CN105778510A - Method for preparing thermally conductive composite material with directivity - Google Patents
Method for preparing thermally conductive composite material with directivity Download PDFInfo
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- CN105778510A CN105778510A CN201610297089.1A CN201610297089A CN105778510A CN 105778510 A CN105778510 A CN 105778510A CN 201610297089 A CN201610297089 A CN 201610297089A CN 105778510 A CN105778510 A CN 105778510A
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- composite material
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- conductive composite
- silicone rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a method for preparing a thermally conductive composite material with directivity in order to solve the heat dissipation problem of conventional materials and traditional technology electronic components. The method comprises the following steps that: a carbon material accounting for 0.1 to 15wt% of a thermally conductive silicone rubber composite material forms an anisotropic thermally conductive path in a polymer matrix under the action of a strong magnetic field, and the thermally conductive composite material mainly comprises a thermally conductive carbon filler of carbon nanotubes or graphenes or a mixture thereof and a silicone rubber matrix; the carbon material is ultrasonically dispersed and poured into a mold to be molded by curing under the action of the strong magnetic field, so that the carbon nanotubes or graphenes form chain structures to be arranged in the matrix, thus generating the thermally conductive composite material with directivity. The method provided by the invention has the advantages of simple and safe operation and short preparation period, the carbon material without a magnetic function is regularly arranged in structure under the action of the strong magnetic field to form an anisotropic composite material, and the thermal conduction has directivity.
Description
Technical field
The present invention relates to thermal conductive polymer field of compound material, specifically a kind of preparation method with directivity heat-conductive composite material.
Background technology
In recent years, along with the development of modern industry, information industry and new and high technology, particular with the degree of integration of microelectronic component and improving constantly of packing density, the heat radiation of heater element has become as an outstanding problem.It is reported, when temperature often raises 2 DEG C, the reliability of electronic devices and components will decline 10%；And during temperature rising 50 DEG C, the life-span of electronic devices and components shortens 5 times when raising 25 DEG C than temperature.In order to ensure electronic devices and components can long-time stable, run reliably, it is necessary to efficiently control operating temperature.At present, conventional material and conventional art have reached bottleneck stage on the heat dissipation problem solving electronic devices and components, it is necessary to obtain the material with good heat conductive performance with the needs of satisfied reality.Along with the appearance of the superpower Heat Conduction Material such as CNT and Graphene, exploitation is added the novel high polymer heat-conductive composite material of material with carbon element and is become new study hotspot.
The macromolecular material of the overwhelming majority has good electrical insulating property, tolerance to cold, highly-breathable, chemical stability, applied range in electronic devices and components and integrated assembling；But heat conductivility is very poor, general heat conductivity is no more than 0.5W/m.K.CNT is the one-dimensional tube of carbonaceous of a kind of nanoscale, heat conductivity is up to 5800W/m.K, by itself and high molecular polymer compound, content that only need to be very low, just can greatly improve the heat conductivity of polymer, mechanical property and heat stability, thus compensate for macromolecular material some shortcomings in mechanics, hot property, thus in heat-transfer device, conductive devices, aerospace field etc., there is huge application potential.
In sum, using the non magnetic CNT heat filling as silicone rubber, under the effect of high-intensity magnetic field, form anisotropic structure, heat conduction is made to have directivity, can being effectively improved composite heat conductivility and have good mechanical property simultaneously, preparation has important practical usage containing CNT thermally conductive silicone rubber composite material.
Summary of the invention
It is an object of the invention to provide a kind of simple to operate, preparation method with directivity heat-conductive composite material that manufacturing cycle is short, with the problem solving to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of preparation method with directivity heat-conductive composite material, specifically comprises the following steps that
(1) material with carbon element carries out surface treatment: mixed by weight=0.1 ~ 3:10 with deionized water by silane coupler, obtain the aqueous solution of silane coupler, uniform stirring, is subsequently adding 1 ~ 10mg material with carbon element, carries out ultrasonic disperse 0.5 ~ 1h under room temperature condition, obtain material with carbon element suspension, 3000 ~ 4000r/min centrifugation 2 ~ 5min, deionized water wash 3 ~ 5 times, then with absolute ethanol washing 2 ~ 4 times, vacuum drying oven dries 10 ~ 24h under 60 ~ 70 DEG C of conditions, obtains the material with carbon element of surface treatment；
(2) the material with carbon element 0.1 ~ 3wt% of surface treatment obtained for step (1) is dissolved in 5 ~ 10 parts of dispersants, ultrasonic disperse 20 ~ 30min, it is subsequently adding 10 parts of silicone rubber matrix, carry out mechanical uniform stirring 10 ~ 30min, ultrasonic again dispersion until dispersant volatilizees completely, evacuation bubble removing, pour in mould, placing curing molding in 10T high-intensity magnetic field, material with carbon element forms chain structure and is arranged in silicone rubber matrix, generates and has directive heat-conductive composite material.
As the further scheme of the present invention: described material with carbon element content in having directive heat-conductive composite material is 0.1 ~ 3wt%.
As the further scheme of the present invention: described material with carbon element is one or more mixing in CNT, Graphene, white carbon black, graphite, carbon fiber, and length dimension ranges for 3 ~ 12um.
As the further scheme of the present invention: the described thickness with directivity heat-conductive composite material is 0.5 ~ 2mm.
As the further scheme of the present invention: described silicone rubber matrix is the one in dimethyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber.
As the further scheme of the present invention: described dispersant is the one in ethanol, methanol, normal hexane.
As the present invention further scheme: described silane coupler is the one in octadecyl trimethoxysilane, gamma-aminopropyl-triethoxy-silane.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention is simple to operate, safety, manufacturing cycle is short, by the effect of high-intensity magnetic field, the material with carbon element not possessing magnetic function structure under high-intensity magnetic field itself is made to have regular arrangement, form anisotropic structure composite, heat conduction is made to have directivity, make full use of the performance that the high heat conductivity of CNT itself and high intensity etc. are excellent, it is doped in polymeric matrix, polymer matrix composite for developing high heat conduction provides new approaches, improve traditional polymer deficiency on heat conductivility, expand the application of composite further.
Accompanying drawing explanation
Fig. 1 is the preparation process flow chart of the present invention；
Fig. 2 is that embodiment 2 is without the electron-microscope scanning figure of CNT silicone rubber heat-conductive composite material under the action of a magnetic field；
Fig. 3 is embodiment 2 electron-microscope scanning figure of CNT silicone rubber heat-conductive composite material under 10T the action of a magnetic field；
Fig. 4 is the heat conduction result of different content CNT and different structure in the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the technical scheme of this patent is described in more detail.
The present invention has directivity heat-conductive composite material, mainly include material with carbon element heat filling and silicone rubber matrix, material with carbon element percentage by weight in heat-conductive composite material is 0.1 ~ 15wt%, (being preferably 0.1 ~ 3wt%), described material aligns in the composite and forms more passage of heat, described material with carbon element is CNT, Graphene, white carbon black, graphite, one or more mixing in carbon fiber, length dimension ranges for 3 ~ 12um, the described thickness with directivity heat-conductive composite material is 0.5 ~ 2mm, described silicone rubber matrix is dimethyl silicone rubber, methyl vinyl silicone rubber, one in methyl phenyl vinyl silicone rubber.
Embodiment 1
Refer to Fig. 1, in the embodiment of the present invention, a kind of preparation method with directivity heat-conductive composite material, specifically comprise the following steps that
(1) CNT carries out surface treatment: by surfactant, by weight=0.1:10 mixes with deionized water, obtain the aqueous solution of surfactant, uniform stirring, is subsequently adding 1mg CNT, carries out ultrasonic disperse 0.5h under room temperature condition, obtain carbon nano tube suspension, 3000r/min centrifugation 2min, deionized water wash 3 times, then with absolute ethanol washing 2 times, vacuum drying oven dries 10h under 60 DEG C of conditions, obtains the CNT of surface treatment；
(2) the CNT 0.1wt% of surface treatment obtained for step (1) is dissolved in 5 parts of dispersants, ultrasonic disperse 20min, it is subsequently adding 10 parts of silicone rubber matrix, carry out mechanical uniform stirring 10min, ultrasonic again dispersion until dispersant volatilizees completely, evacuation bubble removing, pour in mould, placing curing molding in 10T high-intensity magnetic field, CNT forms chain structure and is arranged in silicone rubber matrix, generates and has directive heat-conductive composite material.
Embodiment 2
A kind of preparation method with directivity heat-conductive composite material, specifically comprises the following steps that
(1) CNT carries out surface treatment: by surfactant, by weight=2:10 mixes with deionized water, obtain the aqueous solution of surfactant, uniform stirring, is subsequently adding 6mg CNT, carries out ultrasonic disperse 0.8h under room temperature condition, obtain carbon nano tube suspension, 3500r/min centrifugation 3min, deionized water wash 4 times, then with absolute ethanol washing 3 times, vacuum drying oven dries 17h under 65 DEG C of conditions, obtains the CNT of surface treatment；
(2) the CNT 0.5wt% of surface treatment obtained for step (1) is dissolved in 8 parts of dispersants, ultrasonic disperse 25min, it is subsequently adding 10 parts of silicone rubber matrix, carry out mechanical uniform stirring 20min, ultrasonic again dispersion until dispersant volatilizees completely, evacuation bubble removing, pour in mould, placing curing molding in 10T high-intensity magnetic field, CNT forms chain structure and is arranged in silicone rubber matrix, generates and has directive heat-conductive composite material.
Refer to Fig. 2-3, Fig. 2 is the electromicroscopic photograph of the carbon nanometer tube/silicon rubber heat-conductive composite material without the action of a magnetic field, Fig. 3 is the stereoscan photograph of carbon nanometer tube/silicon rubber heat-conductive composite material under 10T the action of a magnetic field, comparison diagram 2 and Fig. 3 can be seen that, CNT aligns under the effect of high-intensity magnetic field in silicone rubber, form passage of heat so that the heat conduction of composite has directivity.
Embodiment 3
A kind of preparation method with directivity heat-conductive composite material, specifically comprises the following steps that
(1) CNT carries out surface treatment: by surfactant, by weight=3:10 mixes with deionized water, obtain the aqueous solution of surfactant, uniform stirring, is subsequently adding 10mg CNT, carries out ultrasonic disperse 1h under room temperature condition, obtain carbon nano tube suspension, 4000r/min centrifugation 5min, deionized water wash 5 times, then with absolute ethanol washing 4 times, vacuum drying oven dries 24h under 70 DEG C of conditions, obtains the CNT of surface treatment；
(2) the CNT 1wt% of surface treatment obtained for step (1) is dissolved in 10 parts of dispersants, ultrasonic disperse 30min, it is subsequently adding 10 parts of silicone rubber matrix, carry out mechanical uniform stirring 30min, ultrasonic again dispersion until dispersant volatilizees completely, evacuation bubble removing, pour in mould, placing curing molding in 10T high-intensity magnetic field, CNT forms chain structure and is arranged in silicone rubber matrix, generates and has directive heat-conductive composite material.
Refer to the heat conduction result that Fig. 4, Fig. 4 are carbon nanometer tube/silicon rubber heat-conductive composite material different content CNT and different structure；It can be seen that the heat conductivility of the composite of anisotropic structure is substantially better than the composite of isotropic structure；In anisotropic structure, when hot-fluid is parallel to particle chain direction, heat conductivility is better than vertical direction, and the heat conduction being parallel to particle chain direction when content of carbon nanotubes is 0.6wt% adds 36.5% and 50% respectively than isotropism and vertical direction.
Described dispersant is the one in ethanol, methanol, normal hexane, and described silane coupler is the one in octadecyl trimethoxysilane, gamma-aminopropyl-triethoxy-silane.
In the present invention, CNT is non-magnetic tubular material, it is difficult under general magnetic field and polarizes, but under the effect of high-intensity magnetic field, its tubular structure can arrange along field orientation in polymeric matrix, thus forming the polymer composite of orderly heat conduction chain, compared with isotropism heat-conductive composite material, under identical material and filling proportion, the passage of heat aligning easily formation directivity of heat filling, it is possible to be effectively improved the heat conductivility of polymer composites；
The present invention is simple to operate, safety, manufacturing cycle is short, by the effect of high-intensity magnetic field, the material with carbon element not possessing magnetic function structure under high-intensity magnetic field itself is made to have regular arrangement, form anisotropic structure composite, heat conduction is made to have directivity, make full use of the performance that the high heat conductivity of CNT itself and high intensity etc. are excellent, it is doped in polymeric matrix, polymer matrix composite for developing high heat conduction provides new approaches, improve traditional polymer deficiency on heat conductivility, expand the application of composite further.
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, it is also possible under the premise without departing from this patent objective, make various change.
Claims (7)
1. a preparation method with directivity heat-conductive composite material, it is characterised in that specifically comprise the following steps that
(1) material with carbon element carries out surface treatment: mixed by weight=0.1 ~ 3:10 with deionized water by silane coupler, obtain the aqueous solution of silane coupler, uniform stirring, is subsequently adding 1 ~ 10mg material with carbon element, carries out ultrasonic disperse 0.5 ~ 1h under room temperature condition, obtain material with carbon element suspension, 3000 ~ 4000r/min centrifugation 2 ~ 5min, deionized water wash 3 ~ 5 times, then with absolute ethanol washing 2 ~ 4 times, vacuum drying oven dries 10 ~ 24h under 60 ~ 70 DEG C of conditions, obtains the material with carbon element of surface treatment；
(2) the material with carbon element 0.1 ~ 3wt% of surface treatment obtained for step (1) is dissolved in 5 ~ 10 parts of dispersants, ultrasonic disperse 20 ~ 30min, it is subsequently adding 10 parts of silicone rubber matrix, carry out mechanical uniform stirring 10 ~ 30min, ultrasonic again dispersion until dispersant volatilizees completely, evacuation bubble removing, pour in mould, placing curing molding in 10T high-intensity magnetic field, material with carbon element forms chain structure and is arranged in silicone rubber matrix, generates and has directive heat-conductive composite material.
2. the preparation method with directivity heat-conductive composite material according to claim 1, it is characterised in that described material with carbon element content in having directive heat-conductive composite material is 0.1 ~ 3wt%.
3. the preparation method with directivity heat-conductive composite material according to claim 1, it is characterised in that described material with carbon element is one or more mixing in CNT, Graphene, white carbon black, graphite, carbon fiber, and length dimension ranges for 3 ~ 12um.
4. the preparation method with directivity heat-conductive composite material according to claim 1, it is characterised in that the described thickness with directivity heat-conductive composite material is 0.5 ~ 2mm.
5. the preparation method with directivity heat-conductive composite material according to claim 1, it is characterised in that described silicone rubber matrix is the one in dimethyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber.
6. the preparation method with directivity heat-conductive composite material according to claim 1, it is characterised in that described dispersant is the one in ethanol, methanol, normal hexane.
7. the preparation method with directivity heat-conductive composite material according to claim 1, it is characterised in that described silane coupler is the one in octadecyl trimethoxysilane, gamma-aminopropyl-triethoxy-silane.
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Cited By (16)
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|---|---|---|---|---|
| CN106433133A (en) * | 2016-08-23 | 2017-02-22 | 广东工业大学 | Polymer matrix/three-dimensional graphene thermal interface composite material, and preparation method and application thereof |
| CN106752119A (en) * | 2016-12-23 | 2017-05-31 | 青岛黑猫炭黑科技有限责任公司 | A kind of preparation method of carbon black nano material |
| CN106810719A (en) * | 2017-02-24 | 2017-06-09 | 中国科学院化学研究所 | A kind of hot functional composite material and its preparation method and application |
| CN107868465A (en) * | 2017-11-30 | 2018-04-03 | 中国科学院合肥物质科学研究院 | A kind of heat conductive insulating composite with anisotropic structure and preparation method thereof |
| CN108752713A (en) * | 2018-06-25 | 2018-11-06 | 厦门十维科技有限公司 | One kind aligning graphene superelevation thermal conductivity composite material and preparation method |
| CN109694580A (en) * | 2018-12-28 | 2019-04-30 | 重庆邮电大学 | A kind of magnetic-sensitive material and its preparation method and application that surface roughness is controllable |
| CN109943075A (en) * | 2019-03-27 | 2019-06-28 | 华南理工大学 | A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning |
| CN110117484A (en) * | 2019-06-11 | 2019-08-13 | 哈尔滨工业大学 | A kind of preparation method having directive thermal conductive silicon Gel composite sheets material |
| CN110740629A (en) * | 2019-10-16 | 2020-01-31 | 深圳市飞鸿达科技有限公司 | oriented heat conduction wave absorption plate and preparation method thereof |
| CN111640851A (en) * | 2020-05-29 | 2020-09-08 | 旭宇光电（深圳）股份有限公司 | Deep ultraviolet LED light source and packaging method thereof |
| CN112867361A (en) * | 2021-01-22 | 2021-05-28 | Oppo广东移动通信有限公司 | Display screen assembly and electronic device |
| CN113461989A (en) * | 2021-08-06 | 2021-10-01 | 扬中市华龙橡塑电器有限公司 | Anisotropic heat conduction composite material and preparation method thereof |
| CN113897060A (en) * | 2021-10-21 | 2022-01-07 | 北京旭碳新材料科技有限公司 | Grafted graphene heat dissipation silica gel composition, grafted graphene heat dissipation silica gel, and preparation method and application thereof |
| CN114214023A (en) * | 2021-12-01 | 2022-03-22 | 北京旭碳新材料科技有限公司 | Modified graphene heat dissipation silica gel and preparation method thereof |
| CN114539860A (en) * | 2021-12-31 | 2022-05-27 | 苏州卓纳纳米技术有限公司 | Preparation method of ultrahigh-heat-conductivity graphene carbon nanotube composite material |
| CN114854202A (en) * | 2022-06-07 | 2022-08-05 | 浙江柔灵科技有限公司 | Electrode material of silica gel filled with carbon black-carbon nanotube mixture and process thereof |
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| CN106433133B (en) * | 2016-08-23 | 2021-08-24 | 广东工业大学 | Polymer matrix/three-dimensional graphene thermal interface composite material and preparation method and application thereof |
| CN106433133A (en) * | 2016-08-23 | 2017-02-22 | 广东工业大学 | Polymer matrix/three-dimensional graphene thermal interface composite material, and preparation method and application thereof |
| CN106752119A (en) * | 2016-12-23 | 2017-05-31 | 青岛黑猫炭黑科技有限责任公司 | A kind of preparation method of carbon black nano material |
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| CN109943075A (en) * | 2019-03-27 | 2019-06-28 | 华南理工大学 | A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning |
| CN110117484A (en) * | 2019-06-11 | 2019-08-13 | 哈尔滨工业大学 | A kind of preparation method having directive thermal conductive silicon Gel composite sheets material |
| CN110740629A (en) * | 2019-10-16 | 2020-01-31 | 深圳市飞鸿达科技有限公司 | oriented heat conduction wave absorption plate and preparation method thereof |
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| CN113461989A (en) * | 2021-08-06 | 2021-10-01 | 扬中市华龙橡塑电器有限公司 | Anisotropic heat conduction composite material and preparation method thereof |
| CN113897060A (en) * | 2021-10-21 | 2022-01-07 | 北京旭碳新材料科技有限公司 | Grafted graphene heat dissipation silica gel composition, grafted graphene heat dissipation silica gel, and preparation method and application thereof |
| CN114214023A (en) * | 2021-12-01 | 2022-03-22 | 北京旭碳新材料科技有限公司 | Modified graphene heat dissipation silica gel and preparation method thereof |
| CN114539860A (en) * | 2021-12-31 | 2022-05-27 | 苏州卓纳纳米技术有限公司 | Preparation method of ultrahigh-heat-conductivity graphene carbon nanotube composite material |
| CN114854202A (en) * | 2022-06-07 | 2022-08-05 | 浙江柔灵科技有限公司 | Electrode material of silica gel filled with carbon black-carbon nanotube mixture and process thereof |
| CN114854202B (en) * | 2022-06-07 | 2024-01-26 | 浙江柔灵科技有限公司 | Carbon black-carbon nano tube mixed silica gel filled electrode material and process thereof |
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