CN111286309A - High-performance graphene heat dissipation film, and preparation method and application thereof - Google Patents
High-performance graphene heat dissipation film, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-performance graphene heat dissipation film, and a preparation method and application thereof. The high-performance graphene heat dissipation film is prepared by forming graphene composite slurry by using oxidized thin-layer graphene, non-oxidized thin-layer graphene, a dispersing agent, a solvent and the like according to a certain ratio, and then sequentially performing processes such as coating, drying, thermal reduction, graphitization, calendering and the like. The high-performance graphene heat dissipation film provided by the invention is simple and efficient in production process, can effectively overcome the problems of low drying process efficiency, excessive reduction of film thickness in a carbonization process and the like when pure oxygen graphene is used as a raw material, is low in cost and suitable for large-scale production, is high in heat conductivity coefficient (up to 800-.
Description
Technical Field
The invention relates to a heat dissipation material, in particular to a high-performance graphene heat dissipation film, and a preparation method and application thereof, and belongs to the technical field of nano materials.
Background
With the rapid development of electronic information technology, electronic devices are increasingly developed to be light, thin and small, that is, miniaturization is required, but this causes the power density of the devices to gradually increase, heat to be accumulated and not to be dissipated in a short time, which leads to a sharp rise in the temperature of a chip and severe performance and safety of the electronic devices. At present, the mainstream heat dissipation solution in handheld electronic devices such as mobile phones and flat panels is to use a high-thermal-conductivity graphite film as a main heat dissipation component. The existing commercially available high-thermal-conductivity graphite film is mainly prepared by sintering polyimide (see CN103080005A), and because the graphite film mainly depends on import, the preparation cost is high, and the sintering and heating process is complex, a lot of uncertain factors are brought to production. In addition, the prepared graphite film cannot meet the heat dissipation requirement due to low thickness, and a plurality of layers of graphite films need to be stacked through the binder, so that the performance of the graphite film is seriously influenced and the production efficiency is reduced due to extremely low heat conductivity of the high-molecular binder.
Emerging graphene is a two-dimensional carbon nano-structure material formed by single-layer graphite sheets, the theoretical thermal conductivity can reach 3000-5000W/mK, and the graphene is an ideal heat conduction material. At present, graphene oxide is mainly used as a main raw material for preparing a graphene heat dissipation film, and the preparation method comprises the following steps: graphene oxide is dispersed in water to form a graphene oxide dispersion liquid, and then a graphene heat dissipation film (such as CN110255538A, CN105084858B, and CN108178148A) is obtained through coating, drying, carbonization, graphitization, and calendaring processes, however, in the drying process, moisture in the graphene oxide is difficult to dry in a short time at a low temperature, and if the temperature rises, the moisture volatilizes too fast to cause severe film cavities, so that a long-time low-temperature treatment is required, and the production efficiency is seriously affected. In addition, the thickness of the finally obtained graphene heat dissipation film is obviously reduced due to too many oxygen-containing functional groups of the graphene oxide in the carbonization process.
Disclosure of Invention
The invention mainly aims to provide a high-performance graphene heat dissipation film, and a preparation method and application thereof, so that the defects of the prior art are overcome.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides graphene composite slurry, which comprises thin-layer graphene oxide, thin-layer graphene non-oxide, a dispersing agent and a solvent; wherein the mass ratio of the non-oxidized thin-layer graphene to the oxidized thin-layer graphene is greater than or equal to 1:100 and less than or equal to 100:1, and the viscosity of the composite slurry is 10000-.
Further, the non-oxidized thin-layer graphene comprises graphene nanoplatelets prepared by any one of intercalation cleavage method, liquid phase cleavage method and mechanical exfoliation method, wherein the carbon content is more than 95 wt%.
The embodiment of the invention also provides application of the graphene composite slurry in preparation of a graphene heat dissipation structure.
The embodiment of the invention also provides a preparation method of the high-performance graphene heat dissipation film, which comprises the following steps:
providing the graphene composite slurry;
and carrying out film forming treatment on the graphene composite slurry, and then sequentially carrying out drying, reduction carbonization and graphitization treatment, thereby obtaining the high-performance graphene heat dissipation film.
The embodiment of the invention also provides a preparation method of the high-performance graphene heat dissipation film, which comprises the following steps:
providing the graphene composite slurry;
coating the graphene composite slurry on a substrate after vacuum defoaming treatment, then drying to form a graphene composite membrane, then carrying out reduction carbonization treatment on the graphene composite membrane in a protective atmosphere, then cooling to carry out calendering treatment, then carrying out graphitization treatment in the protective atmosphere, and then carrying out calendering treatment again to obtain the high-performance graphene heat dissipation membrane.
The embodiment of the invention also provides a high-performance graphene heat dissipation film which can be prepared by any one of the methods and has the heat conductivity coefficient of 800-.
The embodiment of the invention also provides a preparation system of the high-performance graphene heat dissipation film, which is applied to any one of the preparation methods, wherein the preparation system comprises:
the dispersion equipment is at least used for uniformly dispersing the oxidized thin-layer graphene slurry, the non-oxidized thin-layer graphene slurry and the dispersing agent to form graphene composite slurry;
the film forming equipment is at least used for coating the graphene composite slurry on a flexible substrate to form a slurry layer;
a drying device at least used for removing the solvent in the slurry layer so as to form a continuous graphene composite membrane;
the high-temperature carbonization equipment is at least used for carrying out reduction carbonization treatment on the graphene composite film so as to form a carbonized graphene film;
a high-temperature graphitization apparatus at least for performing graphitization treatment on the carbonized graphene film to form a graphitized graphene film; and
and the rolling equipment is at least used for rolling the carbonized graphene film and the graphitized graphene film respectively.
The embodiment of the invention also provides application of the high-performance graphene heat dissipation film, such as application in electronic products, electromechanical products, photoelectric equipment, semiconductor equipment and the like.
Compared with the prior art, the invention has the advantages that: the graphene heat dissipation film is prepared by taking the combination of the oxidized thin-layer graphene and the non-oxidized thin-layer graphene as raw materials, so that the problems of low drying process efficiency and excessive reduction of film thickness in the carbonization process when the graphene heat dissipation film is prepared by taking pure graphene oxide as the raw material can be effectively solved, and the obtained graphene heat dissipation film is high in heat conductivity coefficient, controllable in film thickness, wide in application prospect, simple in production process, low in cost and suitable for large-scale production.
Detailed Description
In view of the shortcomings in the prior art, the inventors of the present invention have made extensive studies and extensive practices to propose a technical solution of the present invention, which will be described in detail below.
An aspect of the embodiments of the present invention provides a graphene composite slurry including thin-layer graphene oxide, thin-layer graphene non-oxide, a dispersant, and a solvent; wherein the mass ratio of the non-oxidized thin-layer graphene to the oxidized thin-layer graphene is greater than or equal to 1:100 and less than or equal to 100:1 (preferably greater than 1:100 and less than 100:1), and the viscosity of the composite slurry is 10000-100000 mPas.
In some embodiments, the composite slurry further comprises a dispersant in an amount of 1 to 10 wt% of the amount of the non-oxidized thin-layer graphene.
Further, the dispersant includes one or a combination of two or more of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, cetylammonium bromide, sodium dodecylsulfonate, sodium dodecylbenzenesulfonate, sodium alkyldiphenyletherdisulfonate, Triton-100, tween, Tego Dispers610s, BYK163, BYK190, BYK420, sodium polyacrylate, polyacrylamide, acrylic resin, and modified acrylic resin, and is not limited thereto.
Further, the solvent includes deionized water, and is not limited thereto.
In some embodiments, the composite slurry further comprises 1-10 wt% co-solvent.
Further, the co-solvent includes water-compatible organic solvents including alcohols, ether solvents such as methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, glycerol, n-propanol, isopropanol, n-butanol, isobutanol, t-butanol, tripropylene glycol butyl ether, dipropylene glycol butyl ether, propylene glycol methyl ether, tripropylene glycol methyl ether, dipropylene glycol propyl ether, ethylene glycol hexyl ether, diethylene glycol butyl ether solvents, or any one or a combination of two or more thereof, and is not limited thereto.
Further, the size of the graphene oxide film is 0.1-100 μm, the number of layers is 1-10, and the molar ratio of carbon element to oxygen element is 0.5-10: 1.
in some embodiments, the non-oxidized thin-layer graphene includes graphene nanoplatelets prepared by any one of intercalation cleavage, liquid phase cleavage, mechanical exfoliation.
Further, the size of the non-oxidized thin-layer graphene is 0.5-100 μm, the number of layers is 1-10, and the carbon content is more than 95 wt%, preferably more than 97 wt%.
In some embodiments, the composite slurry is mainly formed by uniformly mixing an oxidized thin-layer graphene slurry with a solid content of 0.5-8 wt%, a non-oxidized thin-layer graphene slurry with a solid content of 3-10 wt% and a dispersing agent.
Another aspect of the embodiments of the present invention provides a use of the graphene composite paste in preparing a graphene heat dissipation structure. The graphene heat dissipation structure can be in a regular shape or an irregular shape such as a film shape, a sheet shape, a plate shape, a block shape and the like. Moreover, the graphene heat dissipation structure can be applied to various occasions needing heat dissipation.
Another aspect of the embodiments of the present invention also provides a method for preparing a high-performance graphene heat dissipation film, including:
providing any one of the graphene composite slurries described above;
and carrying out film forming treatment on the graphene composite slurry, and then sequentially carrying out drying, reduction carbonization and graphitization treatment, thereby obtaining the high-performance graphene heat dissipation film.
In some embodiments, the method of making comprises: mixing oxidized thin-layer graphene and non-oxidized thin-layer graphene according to a certain proportion to form uniformly dispersed graphene composite slurry, and then carrying out processes such as coating, drying, rolling, slicing, carbonizing, graphitizing, calendering and the like to prepare the high-performance graphene heat dissipation film with the heat conductivity coefficient of 800-1600W/m.k.
In some embodiments, the method of making can further comprise: mixing and uniformly dispersing oxidized thin-layer graphene slurry (solid content, namely the content of the oxidized thin-layer graphene is 0.5-8 wt%) and non-oxidized thin-layer graphene slurry (solid content, namely the content of the non-oxidized thin-layer graphene is 3-10 wt%) to form graphene composite slurry, wherein the viscosity of the graphene composite slurry is 10000-100000 mPas. Further, the graphene composite slurry comprises the following components: the graphene oxide film comprises non-oxidized thin-layer graphene, a dispersing agent and deionized water.
Further, the graphene oxide may be prepared by one or more methods known in the art, such as a solution chemical method, an electrochemical method, and a plasma oxidation method, which use graphite as a raw material (but not limited thereto), and then may be dispersed in deionized water to form a graphene oxide slurry.
Further, the non-oxidized thin-layer graphene may be prepared by one or more methods known in the art, such as intercalation and cleavage method, mechanical exfoliation method, etc., and then may be dispersed in deionized water by a dispersant to obtain a non-oxidized thin-layer graphene slurry. Wherein the size of the non-oxidized thin-layer graphene is 0.5-100 mu m, the thickness is 1-20 layers, and the purity is more than 97 wt%.
In some embodiments, the film forming process comprises: and performing vacuum defoaming treatment on the graphene composite slurry, and then coating the graphene composite slurry on a substrate, wherein the coating thickness is 0.5-10 mm.
Further, the substrate includes a flexible substrate, such as a release PET film or a release paper, and the like, and is not limited thereto.
Further, in the film formation process, the substrate is continuously moved at a speed of 0.5 to 5 m/min.
In some embodiments, the drying process comprises: and (3) after the graphene composite slurry is subjected to film forming treatment, heating at 60-100 ℃ for more than 10min to form the graphene composite film.
In some embodiments, the conditions of the reduction carbonization treatment include: the reduction carbonization is carried out in protective atmosphere, and the temperature of the reduction carbonization is 800-1100 ℃ for 1-3 h.
In some embodiments, the graphitization treatment conditions include: graphitizing in protective atmosphere at 2500-3000 deg.C for 2-8 h.
Further, the aforementioned protective atmosphere includes, but is not limited to, a high purity nitrogen atmosphere, an inert atmosphere such as argon, and the like.
In some embodiments, the preparation method specifically may comprise: and after the film forming treatment is carried out on the graphene composite slurry, drying, reduction carbonization, primary rolling, graphitization treatment and secondary rolling treatment are sequentially carried out, so that the high-performance graphene heat dissipation film is obtained.
Further, the pressure adopted by the first calendering treatment is 1-10 MPa.
Further, the pressure of the second rolling treatment is 5-20 MPa.
Another aspect of the embodiments of the present invention also provides a method for preparing a high-performance graphene heat dissipation film, including:
providing the graphene composite slurry;
coating the graphene composite slurry on a substrate after vacuum defoaming treatment, wherein the coating thickness is 0.5-10mm, then drying at 60-100 ℃ for 10-60min to form a graphene composite membrane, then carrying out reduction carbonization on the graphene composite membrane at 800-1100 ℃ in a protective atmosphere for 1-3h, then cooling and carrying out calendering treatment at the pressure of 1-10MPa, then carrying out graphitization at 2500-3000 ℃ in the protective atmosphere for 2-8h, then cooling and calendering treatment at the pressure of 5-20MPa to obtain the high-performance graphene heat dissipation membrane.
In some embodiments, the preparation method specifically may comprise: coating the graphene composite slurry on a flexible substrate after vacuum defoaming treatment, then drying, stripping, rolling and slicing the formed graphene composite film from the flexible substrate, and then carrying out reduction carbonization treatment.
Further, the flexible substrate is continuously traveling at a speed of 0.5 to 5 m/min.
Further, the flexible substrate includes a release PET film or a release paper, and is not limited thereto.
In some more specific embodiments, the preparation method may comprise: coating the graphene composite slurry on a release PET or release paper substrate at the speed of 0.5-5m/min after vacuum defoaming treatment, wherein the coating thickness is 0.5-10mm, then heating at 60-100 ℃ for 10-60min to form a graphene composite film of oxidized thin-layer graphene and non-oxidized thin-layer graphene, and then stripping, rolling and slicing the graphene composite film from the substrate.
In another aspect, the embodiment of the invention further provides a high-performance graphene heat dissipation film prepared by any one of the methods, wherein the thermal conductivity is 800-.
Furthermore, the thickness of the high-performance graphene heat dissipation film is preferably 0.01-1mm, so that the high-performance graphene heat dissipation film can be applied to a plurality of narrow spaces, such as mobile phones, ultra-thin displays, power batteries or other applications requiring high heat conductivity and ultra-thin heat dissipation structures.
Another aspect of the embodiment of the present invention further provides a system for preparing a high-performance graphene heat dissipation film, which is applied to any one of the preparation methods described above; and the preparation system comprises:
the dispersion equipment is at least used for uniformly dispersing the oxidized thin-layer graphene slurry, the non-oxidized thin-layer graphene slurry and the dispersing agent to form graphene composite slurry;
the film forming equipment is at least used for coating the graphene composite slurry on a flexible substrate to form a slurry layer;
a drying device at least used for removing the solvent in the slurry layer so as to form a continuous graphene composite membrane;
the high-temperature carbonization equipment is at least used for carrying out reduction carbonization treatment on the graphene composite film so as to form a carbonized graphene film;
a high-temperature graphitization apparatus at least for performing graphitization treatment on the carbonized graphene film to form a graphitized graphene film; and
and the rolling equipment is at least used for rolling the carbonized graphene film and the graphitized graphene film respectively.
Wherein, the dispersing equipment can be selected from but not limited to a planetary stirrer, a high-speed disperser, a ball mill, a sand mill, a homogenizer and the like.
The film forming apparatus can be selected from, but not limited to, coating apparatuses, such as comma coaters.
The drying device may be, but is not limited to, a tunnel oven, and the oven heating may be one or two of electric heating, natural gas heating, and steam heating, and is not limited thereto.
Wherein, the high-temperature carbonization equipment can be selected from the equipment known in the field, and the maximum working temperature can be 1200 ℃, or higher and lower temperature.
The high temperature graphitization equipment can be selected from the equipment known in the art, and the maximum working temperature can be 3000 ℃ or higher or lower.
The calendering equipment is used for making the graphene film more compact and improving the mechanical property, and the working pressure of the calendering equipment can be more than or equal to 30 MPa.
Another aspect of the embodiments of the present invention further provides a device, including a functional unit and a heat dissipation structure cooperating with the functional unit, where the heat dissipation structure includes any one of the foregoing high performance graphene heat dissipation films. For example, the high-performance graphene heat dissipation film can be directly attached to the functional unit or bonded to the functional unit through a heat conductive adhesive or the like, so that heat generated by the functional unit during operation can be rapidly conducted out and dissipated.
Further, the device includes any one or a combination of electronic devices and mechanical devices, such as a mobile phone, a computer, a television, a chip, a battery, and the like, and is not limited thereto.
According to the invention, the graphene oxide and non-graphene oxide are combined according to a specific proportion as raw materials, and then the graphene heat dissipation film is prepared by using the graphene oxide and non-graphene oxide as raw materials, so that the production process is simple and efficient, the problems of low efficiency in a drying process and excessive reduction of film thickness in a carbonization process existing when pure graphene oxide is used as a raw material can be effectively solved, meanwhile, the cost is low, the graphene heat dissipation film is suitable for large-scale production, the obtained graphene heat dissipation film has high heat conductivity coefficient (up to 800 plus 1600W/m.K), the film thickness is controllable (for example, the film thickness can be adjusted within the range of 0.01-1 mm), and the graphene heat dissipation film has a wide application prospect in the fields of mobile phones, tablet computers, LEDs, ultra-thin displays, power batteries and the like, and especially has an important significance.
The technical solutions of the present invention will be explained in more detail with reference to several embodiments, but the specific embodiments described herein are only for explaining the present invention and are not intended to limit the present invention. The methods in the following examples, unless otherwise specified, are conventional in the art.
Embodiment 1 is a method for preparing a high-performance graphene heat dissipation film, including the steps of:
(1) preparing graphene composite slurry: mixing 12.5 parts (weight parts if not specifically stated below) of graphene oxide thin-layer dispersion liquid with a solid content of 8 wt% and 100 parts (corresponding to a mass ratio of graphene oxide to graphene non-oxide thin-layer) of graphene non-oxide thin-layer dispersion liquid with a solid content of 10 wt% in a double-planetary dispersing machine for 1-6h at a linear speed of 10-50m/min to obtain graphene composite slurry with a viscosity of 30000-.
Wherein, the graphene oxide thin layer is prepared by hummers method according to the known mode in the field, the size is 0.1-100 μm, the number of layers is 1-10, and C/O is 0.5-10, and then the graphene oxide thin layer is dispersed in deionized water to form the graphene oxide thin layer slurry.
The non-oxidized thin-layer graphene is prepared by a mechanical stripping method according to a known mode in the art, the size of the non-oxidized thin-layer graphene is 0.5-100 mu m, the thickness of the thin-layer graphene is 1-10 layers, the carbon content purity is more than 95 wt%, and then the non-oxidized thin-layer graphene slurry is obtained by dispersing a dispersing agent such as polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol or sodium carboxymethylcellulose in deionized water. The amount of the dispersant is 10 wt% of the amount of the non-oxidized thin-layer graphene.
(2) Defoaming the graphene composite slurry by using a vacuum degassing system, conveying the graphene composite slurry to a comma coater through a pipeline, and coating the graphene composite slurry on a release PET (polyethylene terephthalate) film, wherein the thickness of slurry coating is 0.5-10mm, and the speed is 0.5-5 m/min; then, drying by adopting a tunnel type drying oven at the drying temperature of 60-100 ℃ for 10-30min to remove water; and stripping, rolling and slicing the dried graphene dry film from the release PET film, carbonizing for 1-3h at 1100 ℃ under the nitrogen atmosphere, cooling, performing calendering treatment at 1-10MPa, graphitizing for 2-8h at 3000 ℃ under 2500-20 MPa, and performing calendering treatment at 5-20MPa to obtain the graphene heat dissipation film with the thickness of about 0.05-0.5mm and the heat conductivity of 800-1200W/m.K.
Example 2: a preparation method of a high-performance graphene heat dissipation film comprises the following steps:
(1) preparing graphene composite slurry: fully stirring 10 parts of oxidized thin-layer graphene dispersion liquid with the solid content of 0.5 wt% and 100 parts of non-oxidized thin-layer graphene dispersion liquid with the solid content of 5 wt% (corresponding to the mass ratio of oxidized thin-layer graphene to non-oxidized thin-layer graphene being 1: 100) in a double-planet dispersing machine for 1-6h at a linear speed of 10-50m/min to obtain graphene composite slurry with the viscosity of 10000-50000 mPas.
Wherein, the graphene oxide film is prepared by a solution chemical method, an electrochemical method or a plasma oxidation method which takes graphite as a raw material according to a mode known in the art, the size is 0.1-100 μm, the number of layers is 1-10, and C/O is 0.5-10, and then the graphene oxide film is dispersed in deionized water to form the graphene oxide film slurry.
The non-oxidized thin-layer graphene is prepared by intercalation cleavage or liquid phase cleavage according to a known mode in the art, the size is 0.5-100 mu m, the thickness of the thin-layer graphene is 1-10 layers, the carbon content purity is more than 97 wt%, and then dispersing agents such as cetyl ammonium bromide, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, alkyl diphenyl ether disulfonate and the like in deionized water to obtain the non-oxidized thin-layer graphene slurry. The amount of the dispersant is 10 wt% of the amount of the non-oxidized thin-layer graphene.
(2) Defoaming the graphene composite slurry by using a vacuum degassing system, conveying the graphene composite slurry to a comma coater through a pipeline, and coating the graphene composite slurry on a release PET (polyethylene terephthalate) film, wherein the thickness of slurry coating is 0.5-10mm, and the speed is 0.5-2 m/min; then, drying by adopting a tunnel type drying oven at the drying temperature of 60-100 ℃ for 10-30min to remove water; and then, stripping, rolling and slicing the dried graphene dry film from the release PET film, carbonizing for 1-3h at 800-1100 ℃ in a nitrogen atmosphere, cooling, performing calendering treatment at 1-10MPa, graphitizing for 2-8h at 3000 ℃ in 2500-20 MPa, and performing calendering treatment at 5-20MPa to obtain the graphene heat dissipation film with the thickness of 0.1-1mm and the heat conductivity of 800-1200W/m.K.
Example 3: a preparation method of a high-performance graphene heat dissipation film comprises the following steps:
(1) preparing graphene composite slurry: fully stirring 20 parts of oxidized thin-layer graphene dispersion liquid with the solid content of 5 wt% and 1 part of non-oxidized thin-layer graphene dispersion liquid with the solid content of 1 wt% (corresponding to the mass ratio of 100:1 of oxidized thin-layer graphene to non-oxidized thin-layer graphene) in a double-planet dispersing machine for 1-6h at a linear speed of 10-50m/min to obtain graphene composite slurry with the viscosity of 40000 and 80000 mPas.
The preparation method of the graphene oxide and the graphene non-oxide can be the same as that of example 1. In addition, the non-oxidized thin-layer graphene can be dispersed in a solvent formed by mixing ethanol and deionized water according to any volume ratio through a dispersing agent such as sodium polyacrylate, polyacrylamide, acrylic resin, modified acrylic resin and the like to obtain the non-oxidized thin-layer graphene slurry. The amount of the dispersant is 5 wt% of the amount of the non-oxidized thin-layer graphene.
(2) Defoaming the graphene composite slurry by using a vacuum degassing system, conveying the graphene composite slurry to a comma coater through a pipeline, and coating the graphene composite slurry on release paper, wherein the thickness of the slurry coating is 0.5-5mm, and the speed is 1-5 m/min; then, drying by adopting a tunnel type drying oven at the drying temperature of 60-100 ℃ for 10-60min to remove water; stripping, rolling and slicing the dried graphene dry film from a substrate film release base material, then carbonizing for 1-3h at 800-1100 ℃ in a nitrogen atmosphere, cooling, carrying out calendering treatment at 1-10MPa, then graphitizing for 2-8h at 2500-3000 ℃, and carrying out calendering treatment at 5-20MPa to obtain the graphene heat dissipation film with the thickness of 0.01-0.2mm and the heat conductivity coefficient of 1000-1600W/m.K.
Example 4: a preparation method of a high-performance graphene heat dissipation film comprises the following steps:
(1) preparing graphene composite slurry: and (2) fully stirring 100 parts of oxidized thin-layer graphene dispersion liquid with the solid content of 5 wt% and 5 parts of non-oxidized thin-layer graphene dispersion liquid with the solid content of 10 wt% (corresponding to the oxidized thin-layer graphene: 10:1) in a double-planet dispersing machine for 1-6h at a linear speed of 10-50m/min to obtain graphene composite slurry with the viscosity of 30000-60000 mPas.
(2) Defoaming the graphene composite slurry by using a vacuum degassing system, conveying the graphene composite slurry to a comma coater through a pipeline, and coating the graphene composite slurry on a release PET (polyethylene terephthalate) film, wherein the thickness of slurry coating is 0.5-5mm, and the speed is 0.5-5 m/min; drying by adopting a tunnel type drying oven to remove moisture, wherein the drying temperature is 60-100 ℃, the drying time is 10-60min, stripping, rolling and slicing the dried graphene dry film from the release PET film, then carbonizing at 1100 ℃ for 1-3h under the nitrogen atmosphere, cooling, performing calendering treatment at 1-10MPa, then graphitizing at 3000 ℃ of 2500-0.5 mm, and performing calendering treatment at 5-20MPa to obtain the graphene heat dissipation film with the thickness of 0.05-0.5mm and the heat conductivity of 1000-1600W/m.K.
Comparative example 1: this comparative example is essentially the same as example 1, except that: in the prepared graphene composite slurry, the oxide thin-layer graphene: the mass ratio of the non-oxidized thin-layer graphene is 0.1: 100. In the comparative example, the graphene composite slurry is coated on a release PET film to form a film, and after drying treatment, the formed graphene composite film has poor mechanical properties, and the film is easy to crack and cannot be completely peeled. The finally formed graphene heat dissipation film has poor compactness and low heat conductivity coefficient (lower than 600W/m.K).
Comparative example 2: this comparative example is essentially the same as example 1, except that: in the prepared graphene composite slurry, the oxide thin-layer graphene: the mass ratio of the non-oxidized thin-layer graphene is 100: 0.1. in the comparison example, the graphene composite slurry is coated on a release PET film to form a film, and when drying treatment is performed, the dry film can be formed only by drying for more than 1h, so that the time consumption is long, and the efficiency is low. And the finally formed graphene heat dissipation film is low in thickness (about 0.01-0.04 mm).
It should be noted that the above-mentioned embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A graphene composite slurry is characterized by comprising thin-layer graphene oxide, thin-layer graphene non-oxide, a dispersant and a solvent; wherein the mass ratio of the non-oxidized thin-layer graphene to the oxidized thin-layer graphene is greater than or equal to 1:100 and less than or equal to 100:1, and the viscosity of the composite slurry is 10000-.
2. The graphene composite paste according to claim 1, wherein: the composite slurry comprises a dispersant, wherein the dosage of the dispersant is 1-10 wt% of that of the non-oxidized thin-layer graphene: preferably, the dispersant comprises one or a combination of more than two of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, hexadecyl ammonium bromide, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium alkyl diphenyl ether disulfonate, Triton-100, Tween, Tego Dispers610s, BYK163, BYK190, BYK420, sodium polyacrylate, polyacrylamide, acrylic resin and modified acrylic resin; and/or, the solvent comprises deionized water; and/or the size of the graphene oxide film is 0.1-100 μm, the number of layers is 1-10, and the molar ratio of carbon element to oxygen element is 0.5-10: 1; and/or the non-oxidized thin-layer graphene comprises graphene micro-sheets prepared by any one of an intercalation cleavage method, a liquid-phase cleavage method and a mechanical exfoliation method; and/or the non-oxidized thin-layer graphene has the size of 0.5-100 mu m, the number of layers is 1-10, and the carbon content is more than 95 wt%; and/or, the composite slurry also comprises 1-10 wt% of cosolvent; preferably, the cosolvent comprises an organic solvent compatible with water, and the organic solvent comprises any one or a combination of more than two of methanol, ethanol, ethylene glycol, 1, 2-propylene glycol, glycerol, n-propanol, isopropanol, n-butanol, isobutanol, tert-butanol, tripropylene glycol butyl ether, dipropylene glycol butyl ether, propylene glycol methyl ether, tripropylene glycol methyl ether, dipropylene glycol propyl ether, ethylene glycol hexyl ether, diethylene glycol hexyl ether and diethylene glycol butyl ether solvents; preferably, the composite slurry is mainly formed by uniformly mixing an oxidized thin-layer graphene slurry with the solid content of 0.5-8 wt%, a non-oxidized thin-layer graphene slurry with the solid content of 3-10 wt% and a dispersing agent.
3. Use of the graphene composite paste according to any one of claims 1-2 for preparing a graphene heat dissipation structure.
4. A preparation method of a high-performance graphene heat dissipation film is characterized by comprising the following steps:
providing the graphene composite paste of any one of claims 1-2;
performing film forming treatment on the graphene composite slurry, and then sequentially performing drying, reduction carbonization and graphitization treatment to obtain a high-performance graphene heat dissipation film;
preferably, the film formation process includes: performing vacuum defoaming treatment on the graphene composite slurry, and then coating the graphene composite slurry on a substrate, wherein the coating thickness is 0.5-10 mm; the substrate comprises a flexible substrate; more preferably, the flexible substrate comprises a release PET film or a release paper; more preferably, the substrate is continuously moved at a speed of 0.5 to 5m/min during the film formation process;
preferably, the drying process comprises: after film forming treatment is carried out on the graphene composite slurry, heating is carried out for more than 10min at the temperature of 60-100 ℃ to form a graphene composite film;
preferably, the conditions of the reduction carbonization treatment include: carrying out reduction carbonization in protective atmosphere, wherein the temperature of the reduction carbonization is 800-1100 ℃, and the time is 1-3 h;
preferably, the graphitization treatment conditions include: graphitizing in protective atmosphere at 2500-3000 deg.C for 2-8 h.
5. The production method according to claim 4, characterized by comprising: after the graphene composite slurry is subjected to film forming treatment, drying, reduction carbonization, primary rolling, graphitization treatment and secondary rolling treatment are sequentially carried out, so that the high-performance graphene heat dissipation film is obtained;
preferably, the pressure adopted by the first calendering treatment is 1-10 MPa;
preferably, the pressure of the second rolling treatment is 5 to 20 MPa.
6. A preparation method of a high-performance graphene heat dissipation film is characterized by comprising the following steps:
providing the graphene composite paste of any one of claims 1-2;
coating the graphene composite slurry on a substrate after vacuum defoaming treatment, wherein the coating thickness is 0.5-10mm, then drying at 60-100 ℃ for 10-60min to form a graphene composite membrane, then carrying out reduction carbonization on the graphene composite membrane at 800-1100 ℃ in a protective atmosphere for 1-3h, then cooling and carrying out calendering treatment at the pressure of 1-10MPa, then carrying out graphitization at 2500-3000 ℃ in the protective atmosphere for 2-8h, then cooling and calendering treatment at the pressure of 5-20MPa to obtain the high-performance graphene heat dissipation membrane.
7. The production method according to claim 6, characterized by comprising: coating the graphene composite slurry on a flexible substrate after vacuum defoaming treatment, then carrying out drying treatment, stripping, rolling and slicing the formed graphene composite film from the flexible substrate, and then carrying out reduction carbonization treatment; preferably, the flexible substrate is continuously traveling at a speed of 0.5 to 5 m/min; preferably, the flexible substrate comprises a release PET film or a release paper.
8. The high-performance graphene heat dissipation film prepared by the method of any one of claims 3 to 7, which has a thermal conductivity of 800-1600W/m.k; preferably, the thickness of the high-performance graphene heat dissipation film is 0.01-1 mm.
9. A preparation system of a high-performance graphene heat dissipation film is applied to the method of any one of claims 3-7; the preparation system is characterized by comprising:
the dispersion equipment is at least used for uniformly dispersing the oxidized thin-layer graphene slurry, the non-oxidized thin-layer graphene slurry and the dispersing agent to form graphene composite slurry;
the film forming equipment is at least used for coating the graphene composite slurry on a flexible substrate to form a slurry layer;
a drying device at least used for removing the solvent in the slurry layer so as to form a continuous graphene composite membrane;
the high-temperature carbonization equipment is at least used for carrying out reduction carbonization treatment on the graphene composite film so as to form a carbonized graphene film;
a high-temperature graphitization apparatus at least for performing graphitization treatment on the carbonized graphene film to form a graphitized graphene film; and
and the rolling equipment is at least used for rolling the carbonized graphene film and the graphitized graphene film respectively.
10. The utility model provides a device, includes functional unit and with functional unit complex heat radiation structure, its characterized in that: the heat dissipation structure comprises the high performance graphene heat dissipation film of claim 8; preferably, the device comprises any one or combination of more of an electronic device and a mechanical device.
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Effective date of registration: 20211028 Address after: 225400 south of Guoqing East Road, Taixing high tech Industrial Development Zone, Taizhou City, Jiangsu Province Patentee after: Taixing Zhifu Display Technology Co.,Ltd. Address before: 215300 no.1107 Gucheng Road, Baicheng Town, Kunshan City, Suzhou City, Jiangsu Province Patentee before: Kunshan Yinda New Material Technology Co., Ltd Patentee before: SUZHOU GRAPHENE NANO TECHNOLOGY Co.,Ltd. |