material sheet material is placed in to vacuum drying oven, processes 2 hours, obtain thermally conductive silicone rubber composite material 5 for 200 ℃.
Comparative example 2
(1) take the methyl vinyl silicone rubber of 100g, drop in two roller mills, processing temperature is 24 ℃, then adds the Al of 125g
2o
3, and the vulcanizing agent of 0.7g (2,5-dimethyl-2,5-di-t-butyl hexane peroxide), mixing evenly after, thin-pass 8 times, lower.
(2) rubber unvulcanizate is placed in to vacuum drying oven, temperature is 50 ℃, vacuumizes 5 times and removes air entrapment.
(3) rubber unvulcanizate of removing bubble is placed in to suitable mould, add a cover up and down steel plate, be placed in vulcanizing press and carry out high temperature vulcanized being cross-linked with hot-forming, condition is 170 ℃, 10MPa, curing time is 10 minutes, makes the silicon rubber composite material sheet material that heat conductive filler is filled.Above-mentioned gained silicon rubber composite material sheet material is placed in to vacuum drying oven, processes 2 hours, obtain thermally conductive silicone rubber composite material 6 for 200 ℃.
In above-described embodiment and comparative example, raw-silastic continuously used is the silicon rubber that the trade mark is 110-2, adopts the thermal conductivity of thermal conductivity measuring apparatus (DTC-300) working sample of U.S. TA company, and specimen size is that Ф 50mm * 2mm(is as Fig. 3).According to GB/T531.1-2008 standard, with the shore hardness of Shao Er A type hardness tester instrument (XHS-A type Shao Er sclerometer) test compound material; According to GB/T528-2009 standard, with the micro-processor controlled universal testing machine (WSM-50KG) that Changchun Intelligent Apparatus company limited produces, carry out tensile property test and calculate tensile modulus, according to the method for GB/T2941 regulation, preparing dumbbell shape tension specimen.
Thermal conductivity and the mechanical property of table 1 different components graphene/silicon rubber thermally conductive material
Embodiment and comparative example result show, the present invention is without Graphene is carried out to complicated processing, the preparation technology of matrix material is simple, utilize the singularity in graphene-structured, Graphene is mixed with other heat conductive fillers, heat conductive filler and heat conduction network are mixed to optimization design, can, when improving silicon rubber composite material heat conductivility, make silicon rubber keep excellent elasticity and high-flexibility.When the silicon rubber composite material of this interpolation Graphene is used for heat interfacial material, its easy deformability makes it can fully touch any gap between power component and scatterer, contributes to improve radiating efficiency, extends the work-ing life of power component.
Claims (7)
1. a high thermal conductive silicon rubber composite that contains Graphene, is characterized in that, counts by weight, and in this matrix material, matrix is 100 parts, and heat conductive filler is 20~70 parts, and vulcanizing agent is 0.5~5.0 part; Described matrix is raw-silastic continuously, and raw-silastic continuously is that molecular weight is 200000~1000000 the polysiloxane that contains vinyl; Described heat conductive filler is inorganic heat conductive filler, and it is Graphene, or the mixture of Graphene and aluminum oxide.
2. according to the high thermal conductive silicon rubber composite that contains Graphene claimed in claim 1, it is characterized in that, described vulcanizing agent is benzoyl peroxide, dicumyl peroxide or 2,5-dimethyl-2,5-di-t-butyl hexane peroxide.
3. according to the high thermal conductive silicon rubber composite that contains Graphene claimed in claim 1, it is characterized in that, when described inorganic heat conductive filler is the mixture of Graphene and aluminum oxide, the part by weight of Graphene and aluminum oxide is 1:(1~5).
4. according to the high thermal conductive silicon rubber composite that contains Graphene claimed in claim 1, it is characterized in that, described Graphene is Graphene prepared by intercalation stripping method, graphite oxidation reduction method or additive method.
5. a preparation method for the high thermal conductive silicon rubber composite that contains Graphene claimed in claim 1, is characterized in that, comprises the steps:
(1) matrix, heat conductive filler, vulcanizing agent is mixing under 20 ℃~30 ℃ conditions of room temperature, obtain rubber unvulcanizate;
(2) gained rubber unvulcanizate is placed in to vacuum drying oven, at 40 ℃~80 ℃, adopts the method vacuumizing, remove inner bubble;
(3) step (2) gained rubber unvulcanizate is put into mould, be placed in the hot-forming and one step cure of vulcanizing press, then put into loft drier and carry out post vulcanization, obtain high thermal conductive silicon rubber composite.
6. according to the preparation method of the high thermal conductive silicon rubber composite that contains Graphene claimed in claim 5, it is characterized in that, hot-forming and one step cure described in step (3) is: step (2) gained rubber unvulcanizate is placed in to mould, at 130 ℃~185 ℃, under the condition of 10MPa~15MPa, vulcanize 5~25 minutes.
7. according to the preparation method of the high thermal conductive silicon rubber composite that contains Graphene claimed in claim 5, it is characterized in that, post vulcanization described in step (3) is: by the rubber unvulcanizate of hot-forming and one step cure in vacuum drying oven, at 180 ℃~220 ℃, keep 1h~3h, obtain high thermal conductive silicon rubber composite.
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