CN110041571B - Preparation method of high-thermal-conductivity graphene composite material - Google Patents
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- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention relates to a preparation method of a high-thermal-conductivity graphene composite material, in particular to a method for embedding a graphene nanosheet/natural rubber dispersion liquid into three-dimensional graphene foam prepared by a chemical vapor deposition method, and the graphene composite material obtained by the method can be used as a transverse thermal-conductivity radiating fin and a thermal-interface radiating fin. The preparation method mainly comprises the following steps: dispersing graphene nanosheets in a natural rubber solution to prepare a graphene nanosheet/natural rubber dispersion solution; pouring the dispersion liquid into a mold filled with three-dimensional graphene foam, and naturally drying or heating and drying to prepare a graphene nanosheet/three-dimensional graphene foam/natural rubber composite material; and obtaining the high-thermal-conductivity graphene composite material through hot-pressing vulcanization. The invention has simple process, solves the problem that the prior heat conduction material excessively uses heat conduction fillers, such as: aluminum oxide, aluminum nitride, silicon carbide, copper, silver and the like, which cause the problems of reduced mechanical properties, resource shortage, high price, complex equipment and the like.
Description
Technical Field
The invention relates to the field of manufacturing processes of graphene nanosheets, three-dimensional graphene foam, natural rubber, a graphene nanosheet/natural rubber embedded three-dimensional graphene foam pore structure and rubber vulcanization, in particular to a preparation method of a high-thermal-conductivity graphene composite material.
Background
The heat-conducting composite material is an indispensable important component in high-power-consumption electronic devices and is the key for ensuring the long-time normal operation or the operation of the electronic devices under high power consumption. The heat-conducting composite material is prepared by uniformly mixing heat-conducting fillersUniformly dispersed in a polymer matrix to form a composite material. The heat-conducting composite material mainly comprises two contents of a heat-conducting filler and a polymer matrix, wherein the heat-conducting filler is usually Al2O3AlN, SiC, MgO and ZnO, and the alumina with the highest use frequency has the thermal conductivity coefficient of 30W/mK, namely the commonly used thermal conductive filler generally has low thermal conductivity and large filling amount (50 to 70 weight percent).
Thermally conductive composites have been widely used as a medium between an electronic device and a heat sink, such as: semiconductor power devices, integrated circuits, LED packages, high power supply modules, high speed memory chips, and communication devices. Various techniques for connecting high power electronic devices or devices that are prone to heat generation to heat sinks are used with thermally conductive composites to meet the heat dissipation requirements of such materials. Graphene thermal conductive materials have many advantages over traditional thermal conductive materials, such as: the intrinsic thermal conductivity of the graphene exceeds 5000W/mK, the flexibility is good, the weight is light, the addition amount of the filler is small, the graphene is corrosion-resistant, and the graphene is easy to machine and form with a base material.
While using conventional thermally conductive fillers (e.g., Al)2O3AlN, SiC, etc.), which results in large filler addition, large processing difficulty, reduced mechanical properties and limited application fields. The graphene is used as the heat-conducting filler, so that the heat-conducting property is improved, the process is simplified, the equipment cost is reduced, and the like. With the continuous and deep research, the graphene heat conduction material is gradually replacing the traditional heat conduction material, and the application field is continuously expanded, so that the graphene heat conduction material becomes a new generation of mainstream heat conduction material.
Disclosure of Invention
The invention aims to provide a preparation method of a high-thermal-conductivity graphene composite material, which is simple in preparation process, high in efficiency, free of vacuum and easy to operate, and solves the problems that a heat-conducting filler is large in addition amount in a high-molecular matrix and a complete heat-conducting passage is difficult to form.
The technical scheme of the invention is as follows:
a preparation method of a high-thermal-conductivity graphene composite material is characterized in that a graphene nanosheet/natural rubber dispersion liquid is embedded into three-dimensional graphene foam, and the preparation method mainly comprises the following steps:
(1) dissolving natural rubber by using a toluene solvent under the condition of heating and stirring to form a natural rubber solution;
(2) dispersing graphene nanosheets in toluene by using ultrasonic waves to form graphene nanosheet dispersion liquid; adding the graphene nanosheet dispersion liquid into a natural rubber solution to form a graphene nanosheet/natural rubber dispersion liquid;
(3) adding stearic acid, sulfur, dibenzothiazyl disulfide and zinc oxide into the graphene nanosheet/natural rubber dispersion liquid;
(4) pouring the solution obtained in the step (3) into a polytetrafluoroethylene mold filled with three-dimensional graphene foam, and removing a toluene solvent by utilizing natural drying or heating and drying to obtain a graphene nanosheet/three-dimensional graphene foam/natural rubber composite material;
(5) and obtaining the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material through hot-pressing vulcanization.
According to the preparation method of the high-thermal-conductivity graphene composite material, in the step (1), the technological parameters for dissolving the natural rubber are as follows: the temperature is 40-70 ℃, the magnetic stirring speed is 200-1000 r/min, and the stirring time is 3-8 h.
According to the preparation method of the high-thermal-conductivity graphene composite material, the size of the graphene nanosheet is 3-5 microns, the number of layers is less than or equal to 10, the three-dimensional graphene foam is prepared by a chemical vapor deposition method, the porosity is greater than or equal to 99.58%, and the pore size is 400-600 microns.
According to the preparation method of the high-thermal-conductivity graphene composite material, the natural rubber is a first-grade natural rubber smoked sheet.
According to the preparation method of the high-thermal-conductivity graphene composite material, when the graphene nanosheet/natural rubber dispersion liquid is prepared, the concentration of the natural rubber solution is 12-40 mg/ml, the concentration of the graphene nanosheet dispersion liquid is 6-12 mg/ml, and the graphene nanosheet dispersion liquid is prepared by mixing the following components in a weight ratio of 1: 10-1: 2, adding the graphene nanosheet dispersion liquid into a natural rubber solution, and heating and stirring for 2-24 hours at the temperature of 60-90 ℃ and the rotating speed of 600-1500 r/min to obtain the graphene nanosheet/natural rubber dispersion liquid.
According to the preparation method of the high-thermal-conductivity graphene composite material, in the solution obtained in the step (3), the stearic acid, the sulfur, the dibenzothiazyl disulfide and the zinc oxide respectively account for the following components in percentage by weight: 1-5%, 2-8%, 0.2-0.7%, 3-10%.
In the preparation method of the high-thermal-conductivity graphene composite material, in the step (4), the natural drying time is 12-72 hours, and the heating and drying are as follows: and drying for 6-12 h at 30-90 ℃ to enable the graphene nanosheets/natural rubber to be embedded into the three-dimensional graphene foam.
In the preparation method of the high-thermal-conductivity graphene composite material, in the step (5), the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material is placed in a cast iron mold for hot-pressing vulcanization: the temperature is 140-170 ℃, the pressure is 5-15 MPa, and the time is 1-5 h, so that the graphene nanosheets are directionally arranged, the composite material is densified, and the thermal conductivity is improved.
According to the preparation method of the high-thermal-conductivity graphene composite material, in the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material, the graphene content is 8-25 wt%, the in-plane thermal conductivity is 8-12W/mK, and the vertical thermal conductivity is 2-4W/mK.
The design idea of the invention is as follows:
the method mainly comprises the following steps: dispersing graphene nanosheets in a natural rubber solution to prepare a graphene nanosheet/natural rubber dispersion solution; pouring the dispersion liquid into a mold filled with three-dimensional graphene foam, and naturally drying or heating and drying to prepare a graphene nanosheet/three-dimensional graphene foam/natural rubber composite material; and obtaining the high-thermal-conductivity graphene composite material through hot-pressing vulcanization. The graphene nanosheet/natural rubber dispersion liquid is embedded into the three-dimensional graphene foam prepared by a Chemical Vapor Deposition (CVD) method, and the hot-pressing vulcanization method is suitable for preparing transverse quick heat-conducting radiating fins and thermal interface radiating fins and assembling processes of high-power-consumption electronic product quick radiating parts related to the transverse quick heat-conducting radiating fins and the thermal interface radiating fins.
The invention has the advantages and beneficial effects that:
1. the invention provides a method for directly constructing a three-dimensional network heat conduction path in a polymer matrix by graphene, which is compared with the traditional filler (Al)2O3AlN and SiC), the addition amount of the filler is reduced, the thermal conductivity is obviously increased, and a new idea about applying the graphene to the heat-conducting composite material is provided. The heat conduction path is the key for preparing the heat conduction composite material, the completeness of the three-dimensional graphene heat conduction path in a polymer matrix is realized, the graphene nanosheets form the heat conduction path along the three-dimensional graphene foam holes and are arranged in a directional mode, and the heat conduction path is increased.
2. The invention has simple preparation process, low requirement on required equipment and easy large-scale production, and solves the problems that the prior heat conduction material excessively uses heat conduction fillers, such as: aluminum oxide (Al)2O3) Aluminum nitride (AlN), silicon carbide (SiC), copper (Cu), silver (Ag), and the like, and cause problems of reduced mechanical properties, resource shortage, high price, complicated equipment, and the like.
Drawings
Fig. 1 is a schematic flow chart of a method for constructing and preparing a high thermal conductivity graphene composite material by using a three-dimensional network according to the present invention.
Fig. 2(a) is a topography of a high thermal conductivity graphene composite material, fig. 2(b) is a topography of a graphene nanosheet/natural rubber and three-dimensional graphene foam skeleton, and fig. 2(c) is a topography of a directionally arranged graphene nanosheet.
Detailed Description
As shown in fig. 1, in a specific embodiment, the preparation method of the high thermal conductivity graphene composite material of the present invention specifically includes the following steps:
(1) the preparation method comprises the steps of completely dissolving natural rubber by utilizing a toluene solvent under the condition of heating and stirring (the temperature is 40-70 ℃, the magnetic stirring speed is 200-1000 r/min, and the stirring time is 6-8 h), dispersing graphene nanosheets in toluene through ultrasonic waves, adding a graphene nanosheet dispersion liquid into a natural rubber solution, obtaining the graphene nanosheet/natural rubber dispersion liquid under the condition of heating and stirring (the temperature is 60-90 ℃, the stirring speed is 600-1500 r/min, and the stirring time is 2-24 h), then sequentially adding stearic acid, sulfur, dibenzothiazyl Disulfide (DM), zinc oxide, stearic acid and zinc oxide which have the functions of an active agent, and sulfur and dibenzothiazyl Disulfide (DM) which have the functions of a vulcanizing agent and an accelerating agent respectively.
(2) And pouring the graphene nanosheet/natural rubber dispersion liquid into a Polytetrafluoroethylene (PTFE) mold filled with three-dimensional graphene foam to obtain a graphene nanosheet/three-dimensional graphene foam/natural rubber composite material, and removing the toluene solvent by utilizing natural drying for 12-72 h or drying for 6-12 h at 30-90 ℃.
(3) And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization, wherein the hot-pressing vulcanization condition is 140-170 ℃, the pressure is 5-15 MPa, and the time is 1-5 h. Thereby obtaining the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
The preparation method of the three-dimensional graphene foam comprises the following steps: according to Chinese patent application (publication number: CN 102674321A; invention name: graphene foam with a three-dimensional fully-connected network and a macro preparation method thereof; application date: 2011, 3, month and 10 days), graphene grows on the surface of a nickel foam porous metal, and after nickel foam is etched, the three-dimensional graphene foam is obtained.
The present invention will be described in further detail below by way of examples and figures.
Example 1
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
and (3) dissolving 3g of natural rubber in 80-150 ml of toluene solvent under the condition of heating and stirring, wherein the temperature is 40 ℃, the magnetic stirring speed is 300r/min, and the stirring time is 6 hours, so as to form a natural rubber solution. Taking 300-600 mg of graphene nanosheets, and dispersing the graphene nanosheets in 60ml of toluene through ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.03g of stearic acid, 0.15g of sulfur, 0.006g of DM and 0.09g of zinc oxide. The temperature is 60 ℃, the stirring speed is 800r/min, and the time is 12 h.
And (3) pouring 30ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and removing the toluene solvent by utilizing natural drying to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 140 ℃, 10MPa of pressure and 1h of time, so as to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 8-15 wt%, the in-plane thermal conductivity is 10.0W/mK, and the vertical thermal conductivity is 3.0W/mK.
As shown in fig. 2(a), it can be seen from the morphology of the high thermal conductivity graphene composite material that the sample surface is smooth and compact and has no pores.
As shown in fig. 2(b), it can be seen from the morphologies of the graphene nanoplatelets/natural rubber and the three-dimensional graphene foam skeleton that the graphene foam skeleton is tightly combined with the graphene nanoplatelets/natural rubber.
As shown in fig. 2(c), it can be seen from the morphology of the directionally aligned graphene nanosheets that the graphene nanosheets are aligned along the same direction, which is helpful for improving the thermal conductivity in this direction.
Example 2
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
taking 90ml of toluene solvent, dissolving 3g of natural rubber under the condition of heating and stirring, wherein the temperature is 40 ℃, the magnetic stirring speed is 200r/min, and the stirring time is 8 hours, so as to form the natural rubber solution. Taking 400mg of graphene nanosheets, and dispersing the graphene nanosheets in 80ml of toluene by ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.12g of stearic acid, 0.15g of sulfur, 0.021g of DM and 0.09g of zinc oxide. The temperature is 60 ℃, the stirring speed is 800r/min, and the time is 12 h.
And (3) pouring 25ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and removing a toluene solvent by utilizing natural drying to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 150 ℃, 15MPa and 3h, so as to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 10 wt%, the in-plane thermal conductivity is 8.0W/mK, and the vertical thermal conductivity is 2.0W/mK.
Example 3
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
taking 120ml of toluene solvent, and dissolving 3g of natural rubber under the condition of heating and stirring, wherein the temperature is 40 ℃, the magnetic stirring speed is 300-600 r/min, and the stirring time is 6-8 h, so as to form a natural rubber solution. Taking 500mg of graphene nanosheets, and dispersing the graphene nanosheets in 100ml of toluene by ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.03g of stearic acid, 0.12g of sulfur, 0.021g of DM and 0.24g of zinc oxide. The temperature is 60 ℃, the stirring speed is 1000r/min, and the time is 12 h.
And adding 30ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and removing a toluene solvent by utilizing natural drying to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 150 ℃, 15MPa of pressure and 3h of time to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 12 wt%, the in-plane thermal conductivity is 10.5W/mK, and the vertical thermal conductivity is 3.0W/mK.
Example 4
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
and (3) dissolving 2g of natural rubber in 100ml of toluene solvent under the condition of heating and stirring, wherein the temperature is 50 ℃, the magnetic stirring speed is 500r/min, and the stirring time is 6-8 h to form a natural rubber solution. Taking 400-500 mg of graphene nanosheets, and dispersing the graphene nanosheets in 70ml of toluene through ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.03g of stearic acid, 0.03g of sulfur, 0.009g of DM and 0.05g of zinc oxide. The temperature is 80 ℃, the stirring speed is 800r/min, and the time is 8-12 h.
Adding 35-40 ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and removing a toluene solvent by utilizing natural drying to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 160 ℃, 9-10 MPa and 5h to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 18-25 wt%, the in-plane thermal conductivity is 9.0W/mK, and the vertical thermal conductivity is 2.2W/mK.
Example 5
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
taking 80 toluene solvent, dissolving 2g of natural rubber under the condition of heating and stirring, wherein the temperature is 70 ℃, the magnetic stirring speed is 600r/min, and the stirring time is 8h, so as to form the natural rubber solution. Taking 350-400 mg of graphene nanosheets, and dispersing the graphene nanosheets in 60ml of toluene through ultrasonic waves to form graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.03g of stearic acid, 0.02g of sulfur, 0.005g of DM and 0.06g of zinc oxide. The temperature is 70 ℃, the stirring speed is 900r/min, and the time is 8-12 h.
Adding 35-40 ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and heating and drying at 90 ℃ to remove a toluene solvent to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 170 ℃, 15MPa of pressure and 1h of time to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 15-19 wt%, the in-plane thermal conductivity is 8.5W/mK, and the vertical thermal conductivity is 2.8W/mK.
Example 6
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
taking 120-150 ml of toluene solvent, and dissolving 4g of natural rubber under the condition of heating and stirring, wherein the temperature is 50 ℃, the magnetic stirring speed is 1000r/min, and the stirring time is 6-8 h, so as to form a natural rubber solution. Taking 500-700 mg of graphene nanosheets, and dispersing the graphene nanosheets in 120ml of toluene through ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.09g of stearic acid, 0.08g of sulfur, 0.018g of DM and 0.15g of zinc oxide. The temperature is 70 ℃, the stirring speed is 1000r/min, and the time is 8-12 h.
And adding 40ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and removing a toluene solvent by utilizing natural drying to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 150 ℃, 8-10 MPa and 1.5h to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 10-17 wt%, the in-plane thermal conductivity is 10.5W/mK, and the vertical thermal conductivity is 3.5W/mK.
Example 7
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
taking 120-150 ml of toluene solvent, dissolving 4g of natural rubber under the condition of heating and stirring, wherein the temperature is 40 ℃, the magnetic stirring speed is 300r/min, and the stirring time is 8 hours, so as to form a natural rubber solution. Taking 700mg of graphene nanosheets, and dispersing the graphene nanosheets in 100ml of toluene by ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.15g of stearic acid, 0.09g of sulfur, 0.028g of DM and 0.2g of zinc oxide. The temperature is 60 ℃, the stirring speed is 1500r/min, and the time is 8-12 h.
And adding 25ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and removing a toluene solvent by utilizing natural drying to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 140 ℃, 12MPa of pressure and 1h of time to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 16 wt%, the in-plane thermal conductivity is 11.0W/mK, and the vertical thermal conductivity is 4.0W/mK.
Example 8
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
taking 180ml of toluene solvent, and dissolving 5g of natural rubber under the condition of heating and stirring, wherein the temperature is 70 ℃, the magnetic stirring speed is 800r/min, and the stirring time is 6-8 h, so as to form a natural rubber solution. Taking 800mg of graphene nanosheets, and dispersing the graphene nanosheets in 100ml of toluene by ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.2g of stearic acid, 0.2g of sulfur, 0.025g of DM and 0.2g of zinc oxide. The temperature is 70 ℃, the stirring speed is 1000r/min, and the time is 8-12 h.
Adding 30ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and heating and drying at 50 ℃ to remove a toluene solvent, thereby obtaining the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 160 ℃, 15MPa of pressure and 5 hours of time to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 14 wt%, the in-plane thermal conductivity is 11.2W/mK, and the vertical thermal conductivity is 4.0W/mK.
Example 9
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
taking 200ml of toluene solvent, dissolving 5g of natural rubber under the condition of heating and stirring, wherein the temperature is 50 ℃, the magnetic stirring speed is 400r/min, and the stirring time is 8 hours, so as to form a natural rubber solution. Taking 800mg of graphene nanosheets, and dispersing the graphene nanosheets in 120ml of toluene by ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.15g of stearic acid, 0.15g of sulfur, 0.021g of DM and 0.15g of zinc oxide. The temperature is 50 ℃, the stirring speed is 1000r/min, and the time is 8-12 h.
Adding 35-45 ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and heating and drying at 50 ℃ to remove a toluene solvent to obtain the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 150 ℃, 10MPa of pressure and 2h of time to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 12 wt%, the in-plane thermal conductivity is 11.0W/mK, and the vertical thermal conductivity is 3.5W/mK.
Example 10
In this embodiment, the preparation method of the high thermal conductivity graphene composite material is as follows:
and (3) taking 260-300 ml of toluene solvent, and dissolving 5g of natural rubber under the condition of heating and stirring, wherein the temperature is 60 ℃, the magnetic stirring speed is 400r/min, and the stirring time is 6 hours, so as to form a natural rubber solution. Taking 1500mg of graphene nanosheets, and dispersing the graphene nanosheets in 90ml of toluene by ultrasonic waves to form a graphene nanosheet dispersion liquid. Adding the graphene nanosheet dispersion liquid into a natural rubber solution, heating and stirring to obtain the graphene nanosheet/natural rubber dispersion liquid, and sequentially adding 0.20g of stearic acid, 0.15g of sulfur, 0.012g of DM and 0.20g of zinc oxide. The temperature is 60 ℃, the stirring speed is 1000r/min, and the time is 8-12 h.
Adding 30ml of graphene nanosheet/natural rubber dispersion liquid into a PTFE (polytetrafluoroethylene) mold filled with three-dimensional graphene foam, and heating and drying at 80 ℃ to remove a toluene solvent, thereby obtaining the graphene nanosheet/three-dimensional graphene foam/natural rubber composite material.
And (3) compacting the composite material and orienting the graphene nanosheets by utilizing hot-pressing vulcanization under the conditions of 140 ℃, 10MPa of pressure and 5h of time to obtain the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material. The graphene content is 25 wt%, the in-plane thermal conductivity is 11.6W/mK, and the vertical thermal conductivity is 3.8W/mK.
The embodiment result shows that the three-dimensional heat conduction path is directly constructed by the low-content heat conduction filler in the high polymer matrix, and the obtained graphene nanosheet/three-dimensional graphene foam/natural rubber composite material has high heat conductivity.
Claims (9)
1. A preparation method of a high-thermal-conductivity graphene composite material is characterized in that a graphene nanosheet/natural rubber dispersion liquid is embedded into a three-dimensional graphene foam, and mainly comprises the following steps:
(1) dissolving natural rubber by using a toluene solvent under the condition of heating and stirring to form a natural rubber solution;
(2) dispersing graphene nanosheets in toluene by using ultrasonic waves to form graphene nanosheet dispersion liquid; adding the graphene nanosheet dispersion liquid into a natural rubber solution to form a graphene nanosheet/natural rubber dispersion liquid;
(3) adding stearic acid, sulfur, dibenzothiazyl disulfide and zinc oxide into the graphene nanosheet/natural rubber dispersion liquid;
(4) pouring the solution obtained in the step (3) into a polytetrafluoroethylene mold filled with three-dimensional graphene foam, and removing a toluene solvent by utilizing natural drying or heating and drying to obtain a graphene nanosheet/three-dimensional graphene foam/natural rubber composite material;
(5) obtaining a high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material through hot-pressing vulcanization;
in the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material, the graphene content is 8-25 wt%.
2. The preparation method of the high thermal conductivity graphene composite material according to claim 1, wherein in the step (1), the process parameters for dissolving the natural rubber are as follows: the temperature is 40-70 ℃, the magnetic stirring speed is 200-1000 r/min, and the stirring time is 3-8 h.
3. The preparation method of the high-thermal-conductivity graphene composite material as claimed in claim 1, wherein the size of the graphene nanoplatelets is 3-5 μm, the number of layers is less than or equal to 10, the three-dimensional graphene foam is prepared by a chemical vapor deposition method, the porosity is greater than or equal to 99.58%, and the pore size is 400-600 μm.
4. The method for preparing a graphene composite material with high thermal conductivity according to claim 1, wherein the natural rubber is a first-grade natural rubber smoked sheet.
5. The preparation method of the high-thermal-conductivity graphene composite material as claimed in claim 1, wherein when preparing the graphene nanosheet/natural rubber dispersion, the concentration of the natural rubber solution is 12-40 mg/ml, the concentration of the graphene nanosheet dispersion is 6-12 mg/ml, and the weight ratio is 1: 10-1: 2, adding the graphene nanosheet dispersion liquid into a natural rubber solution, and heating and stirring for 2-24 hours at the temperature of 60-90 ℃ and the rotating speed of 600-1500 r/min to obtain the graphene nanosheet/natural rubber dispersion liquid.
6. The preparation method of the high thermal conductivity graphene composite material according to claim 1, wherein in the solution obtained in the step (3), the stearic acid, the sulfur, the dibenzothiazyl disulfide and the zinc oxide respectively account for the following components in percentage by weight: 1-5%, 2-8%, 0.2-0.7%, 3-10%.
7. The preparation method of the high-thermal-conductivity graphene composite material according to claim 1, wherein in the step (4), the natural drying time is 12-72 hours, and the heating and drying are as follows: and drying for 6-12 h at 30-90 ℃ to enable the graphene nanosheets/natural rubber to be embedded into the three-dimensional graphene foam.
8. The preparation method of the high thermal conductivity graphene composite material according to claim 1, wherein in the step (5), the graphene nanoplatelets/three-dimensional graphene foam/natural rubber composite material is placed in a cast iron mold for hot-press vulcanization: the temperature is 140-170 ℃, the pressure is 5-15 MPa, and the time is 1-5 h, so that the graphene nanosheets are directionally arranged, the composite material is densified, and the thermal conductivity is improved.
9. The preparation method of the high-thermal-conductivity graphene composite material according to claim 1 or 8, wherein in the high-thermal-conductivity graphene nanosheet/three-dimensional graphene foam/natural rubber composite material, the in-plane thermal conductivity is 8-12W/mK, and the vertical thermal conductivity is 2-4W/mK.
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