CN113184836A - High-thermal-conductivity graphene film and preparation method thereof - Google Patents
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Abstract
The invention discloses a graphene film with high thermal conductivity and a preparation method thereof, and belongs to the technical field of thermal conductive materials. The graphene oxide adopted by the invention can be uniformly dispersed in water. According to the invention, graphene oxide and fiber are mixed and ground into slurry, the graphene oxide permeates into the fiber and is firmly combined with the fiber, a certain amount of binder is added into the mixed slurry of the graphene oxide and the fiber, a graphene oxide film is obtained through vacuum filtration, and a graphene heat-conducting film with high heat conductivity and high flexibility is obtained through high-temperature carbonization and graphitization in the later stage. The graphene heat-conducting film can be prepared by a simple preparation process, is low in cost, controllable in thickness, simple to operate and high in production efficiency, and is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, and particularly relates to a preparation method of a graphene film with high heat conduction.
Background
In recent years, along with the continuous miniaturization and integration of electronic systems, the performance and reliability of electronic systems are increasingly limited by the problem of heat conduction, and the requirements of the field of consumer electronics (smart phones, ultrathin notebook computers and tablet computers) on heat conduction are becoming more and more strict. The service life and stability of electronic components can be greatly influenced by too high heat productivity and dissipation power density, and the traditional heat conduction materials mainly comprise metal thin films, graphite rolled films, graphitized polyimide films and the like. The metal film has the defects of heavy mass, easy corrosion, low heat conductivity and the like, and the graphite calendered film and the graphitized polyimide film are brittle and easy to fall off powder in the use process, so that the metal film is not suitable for the field of precise instrument management with complex structure and high cleanliness requirement. On the other hand, the traditional graphitized polyimide film is usually produced by batch operation, and a large amount of time (at least 6-10 h of heating time and at least 10h of cooling time) and energy (at least 50-70 KW/h of energy consumption of an experimental furnace) are consumed in the graphitizing process.
Graphene as a newly developed two-dimensional material has a plurality of excellent performances, the thermal conductivity of single-layer defect-free graphene can reach 5300W/(m.k), which is much higher than that of metal thermal conductivity materials such as copper (398W/(m.k)), the in-plane thermal conductivity of a single layer of a graphene thermal conductive film can reach 4800W/(m.k) -5300W/(m.k), and the graphene thermal conductive film has excellent characteristics such as low density, low thermal expansion coefficient and good mechanical performance, and is a novel thermal conductive and heat dissipation material. Therefore, a preparation method of the graphene heat conduction film is provided.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity graphene film and a preparation method thereof, and the graphene film has the advantages of low cost, excellent film-forming performance, high thermal conductivity, simple preparation process, large-scale production and the like.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a graphene heat conduction film comprises the following steps:
mixing graphene oxide and fiber raw materials, and putting the mixture into a PFI disc mill for grinding to obtain mixed slurry of graphene oxide and fiber, wherein the concentration of the mixed slurry is 10%.
And secondly, adding a binder into the mixed slurry prepared in the step one, and performing vacuum filtration to obtain a graphene oxide membrane (GO membrane).
Placing the GO membrane prepared in the step II into a vacuum drying oven for drying for 2 hours to obtain a dried GO membrane, wherein the drying temperature is 80 ℃;
fourthly, putting the GO membrane obtained by drying in the third step into a tubular furnace, carrying out carbonization treatment, and then naturally cooling.
And fifthly, putting the reduced graphene oxide (rGO) film obtained in the fourth step into a graphitization furnace, performing graphitization atom recombination treatment, and naturally cooling to room temperature to obtain the graphene heat conduction film.
And sixthly, calendering the graphene heat-conducting film obtained in the fifth step to obtain the graphene film with high flexibility, high compactness and high heat conductivity.
Preferably, the fiber raw material comprises plant fiber, chemical fiber and mixed fiber thereof, and plant fiber is further selected.
Preferentially, the vacuum drying time of the GO membrane is 2 hours, and the drying temperature is 80 ℃.
Preferably, the beating degree of the PFI refining is in the range of 40-50 DEG SR, and the PFI refining is further selected to be ground to 45 DEG SR.
Preferably, the concentration of the graphene oxide is 10% -80%, and preferably 40%.
Preferably, the binder comprises polyvinylidene fluoride, sodium carboxymethylcellulose, polyvinyl alcohol and styrene butadiene rubber, and polyvinyl alcohol is further selected.
Preferably, the concentration of the added binder is 2% -10%, and further 5%.
Preferably, the prepared graphene oxide film has a quantitative ratio of 50-80g/m2Further, 60g/m is selected2。
Preferentially, in the carbonization process, the temperature is firstly increased to 300 ℃, the temperature is kept for 30-50min, further 40min is selected, the temperature is continuously increased to 500 ℃, the temperature is kept for 30-50min, further 40min is selected, the temperature is continuously increased to 600-1000 ℃, the temperature is kept for 30-50min, further temperature is increased to 800 ℃, the temperature is kept for 40min, and the temperature increase rate is 10 ℃/min.
Preferably, the temperature of graphene is 2500-3000 ℃, the heat preservation is carried out for 5-8h, and further the temperature of graphitization is 2800 ℃, and the heat preservation is carried out for 6 h.
Preferably, the calendering pressure is 40-60N/cm and the calendering speed is 2-5m/min, and further, the calendering pressure is 50N/cm and the calendering speed is 3 m/min.
The invention provides the graphene heat-conducting film prepared by the method in the scheme, and the thickness of the graphene heat-conducting film is 60100um below zero, a thermal conductivity not less than 1000W/(m.k), a folding endurance more than 104Next, the process is carried out.
Compared with the prior art, the invention has the beneficial effects that:
compared with the graphene which is mechanically stripped, the graphene oxide adopted by the invention has the advantages of large sheet diameter, high single-layer rate, generation of tiny air bags during high-temperature reduction, good mechanical performance after rolling, and the graphene is of a six-membered alkene ring structure, so that compared with the polyimide graphitization process, the energy required by atom rearrangement repair is less, and the energy consumption is saved.
According to the invention, the graphene oxide and the fibers are ground into slurry, so that the graphene oxide and the fibers are fully mixed, the film forming property of the graphene oxide is facilitated, and the prepared graphene film has uniform heat conductivity. The beating degree is controlled to enable the fibers and the graphene oxide to reach a proper film forming condition, and the binding agent is added to increase the film forming strength of the fibers and the graphene oxide, so that the fibers and the graphene oxide cannot fall off in the high-temperature carbonization process. Meanwhile, the graphene oxide is embedded in the fiber network and forms a heat conduction network structure with the fibers, and in the high-temperature carbonization treatment process, the graphene oxide is reduced into reduced graphene oxide, so that the heat conduction network structure formed by combining the graphene oxide and the fibers is more compact, and the heat conduction performance of the heat conduction film is better improved.
The graphene heat-conducting film can be formed on a paper machine, the production efficiency is high, the large-scale production can be realized quickly, and the later-stage carbonized film can keep certain mechanical strength by controlling and adjusting the using amount of the binder.
Drawings
Fig. 1 is a diagram of a graphene thermal conductive film product according to the present invention;
fig. 2 is an SEM image of the graphene thermal conductive film prepared in example 1.
Detailed Description
The present invention is described in detail below with reference to specific examples, which will help those skilled in the art to further understand the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
Mixing 6g of graphene oxide and 24g of hardwood fiber raw materials, adding water into the mixed slurry to dilute the mixed slurry until the concentration is 10%, wherein the mass of the graphene oxide accounts for 20% of the total mass of the fiber raw materials and the graphene oxide, mixing the slurry and putting the mixture into a PFI disc mill to carry out pulp grinding to obtain the mixed slurry of the graphene oxide and the fibers, and the beating degree is 45 DEG SR.
15g of polyvinyl alcohol is added into the prepared mixed slurry, the mass concentration of the added polyvinyl alcohol is 5%, and the graphene oxide membrane (GO membrane) is obtained through vacuum filtration.
Placing the GO membrane prepared in the step II into a vacuum drying oven for drying for 2 hours to obtain a dried GO membrane, wherein the drying temperature is 80 ℃;
fourthly, putting the GO membrane obtained by drying in the third step into a tubular furnace, carrying out carbonization treatment, firstly heating to 300 ℃ in the carbonization process, keeping the temperature for 40min, continuously heating to 500 ℃, keeping the temperature for 40min, continuously heating to 800 ℃, keeping the temperature for 40min, and naturally cooling at the heating rate of 10 ℃/min.
And fifthly, putting the reduced graphene oxide (rGO) film obtained in the fourth step into a graphitization furnace, performing graphitization atom recombination treatment, keeping the graphene temperature at 2800 ℃, and naturally cooling to room temperature for 6 hours to obtain the graphene heat-conducting film.
And sixthly, calendering the graphene heat-conducting film obtained in the fifth step, wherein the calendering pressure is 50N/cm, and the calendering speed is 3m/min, and finally obtaining the high-flexibility, high-density and high-heat-conductivity graphene heat-conducting film.
As can be seen from the SEM image of the graphene thermal conductive film in fig. 2, the reduced graphene oxide covers the surface of the fiber network structure or is embedded therein, and is tightly bonded with the fibers to construct a thermal conductive network structure, and the reduced graphene oxide is uniformly distributed and well oriented in the thermal conductive network structure, thereby greatly improving the thermal conductive performance and mechanical performance of the thermal conductive film in the plane.
Example 2
Mixing 12g of graphene oxide and 18g of hardwood fiber raw materials, adding water into the mixed slurry to dilute the mixed slurry until the concentration is 10%, wherein the mass of the graphene oxide accounts for 40% of the total mass of the fiber raw materials and the graphene oxide, mixing the slurry and putting the mixture into a PFI disc mill to carry out pulp grinding to obtain the mixed slurry of the graphene oxide and the fibers, and the beating degree is 45 DEG SR.
Adding 15g of polyvinyl alcohol into the prepared mixed slurry, wherein the mass concentration of the added polyvinyl alcohol is 5%, and performing vacuum filtration to obtain a graphene oxide membrane (GO membrane).
Placing the GO membrane prepared in the step II into a vacuum drying oven for drying for 2 hours to obtain a dried GO membrane, wherein the drying temperature is 80 ℃;
fourthly, putting the GO membrane obtained by drying in the third step into a tubular furnace, carrying out carbonization treatment, firstly heating to 300 ℃ in the carbonization process, keeping the temperature for 40min, continuously heating to 500 ℃, keeping the temperature for 40min, continuously heating to 800 ℃, keeping the temperature for 40min, and naturally cooling at the heating rate of 10 ℃/min.
And fifthly, putting the reduced graphene oxide (rGO) film obtained in the fourth step into a graphitization furnace, performing graphitization atom recombination treatment, keeping the graphene temperature at 2800 ℃, and naturally cooling to room temperature for 6 hours to obtain the graphene heat-conducting film.
And sixthly, calendering the graphene heat-conducting film obtained in the fifth step, wherein the calendering pressure is 50N/cm, and the calendering speed is 3m/min, and finally obtaining the high-flexibility, high-density and high-heat-conductivity graphene heat-conducting film.
Example 3
Mixing 18g of graphene oxide and 12g of hardwood fiber raw materials, adding water into the mixed slurry to dilute the mixed slurry until the concentration is 10%, wherein the mass of the graphene oxide accounts for 60% of the total mass of the fiber raw materials and the graphene oxide, mixing the slurry and putting the mixture into a PFI disc mill to carry out pulp grinding to obtain the mixed slurry of the graphene oxide and the fibers, and the beating degree is 45 DEG SR.
And adding 18g of polyvinyl alcohol into the prepared mixed slurry, wherein the mass concentration of the added polyvinyl alcohol is 6%, and performing vacuum filtration to obtain a graphene oxide membrane (GO membrane).
Placing the GO membrane prepared in the step II into a vacuum drying oven for drying for 2 hours to obtain a dried GO membrane, wherein the drying temperature is 80 ℃;
fourthly, putting the GO membrane obtained by drying in the third step into a tubular furnace, carrying out carbonization treatment, firstly heating to 300 ℃ in the carbonization process, keeping the temperature for 30min, continuously heating to 500 ℃, keeping the temperature for 30min, continuously heating to 800 ℃, keeping the temperature for 30min, and naturally cooling at the heating rate of 10 ℃/min.
And fifthly, putting the reduced graphene oxide (rGO) membrane obtained in the fourth step into a graphitization furnace, performing graphitization atom recombination treatment, keeping the graphene temperature at 2500 ℃, and naturally cooling to room temperature for 5 hours to obtain the graphene heat-conducting membrane.
And sixthly, calendering the graphene heat-conducting film obtained in the fifth step, wherein the calendering pressure is 40N/cm, and the calendering speed is 2m/min, and finally obtaining the high-flexibility, high-density and high-heat-conductivity graphene heat-conducting film.
Example 4
Mixing 24g of graphene oxide and 6g of hardwood fiber raw materials, adding water into the mixed slurry to dilute the mixed slurry until the concentration is 10%, wherein the mass of the graphene oxide accounts for 80% of the total mass of the fiber raw materials and the graphene oxide, mixing the slurry and putting the mixture into a PFI disc mill to carry out pulp grinding to obtain the mixed slurry of the graphene oxide and the fibers, and the beating degree is 45 DEG SR.
And adding 30g of polyvinyl alcohol into the prepared mixed slurry, wherein the mass concentration of the added polyvinyl alcohol is 10%, and performing vacuum filtration to obtain a graphene oxide membrane (GO membrane).
Placing the GO membrane prepared in the step II into a vacuum drying oven for drying for 2 hours to obtain a dried GO membrane, wherein the drying temperature is 80 ℃;
fourthly, putting the GO membrane obtained by drying in the third step into a tubular furnace, carrying out carbonization treatment, firstly heating to 300 ℃ in the carbonization process, keeping the temperature for 30min, continuously heating to 500 ℃, keeping the temperature for 30min, continuously heating to 800 ℃, keeping the temperature for 30min, and naturally cooling at the heating rate of 10 ℃/min.
And fifthly, putting the reduced graphene oxide (rGO) membrane obtained in the fourth step into a graphitization furnace, performing graphitization atom recombination treatment, keeping the graphene temperature at 2500 ℃, and naturally cooling to room temperature for 5 hours to obtain the graphene heat-conducting membrane.
And sixthly, calendering the graphene heat-conducting film obtained in the fifth step, wherein the calendering pressure is 40N/cm, and the calendering speed is 2m/min, and finally obtaining the high-flexibility, high-density and high-heat-conductivity graphene heat-conducting film.
The products prepared in examples 1 to 4 can be seen in FIG. 1.
Table 1 graphene thermal conductive film performance test results
As can be seen from Table 1, the thermal conductivity of the graphene thermal conductive film increases with the increase of the content of graphene, and the thickness of the graphene thermal conductive film prepared in examples 1 to 4 is 60 to 100um, the thermal conductivity is not less than 1000W/(m.K), and the folding endurance is more than 104Inferior high heat conduction graphite alkene heat conduction membrane, graphite alkene heat conduction membrane surface is level and smooth moreover, and the film forming property is excellent. Example 4 is the best example, and the thermal conductivity coefficient reaches 1848W/m.k. The above embodiment shows that the thermal conductivity coefficient of the graphene can reach over 1000W/m.k when the graphene is used in a small amount, and the heat dissipation requirement of most electronic components can be basically met. Therefore, the graphene heat-conducting film prepared by the preparation method has good high heat-conducting and high-temperature-resistant properties and good film-forming property.
It should be understood that the above detailed description of the embodiments of the present invention with reference to the preferred embodiments is illustrative and not restrictive, and it should not be considered that the detailed description of the embodiments of the present invention is limited thereto, and it should be understood that those skilled in the art to which the present invention pertains that modifications may be made to the embodiments described in the embodiments or that equivalents may be substituted for some of the features thereof without departing from the spirit of the present invention and the scope of the patent protection is defined by the claims to be filed with the present invention.
The above examples of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a graphene film with high thermal conductivity is characterized by comprising the following steps:
firstly, mixing graphene oxide and fiber raw materials, and putting the mixture into a PFI disc mill for grinding to obtain mixed slurry of the graphene oxide and the fiber, wherein the concentration of the mixed slurry is 10%;
secondly, adding a binder into the mixed slurry prepared in the step one, and performing vacuum filtration to obtain a graphene oxide membrane (GO membrane);
thirdly, drying the GO membrane prepared in the second step in a vacuum drying oven for 2-4 hours to obtain a dried GO membrane;
fourthly, putting the GO membrane obtained by drying in the third step into a tubular furnace, carrying out carbonization treatment, and then naturally cooling;
placing the reduced graphene oxide film obtained in the step (iv) into a graphitization furnace, performing graphitization atom recombination treatment, and naturally cooling to room temperature to obtain a graphene heat conduction film;
sixthly, calendaring the graphene heat-conducting film obtained in the fifth step to obtain the graphene film with high flexibility, high compactness and high heat conductivity.
2. The preparation method of the graphene film with high thermal conductivity according to claim 1, wherein in the step (i), the fiber raw material comprises plant fibers, chemical fibers and mixed fibers of the plant fibers and the chemical fibers, and the PFI is disc-milled until the beating degree is 40-50 ° SR.
3. The preparation method of the graphene film with high thermal conductivity according to claim 1, wherein in the step (i), the mass of the graphene oxide accounts for 10% -80% of the total mass of the fiber raw material and the graphene oxide.
4. The method for preparing the graphene film with high thermal conductivity according to claim 1, wherein in the step (II), the binder comprises polyvinylidene fluoride, sodium carboxymethylcellulose, polyvinyl alcohol or styrene-butadiene rubber.
5. The preparation method of the graphene film with high thermal conductivity according to claim 1, wherein in the second step, the concentration of the binder is 2%-10% and the quantitative amount of graphene oxide film is 50-80g/m2。
6. The method for preparing the graphene film with high thermal conductivity according to claim 1, wherein in the third step, the drying temperature is 80-100 ℃.
7. The preparation method of the graphene film with high thermal conductivity according to claim 1, wherein in the step (iv), the temperature is raised to 300 ℃ and maintained for 30-50min in the carbonization process, the temperature is raised to 500 ℃ and maintained for 30-50min, the temperature is raised to 600-1000 ℃ and maintained for 30-50min, and the temperature raising rate is 10 ℃/min.
8. The method for preparing the graphene film with high thermal conductivity according to claim 1, wherein in the fifth step, the graphene temperature is 2500 ℃ to 3000 ℃, and the temperature is kept for 5 to 8 hours.
9. The method for preparing the graphene film with high thermal conductivity according to claim 1, wherein the calendering pressure in the step (sixthly) is 40 to 60N/cm, and the calendering speed is 2 to 5 m/min.
10. The graphene film with high thermal conductivity prepared by the method of any one of claims 1 to 9, wherein the graphene film with high thermal conductivity has a thickness of 60-100um, a thermal conductivity of not less than 1000W/(m.k), and a folding endurance of more than 104Next, the process is carried out.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115285980A (en) * | 2022-08-17 | 2022-11-04 | 安徽汉烯科技有限公司 | Super-thick macroscopic graphene radiating fin for heat source and preparation method |
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| CN106968128A (en) * | 2017-04-12 | 2017-07-21 | 株洲时代新材料科技股份有限公司 | A kind of soft graphite alkenyl extrusion coating paper and its preparation method and application |
| CN109956466A (en) * | 2019-04-10 | 2019-07-02 | 湖南大学 | It is a kind of to have both direction and the graphene-based composite membrane of thickness direction high heat conductance and preparation method thereof in face |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106968128A (en) * | 2017-04-12 | 2017-07-21 | 株洲时代新材料科技股份有限公司 | A kind of soft graphite alkenyl extrusion coating paper and its preparation method and application |
| CN109956466A (en) * | 2019-04-10 | 2019-07-02 | 湖南大学 | It is a kind of to have both direction and the graphene-based composite membrane of thickness direction high heat conductance and preparation method thereof in face |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115285980A (en) * | 2022-08-17 | 2022-11-04 | 安徽汉烯科技有限公司 | Super-thick macroscopic graphene radiating fin for heat source and preparation method |
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