CN112794716A - Graphene membrane material with specified thickness and preparation method thereof - Google Patents
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Abstract
The invention discloses a graphene membrane material with specified thickness and a preparation method thereof, wherein the formula comprises the following components: the graphene oxide dispersion liquid comprises the following components in percentage: 100% graphene oxide dispersion; according to the invention, only a few graphene films with concentrated standard thickness need to be produced, and the graphene films with any thickness are combined by bonding and stacking through the method, so that the standardized production is facilitated, the production difficulty and cost of a coating link are reduced, the large-scale production of the graphene films is facilitated, a chemical bond is formed between a binder and graphene oxide molecules, the C-C bond is retained after high-temperature thermal reduction, a formed carbon chain is connected with a graphene sheet layer, the phonon heat transfer process can be carried out, compared with other modes for combining the graphene films, the loss of heat conductivity between layers is avoided to the greatest extent, and the binder is a common industrial raw material, is low in cost, is convenient to obtain, has good affinity with graphene oxide, and provides convenience for large-scale production.
Description
Technical Field
The invention relates to the technical field of graphene materials, in particular to a graphene film material with a specified thickness and a preparation method thereof.
Background
Since the availability of graphene in 2004, graphene has attracted extensive attention from the material industry due to its ultra-high thermal conductivity, and in recent years, a method for preparing a graphene thermal conductive film based on the principle of graphene through oxidation-reduction reaction and a product thereof have been developed, and the graphene thermal conductive film is used for heat dissipation of electronic products.
The thickness of the common electronic product heat conduction material artificial graphite is limited by a raw material PI film, the thickness of the common electronic product heat conduction material artificial graphite cannot exceed 100 mu m at present, along with the updating and updating of electronic products, particularly chips, the use power is gradually improved, the requirement on heat dissipation is higher and higher, a thicker heat dissipation material is needed, the thickness is increased to improve the heat flux on the premise of keeping the current heat conductivity coefficient, and a better heat equalizing effect is achieved.
Disclosure of Invention
The invention aims to provide a graphene film with a specified thickness and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a graphene film of a specified thickness, the formulation comprising: the graphene oxide dispersion liquid comprises the following components in percentage: 100% graphene oxide dispersion.
A preparation method of a graphene film with a specified thickness comprises the following steps of preparing a film; step two, preparing a preparation; step three, bonding; step four, sizing;
in the first step, a proper amount of graphene oxide dispersion liquid with specified specifications is injected into a coating machine, a forming die with a prefabricated shape is additionally arranged, the graphene oxide dispersion liquid is uniformly coated on the forming die, and the graphene oxide film is obtained after drying and curing;
in the second step, pouring a proper amount of solvent into a beaker, placing the beaker on a magnetic stirrer, slowly adding a proper amount of solute, carrying out primary stirring by using a stirring rod, carrying out secondary stirring by using a high-speed dispersion disc after the solute is completely dissolved in the solvent to completely disperse the solute in the solvent, and finally transferring the solvent into a defoaming machine to completely remove bubbles in the mixed solution to obtain the binder with the prefabricated specification;
in the third step, the graphene oxide films obtained in the first step are placed on a pressing machine according to the specified thickness, the corresponding amount of the binder obtained in the second step is injected, the graphene oxide films are uniformly coated with the binder and are stacked, and the graphene oxide films are repeatedly rolled by a rolling roller for multiple times to obtain graphene film blanks with the specified thickness;
and in the fourth step, the graphene film blank obtained in the third step is placed into a carbonization furnace for heating, and then is transferred into a graphitization furnace for heating, and the graphene film blank with the specified thickness is obtained after the furnace is cooled.
According to the technical scheme, the graphene oxide dispersion liquid is prepared by a Hummer's method, and the graphene oxide dispersion liquid has a solid content of 3-10% and a viscosity of 100000-1000000 cp.
According to the technical scheme, in the first step, the forming thickness of the graphene oxide film is 10-100 μm.
According to the technical scheme, in the second step, the solvent is any one or more of carboxymethyl cellulose, hydroxypropyl methyl cellulose ether, polyethyleneimine, ascorbic acid and chitosan.
According to the technical scheme, in the second step, the solute is any one of deionized water, ammonia water, ethanol and dimethylformamide.
According to the technical scheme, in the second step, the rotation speed of primary stirring of the magnetic stirrer is 400-800 rpm, the time of primary stirring is 0.5-3 h, the rotation speed of secondary stirring is 2000-3000 rpm, and the time of secondary stirring is 0.5-1 h.
According to the technical scheme, in the second step, the defoaming machine is a vacuum defoaming machine, and the defoaming time is 1-2 hours.
According to the technical scheme, in the second step, the mass concentration of the binder is 1-15%.
According to the technical scheme, in the third step, the rolling roller is 10-30 kg in weight, and the reciprocating rolling times are 3-5 times.
According to the technical scheme, in the third step, the corresponding amount of the binder is calculated according to the taking amount of the graphene oxide film, and the using amount is 0.1-0.3 g/cm2。
According to the technical scheme, in the fourth step, the heating temperature of the carbonization furnace is 1000 ℃.
According to the technical scheme, in the fourth step, the heating temperature of the graphitization furnace is 2800 ℃.
According to the technical scheme, in the fourth step, the graphene film material has the thickness of 20-400 mu m and the density of 2.1g/cm3The thermal conductivity was 1500W/m.K.
Compared with the prior art, the invention has the following beneficial effects: the invention utilizes the chemical bond formed between the binder and the graphene oxide molecules, the C-C bond is retained after high-temperature thermal reduction, the formed carbon chain is connected with the graphene sheet layer, the phonon heat transfer process can be carried out, compared with other modes of combining the graphene film, the loss of the heat conductivity between layers is avoided to the greatest extent, the adhesive is common industrial raw materials, has low cost, is convenient to obtain, has good affinity with graphene oxide, provides convenience for large-scale production, meanwhile, in the bonding process, other additional conditions except for the bonding agent are not needed, the operation is simple and convenient, the large-scale popularization is convenient, only a few graphene films with concentrated standard thicknesses need to be produced, and then the graphene films with any thickness need to be bonded and stacked by the method, so that the standard production is convenient, the production difficulty and cost of the coating link are reduced, and the large-scale production of the graphene films is facilitated.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution:
example 1:
a graphene film of a specified thickness, the formulation comprising: the graphene oxide dispersion liquid comprises the following components in percentage: the graphene oxide dispersion liquid is 100% and is prepared by a Hummer's method, and the solid content of the graphene oxide dispersion liquid is 3-10% and the viscosity of the graphene oxide dispersion liquid is 100000-1000000 cp.
A preparation method of a graphene film with a specified thickness comprises the following steps of preparing a film; step two, preparing a preparation; step three, bonding; step four, sizing;
in the first step, injecting a proper amount of graphene oxide dispersion liquid with solid content of 4% and viscosity of 200000cp into a coating machine, adding a forming mold with a prefabricated shape, uniformly coating the graphene oxide dispersion liquid on the forming mold, drying at 80 ℃ for 2h, and curing to obtain two graphene oxide films with the thickness of 350mm multiplied by 250mm multiplied by 20 mu m;
in the second step, 2.5g of carboxymethyl cellulose is poured into a beaker and placed on a magnetic stirrer, 97.5g of deionized water is slowly added, primary stirring is carried out by a stirring rod, the primary stirring speed of the magnetic stirrer is 500rpm, the primary stirring time is 0.5h, after the solute is completely dissolved in the solvent, secondary stirring is carried out by a high-speed dispersion disc, the secondary stirring speed is 2500rpm, the secondary stirring time is 0.5h, so that the solute is completely dispersed in the solvent, finally the solute is transferred into a defoaming machine, the defoaming machine is a vacuum defoaming machine, the defoaming time is 0.5h, bubbles in the mixed solution are thoroughly removed, and the binder with the concentration of 2.5% is obtained;
in the third step, the two graphene oxide films obtained in the first step are placed on a laminating machine, the binder obtained in the second step is injected with corresponding amount, the corresponding amount of the binder is calculated according to the using amount of the graphene oxide films, and the using amount of the binder is 0.1-0.3 g/cm2Stacking while uniformly coating the binder between two graphene oxide films, and performing 3-time reciprocating rolling by a rolling roller of 10kg to obtain a graphene film blank;
in the fourth step, a graphene film blank obtained in the third step is put into a carbonization furnace, heated to 1000 ℃, then transferred into a graphitization furnace to be heated to 2800 ℃, and cooled in the furnace to obtain a graphene film material with the density of 2.1g/cm and the thickness of 50mm multiplied by 250mm multiplied by 40 mu m3The thermal conductivity was 1500W/m.K.
Example 2:
a graphene film of a specified thickness, the formulation comprising: the graphene oxide dispersion liquid comprises the following components in percentage: the graphene oxide dispersion liquid is 100% and is prepared by a Hummer's method, and the solid content of the graphene oxide dispersion liquid is 3-10% and the viscosity of the graphene oxide dispersion liquid is 100000-1000000 cp.
A preparation method of a graphene film with a specified thickness comprises the following steps of preparing a film; step two, preparing a preparation; step three, bonding; step four, sizing;
in the first step, a proper amount of graphene oxide dispersion liquid with the solid content of 6% and the viscosity of 800000cp is injected into a coating machine, a forming die with a prefabricated shape is additionally arranged, the graphene oxide dispersion liquid is uniformly coated on the forming die, and after drying for 2 hours at the temperature of 80 ℃, the graphene oxide dispersion liquid is solidified to obtain four graphene oxide films with the thickness of 450mm multiplied by 100 mu m;
in the second step, 5g of hydroxypropyl methyl cellulose ether is poured into a beaker and placed on a magnetic stirrer, 95g of ethanol is slowly added, primary stirring is carried out by a stirring rod, the primary stirring speed of the magnetic stirrer is 750rpm, the primary stirring time is 2 hours, after the solute is completely dissolved in the solvent, secondary stirring is carried out by a high-speed dispersion disc, the secondary stirring speed is 2500rpm, the secondary stirring time is 2 hours, the solute is completely dispersed in the solvent, and finally the solvent is transferred into a defoaming machine, wherein the defoaming machine adopts a vacuum defoaming machine, the defoaming time is 1 hour, and bubbles in the mixed solution are completely removed, so that the binder with the mass concentration of 5% is obtained;
in the third step, the four graphene oxide films obtained in the first step are placed on a laminating machine, the binder obtained in the second step is injected in a corresponding amount, and the corresponding amount of the binder is calculated according to the using amount of the graphene oxide films and is 0.1-0.3 g/cm2Uniformly coating a binder among four graphene oxide films, stacking, and performing 5-time reciprocating rolling by using a rolling roller of 20kg to obtain a graphene film blank with a specified thickness;
in the fourth step, the graphene film blank obtained in the third step is placed into a carbonization furnace, heated to 1000 ℃, then transferred into a graphitization furnace to be heated to 2800 ℃, and cooled in the furnace to obtain a graphene film material with the density of 2.1g/cm and the thickness of 450mm multiplied by 400 mu m3The thermal conductivity was 1500W/m.K.
The graphene films obtained in the above embodiments are respectively subjected to a cohesion test, and a common graphene film prepared by adhesion by a hot pressing method is used as a control group for comparison, and the obtained data are as follows:
| average value of cohesion/N | |
| Example 1 | 0.7633 |
| Example 2 | 0.7633 |
| Comparative example | 0.39 |
Compared with the prior art, the invention has the following beneficial effects: the invention only needs to produce a few graphene films with concentrated standard thickness, and then the graphene films with any thickness are bonded and stacked by the method to form the graphene film with any thickness, thereby facilitating the standardized production, reducing the production difficulty and cost of the coating link, being beneficial to the large-scale production of the graphene film, forming chemical bonds between the binder and graphene oxide molecules, retaining the C-C bonds after high-temperature thermal reduction, connecting the formed carbon chains with the graphene sheet layer, the phonon heat transfer process can be carried out, compared with other modes of combining the graphene film, the loss of the heat conductivity between layers is avoided to the greatest extent, the adhesive is common industrial raw materials, has low cost, is convenient to obtain, has good affinity with graphene oxide, provides convenience for large-scale production, meanwhile, in the bonding process, other additional conditions except for the bonding agent are not needed, the operation is simple and convenient, and the wide-range popularization is facilitated.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (14)
1. A graphene film of a specified thickness, the formulation comprising: the graphene oxide dispersion liquid is characterized in that: the percentage of the components is as follows: 100% graphene oxide dispersion.
2. A preparation method of a graphene film with a specified thickness comprises the following steps of preparing a film; step two, preparing a preparation; step three, bonding; step four, sizing; the method is characterized in that:
in the first step, a proper amount of graphene oxide dispersion liquid with specified specifications is injected into a coating machine, a forming die with a prefabricated shape is additionally arranged, the graphene oxide dispersion liquid is uniformly coated on the forming die, and the graphene oxide film is obtained after drying and curing;
in the second step, pouring a proper amount of solvent into a beaker, placing the beaker on a magnetic stirrer, slowly adding a proper amount of solute, carrying out primary stirring by using a stirring rod, carrying out secondary stirring by using a high-speed dispersion disc after the solute is completely dissolved in the solvent to completely disperse the solute in the solvent, and finally transferring the solvent into a defoaming machine to completely remove bubbles in the mixed solution to obtain the binder with the prefabricated specification;
in the third step, the graphene oxide films obtained in the first step are placed on a pressing machine according to the specified thickness, the corresponding amount of the binder obtained in the second step is injected, the graphene oxide films are uniformly coated with the binder and are stacked, and the graphene oxide films are repeatedly rolled by a rolling roller for multiple times to obtain graphene film blanks with the specified thickness;
and in the fourth step, the graphene film blank obtained in the third step is placed into a carbonization furnace for heating, and then is transferred into a graphitization furnace for heating, and the graphene film blank with the specified thickness is obtained after the furnace is cooled.
3. The graphene film material of claim 1, wherein: the graphene oxide dispersion liquid is prepared by a Hummer's method, and the solid content of the graphene oxide dispersion liquid is 3-10% and the viscosity of the graphene oxide dispersion liquid is 100000-1000000 cp.
4. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the first step, the forming thickness of the graphene oxide film is 10-100 μm.
5. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the second step, the solvent is any one or more of carboxymethyl cellulose, hydroxypropyl methyl cellulose ether, polyethyleneimine, ascorbic acid and chitosan.
6. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the second step, the solute is any one of deionized water, ammonia water, ethanol and dimethylformamide.
7. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the second step, the rotation speed of the primary stirring of the magnetic stirrer is 400-800 rpm, the time of the primary stirring is 0.5-3 h, the rotation speed of the secondary stirring is 2000-3000 rpm, and the time of the secondary stirring is 0.5-1 h.
8. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the second step, the defoaming machine is a vacuum defoaming machine, and the defoaming time is 1-2 h.
9. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the second step, the mass concentration of the binder is 1-15%.
10. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the third step, the rolling roller is 10-30 kg in weight, and the reciprocating rolling times are 3-5 times.
11. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the third step, the corresponding amount of the binder is calculated according to the use amount of the graphene oxide film, and the use amount is 0.1-0.3 g/cm2。
12. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the fourth step, the heating temperature of the carbonization furnace is 1000 ℃.
13. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the fourth step, the heating temperature of the graphitization furnace is 2800 ℃.
14. The method for preparing the graphene film with the specified thickness according to claim 2, wherein: in the fourth step, the graphene film material has a thickness of 20-400 μm and a density of 2.1g/cm3The thermal conductivity was 1500W/m.K.
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