CN113999445B - Graphene/polyethylene composite material and preparation method thereof - Google Patents
Graphene/polyethylene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene/polyethylene composite material and a preparation method thereof, wherein the preparation method comprises the following steps: preparing positively charged coated graphene P-GNPs; preparing negative charge coated polyethylene N-PE; ultrasonically dispersing the P-GNPs and the N-PE into absolute ethyl alcohol, stirring, uniformly adsorbing the P-GNPs on the outer surface of the N-PE particles, vacuum-filtering, and collecting the P-GNPs@N-PE microspheres; and placing the P-GNPs@N-PE microspheres in a die, performing hot pressing treatment, and performing cold pressing treatment to obtain the graphene/polyethylene composite material. According to the preparation method, the graphene/polyethylene composite material with the double-isolation structure and the honeycomb graphene frame can be prepared by a simple, safe and controllable process, and the thermal conductivity of the composite material is improved by adjusting the content of P-GNPs.
Description
Technical Field
The invention relates to a graphene/polyethylene composite material and a preparation method thereof, and belongs to the technical field of functional materials.
Background
Graphene is a common high-thermal-conductivity nano filler for preparing high-performance polymer composite materials, and is a flaky two-dimensional material with a honeycomb lattice. Because the heat conduction performance is extremely excellent (3000-5000W/(m.K)), the graphene is known as the optimal filler for improving the heat conduction performance of the polymer. However, if the thermal conductivity of the composite material is to be greatly improved, the key problem to be solved is to achieve uniform dispersion of graphene in the polymer matrix. However, the graphene agglomeration effect is very severe due to the strong pi-pi interactions between the sheets. In addition, the compatibility of the graphene and the polymer matrix is poor, a large number of gaps and defects exist at the interface, so that extra phonon scattering is caused, and the thermal conductivity of the composite material is restricted by the greatly increased interface thermal resistance.
Constructing a three-dimensional (3D) graphene framework in a polymer matrix is an effective solution to solve the problem of graphene agglomeration. Various self-assembly techniques are widely used to construct 3D graphene frames, such as by hydrothermal reaction or sol-gel, followed by lyophilization. In addition, graphene is grown on a metal catalyst (copper, gold or nickel foam) by chemical vapor deposition, and then a 3D graphene frame can be obtained by etching a metal template.
Heretofore, a variety of 3D graphene frameworks have been introduced into polymer matrices to obtain high performance composites. For example, chinese patent CN102786705a discloses a method for preparing graphene/polyaniline composite material based on layer-by-layer self-assembly technology, wherein polyaniline and graphene are used as structural units, and the layer-by-layer self-assembly technology is adopted to construct graphene-polyaniline composite material with ordered structure; chinese patent CN106185885a discloses a three-dimensional graphene sponge body and carbon nanotube composite material with isotropy, high heat conductivity and elasticity and a preparation method, wherein graphene oxide is subjected to hydrothermal reaction to form a three-dimensional porous morphology, and then carbon nanotubes are grown in the internal gaps of the graphene sponge body by chemical vapor deposition. However, most of the above schemes are to prefabricate the 3D graphene frame first and then compound the polymer matrix, which results in complex preparation process, time consuming and difficult mass production, and cannot meet the practical application.
Accordingly, there is a strong need for those skilled in the art to find a simple solution for preparing high thermal conductivity graphene/polymer composites.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a graphene/polyethylene composite material and a preparation method thereof, wherein the graphene/polyethylene composite material with a honeycomb graphene frame is prepared through a simple process so as to improve the heat conductivity.
In order to achieve the above purpose, in one aspect, the present invention provides a preparation method of a graphene/polyethylene composite material, comprising the following steps:
preparing positively charged coated graphene P-GNPs;
preparing negative charge coated polyethylene N-PE;
ultrasonically dispersing the P-GNPs and the N-PE into absolute ethyl alcohol, stirring, uniformly adsorbing the P-GNPs on the outer surface of the N-PE particles, vacuum-filtering, and collecting the P-GNPs@N-PE microspheres;
and (3) placing the P-GNPs@N-PE microspheres in a stainless steel mold, performing hot pressing treatment, and performing pressure treatment again to obtain the graphene/polyethylene composite material.
Further, the preparation of the positively charged coated graphene P-GNPs comprises the following steps:
dispersing graphene nano-sheets in a tetramethyl ammonium hydroxide aqueous solution in an ultrasonic manner, dropwise adding a polydiallyl dimethyl ammonium chloride aqueous solution, and continuously stirring for 6-18 hours;
centrifuging the stirred solution;
washing the centrifuged precipitate with absolute ethyl alcohol for several times to obtain the polydiallyl dimethyl ammonium chloride positively charged coated graphene nanoplatelets P-GNPs.
Further, the centrifugal treatment results in a rotational speed of 1000rpm to 4000rpm.
Further, in the step of preparing the positively charged coated graphene P-GNPs:
the mass volume ratio of the graphene nano-sheet to the tetramethylammonium hydroxide aqueous solution is 1 (300-600), and the unit is g/mL;
the molar concentration of the tetramethylammonium hydroxide aqueous solution is 0.05-0.15mol/L.
Further, in the step of preparing the positively charged coated graphene P-GNPs: the volume ratio of the tetramethyl ammonium hydroxide aqueous solution to the polydiallyl dimethyl ammonium chloride aqueous solution is (20-40): 1
Further, in the step of preparing the positively charged coated graphene P-GNPs: the mass fraction of the polydiallyl dimethyl ammonium chloride aqueous solution is 10-20wt%.
Further, the preparation of the negatively charged coated polyethylene N-PE comprises the following steps:
ultrasonically dispersing polyethylene powder into a sodium polystyrene sulfonate aqueous solution, and stirring;
centrifuging the stirred mixture;
washing the centrifuged precipitate with absolute ethyl alcohol for several times to obtain polyethylene powder N-PE coated with negative charges of sodium polystyrene sulfonate.
Further, in the step of preparing the negatively charged coated polyethylene N-PE:
the stirring speed is 300-600rpm;
the stirring time is 12-18h.
Further, in the step of preparing the negatively charged coated polyethylene N-PE:
the rotational speed of the centrifugal treatment is 1000-2000rpm. Further, the method is characterized in that in the step of preparing the negative charge coated polyethylene N-PE:
the mass volume ratio of the polyethylene powder to the polystyrene sodium sulfonate aqueous solution is 1 (100-400), and the unit is g/mL;
the mass fraction of the sodium polystyrene sulfonate aqueous solution is 0.5-1.5wt%.
Further, the mass ratio of the P-GNPs to the N-PE is (1-4): (16-19).
Further, the mass ratio of the P-GNPs to the N-PE is 1:4.
further, the pressure of the hot pressing and the cold pressing is 10-20 MPa; the hot pressing temperature is set to 130-140 ℃ and the hot pressing time is 5-20 min; the cold pressing temperature is room temperature, and the cold pressing time is 5-20 min.
Further, the stirring speed is 300-600rpm; the stirring time is 6-18 h.
On the other hand, the invention provides a graphene/polyethylene composite material, which is prepared by adopting the preparation method of the graphene/polyethylene composite material.
Compared with the prior art, the invention has the beneficial effects that:
the invention makes the P-GNPs uniformly adsorbed on the outer surface of the N-PE particles by utilizing the electrostatic induction effect to form P-GNPs@N-PE microspheres; P-GNPs@N-PE microspheres are subjected to hot pressing treatment at a melting temperature, so that the P-GNPs are selectively distributed at the deformed hybrid microsphere interface, a three-dimensional continuous honeycomb graphene heat conduction frame is constructed, and heat conduction phonons are transmitted along a highway formed by the three-dimensional graphene frame to promote rapid heat transfer, so that the heat conduction performance of the graphene/polyethylene composite material is greatly improved.
According to the preparation method, the graphene/polyethylene composite material is prepared through simple process steps, the polyethylene and the polyethylene are isolated through the graphene, the graphene is in a honeycomb shape and is wrapped on the periphery of the polyethylene, and the graphene/polyethylene composite material with a double-isolation structure and a honeycomb-shaped graphene frame and a polyethylene matrix is formed, so that heat can be conducted at a high speed along the honeycomb-shaped continuous graphene frame, and the polyethylene matrix provides mechanical properties. The preparation process is environment-friendly, safe and controllable in preparation process operation, and suitable for large-scale application. Drawings
FIG. 1 is a flow chart of one embodiment of a method of preparing a graphene/polyethylene composite material of the present invention;
FIG. 2 is a SEM scan cross-sectional view of one embodiment of a graphene/polyethylene composite material of the present invention;
FIG. 3 is a graph showing the thermal conductivity of an embodiment of the graphene/polyethylene composite material of the present invention;
fig. 4 is a schematic structural diagram of an embodiment of a graphene/polyethylene composite material dual-isolation structure according to the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
Example 1
Preparing positively charged coated graphene P-GNPs:
referring to FIG. 1, 0.5g of graphene nanoplatelets are weighed and ultrasonically dispersed in 150mL of 0.05mol/L aqueous tetramethylammonium hydroxide solution; then, 7.5 mL of 10wt% polydiallyl dimethyl ammonium chloride aqueous solution is slowly added dropwise into the solution and stirred continuously for 6 hours; then centrifuging the stirred mixture at 1000 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the graphene P-GNPs coated with positive charges.
Preparation of negatively charged coated polyethylene N-PE:
referring to fig. 1, 1.5g of polyethylene powder was weighed and ultrasonically dispersed in 200 ml of 0.5wt% aqueous sodium polystyrene sulfonate solution; then stirring the solution at 300 rpm for 18 hours; then centrifuging the stirred solution at 2000 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the polyethylene N-PE coated with negative charges.
Preparing a graphene/polyethylene composite material:
referring to FIG. 1, P-GNPs and N-PE are respectively weighed according to a mass ratio of 1:4, and are ultrasonically dispersed in absolute ethyl alcohol; then stirring the solution 18 at 300 rpm for h, wherein the positively charged coated graphene P-GNPs are uniformly adsorbed on the outer surface of the negatively charged coated polyethylene N-PE due to strong electrostatic interaction; and then collecting the P-GNPs@N-PE microspheres by vacuum filtration.
Weighing 4 gP-GNPs@N-PE microspheres, placing the microspheres in a stainless steel mold with the pressure of 15MPa, hot-pressing the microspheres at 130 ℃ for 20min, and cold-pressing the microspheres at room temperature for 20min to obtain the graphene/polyethylene composite material.
As shown in fig. 4, in the graphene/polyethylene composite material prepared in this embodiment, the polyethylene is isolated from the polyethylene by the graphene, and the graphene is honeycomb-shaped and wraps the periphery of the polyethylene, so as to form a graphene/polyethylene composite material with a double-isolation structure, wherein the polyethylene matrix is used for providing mechanical properties, and the graphene frame is used for conducting heat at a high speed.
Example 2
Preparing positively charged coated graphene P-GNPs:
referring to FIG. 1, 0.5g of graphene nanoplatelets are weighed and ultrasonically dispersed in 200 mL of 0.1mol/L aqueous tetramethylammonium hydroxide solution; then 5 mL 15wt% polydiallyl dimethyl ammonium chloride aqueous solution is slowly added dropwise to the solution and stirring is continued for 12h; then centrifuging the stirred mixture at 3000 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the graphene GNPs coated with positive charges.
Preparation of negatively charged coated polyethylene N-PE:
referring to FIG. 1, 1.5g of polyethylene powder was weighed and ultrasonically dispersed in 200 mL of a 1wt% aqueous solution of sodium polystyrene sulfonate; then stirring the solution at 400 rpm for 12 hours; then centrifuging the stirred solution at 1000 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the polyethylene N-PE coated with negative charges.
Preparing a graphene/polyethylene composite material:
referring to FIG. 1, P-GNPs and N-PE are respectively weighed according to the mass ratio of 3:17, and are ultrasonically dispersed in absolute ethyl alcohol; then stirring the solution 6h at 400 rpm, wherein the positively charged coated graphene P-GNPs are uniformly adsorbed on the outer surface of the negatively charged coated polyethylene N-PE due to strong electrostatic interaction; and then collecting the P-GNPs@N-PE microspheres by vacuum filtration.
Weighing 4 gP-GNPs@N-PE microspheres, placing the microspheres in a stainless steel mold with the pressure of 10 MPa, hot-pressing the microspheres at 135 ℃ for 10 min, and cold-pressing the microspheres at room temperature for 10 min to obtain the graphene/polyethylene composite material.
As shown in fig. 4, in the graphene/polyethylene composite material prepared in this embodiment, the polyethylene is isolated from the polyethylene by the graphene, and the graphene is honeycomb-shaped and wraps the periphery of the polyethylene, so as to form a graphene/polyethylene composite material with a double-isolation structure, wherein the polyethylene matrix is used for providing mechanical properties, and the graphene frame is used for conducting heat at a high speed.
Example 3
Preparing positively charged coated graphene P-GNPs:
referring to FIG. 1, 0.5g of graphene nanoplatelets are weighed and ultrasonically dispersed in 200 mL of 0.1mol/L aqueous tetramethylammonium hydroxide solution; then 5 mL 15wt% polydiallyl dimethyl ammonium chloride aqueous solution is slowly added dropwise to the solution and stirring is continued for 15h; then centrifuging the stirred mixture at 2500 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the graphene GNPs coated with positive charges.
Preparation of negatively charged coated polyethylene N-PE:
referring to FIG. 1, 1.5g of polyethylene powder was weighed and ultrasonically dispersed in 200 mL of 1.5wt% aqueous sodium polystyrene sulfonate solution; then stirring the solution at 500rpm for 15 hours; then centrifuging the stirred solution at 1500 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the polyethylene N-PE coated with negative charges.
Preparing a graphene/polyethylene composite material:
referring to fig. 1, according to 1:9, respectively weighing P-GNPs and N-PE according to the mass ratio, and dispersing the P-GNPs and the N-PE in absolute ethyl alcohol by ultrasonic; stirring the solution for 10 hours at 500rpm, wherein the positively charged coated graphene P-GNPs are uniformly adsorbed on the outer surface of the negatively charged coated polyethylene N-PE due to strong electrostatic interaction; and then collecting the P-GNPs@N-PE microspheres by vacuum filtration.
Weighing 4 gP-GNPs@N-PE microspheres, placing the microspheres in a stainless steel mold with the pressure of 15MPa, hot-pressing the microspheres at 135 ℃ for 15min, and cold-pressing the microspheres at room temperature for 15min to obtain the graphene/polyethylene composite material.
As shown in fig. 4, in the graphene/polyethylene composite material prepared in this embodiment, the polyethylene is isolated from the polyethylene by the graphene, and the graphene is honeycomb-shaped and wraps the periphery of the polyethylene, so as to form a graphene/polyethylene composite material with a double-isolation structure, wherein the polyethylene matrix is used for providing mechanical properties, and the graphene frame is used for conducting heat at a high speed.
Example 4
Preparing positively charged coated graphene P-GNPs:
referring to FIG. 1, 0.5g of graphene nanoplatelets are weighed and dispersed ultrasonically in 300 mL of 0.15mol/L aqueous tetramethylammonium hydroxide solution; then, 7.5 mL of 20wt% polydiallyl dimethyl ammonium chloride aqueous solution is slowly added dropwise to the solution and stirring is continued for 18h; then centrifuging the stirred mixture at 4000 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the graphene GNPs coated with positive charges.
Preparation of negatively charged coated polyethylene N-PE:
referring to FIG. 1, 1.5g of polyethylene powder was weighed and ultrasonically dispersed in 200 mL of 1.5wt% aqueous sodium polystyrene sulfonate solution; then stirring the solution at 600rpm for 18 hours; then centrifuging the stirred solution at 2000 rpm; and finally washing the precipitate obtained after centrifugation with absolute ethyl alcohol for a plurality of times to obtain the polyethylene N-PE coated with negative charges.
Preparing a graphene/polyethylene composite material:
referring to FIG. 1, P-GNPs and N-PE are respectively weighed according to the mass ratio of 1:19, and are ultrasonically dispersed in absolute ethyl alcohol; stirring the solution at 600rpm for 10 hours, wherein the positively charged coated graphene P-GNPs are uniformly adsorbed on the outer surface of the negatively charged coated polyethylene N-PE due to strong electrostatic interaction; and then collecting the P-GNPs@N-PE microspheres by vacuum filtration.
Weighing 4 gP-GNPs@N-PE microspheres, placing the microspheres in a stainless steel mold with the pressure of 20 MPa, hot-pressing the microspheres at 140 ℃ for 5min, and cold-pressing the microspheres at room temperature for 5min to obtain the graphene/polyethylene composite material.
As shown in fig. 4, in the graphene/polyethylene composite material prepared in this embodiment, the polyethylene is isolated from the polyethylene by the graphene, and the graphene is honeycomb-shaped and wraps the periphery of the polyethylene, so as to form a graphene/polyethylene composite material with a double-isolation structure, wherein the polyethylene matrix is used for providing mechanical properties, and the graphene frame is used for conducting heat at a high speed.
Experiments show that referring to fig. 2, the section of the pure polyethylene powder is shown in the diagram (a), and the whole section is smooth and uniform as no particles are doped; in the figure, (b) shows the cross section of the graphene/polyethylene composite material in example 1, since the polyethylene is subjected to flow deformation near the melting temperature, the P-GNPs are caused to be selectively distributed at the interface of the P-GNPs@N-PE microspheres, so that a three-dimensional continuous honeycomb graphene heat conduction frame is constructed, the cross section is relatively coarse, and the overall appearance similar to a honeycomb network is shown.
It is known from experiments that referring to fig. 3, the thermal conductivity of the graphene/polyethylene composite material shows a monotonically increasing trend with the increase of the P-GNPs filling amount: the thermal conductivity of the pure polyethylene matrix is only 0.44W/(mK); in example 4, when graphene and polyethylene are compounded and the mass fraction of P-GNPs is 5%, the thermal conductivity of the graphene/polyethylene composite is 0.7W/(m·k); in example 3, when graphene and polyethylene are compounded and the mass fraction of P-GNPs is 10%, the thermal conductivity of the graphene/polyethylene composite is 1.2W/(m·k); in example 2, when graphene and polyethylene are compounded and the mass fraction of P-GNPs is 15%, the thermal conductivity of the graphene/polyethylene composite is 1.85W/(m·k); in example 1, when graphene and polyethylene are compounded, and the mass fraction of P-GNPs is 20%, the thermal conductivity of the graphene/polyethylene composite material is as high as 2.51W/(m.K), and 470% is improved compared with pure polyethylene. In summary, the content of the positively charged coated graphene P-GNPs is a key factor affecting the heat conducting property of the graphene/polyethylene composite material.
In summary, according to the embodiment of the invention, the graphene nanosheets and the polyethylene powder are modified by utilizing the cationic electrolyte and the anionic electrolyte respectively to prepare graphene P-GNPs coated with positive charges and polyethylene N-PE coated with negative charges; the invention makes the P-GNPs uniformly adsorbed on the outer surface of the N-PE particles by utilizing strong electrostatic interaction to form P-GNPs@N-PE microspheres; according to the invention, the graphene/polyethylene composite material is obtained through hot pressing treatment and cold pressing treatment successively.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and variations could be made by those skilled in the art without departing from the technical principles of the present invention, and such modifications and variations should also be regarded as being within the scope of the invention.
Claims (13)
1. The preparation method of the graphene/polyethylene composite material is characterized by comprising the following steps of:
preparing positively charged coated graphene P-GNPs;
preparing negative charge coated polyethylene N-PE;
ultrasonically dispersing the P-GNPs and the N-PE into absolute ethyl alcohol, stirring, uniformly adsorbing the P-GNPs on the outer surface of the N-PE particles, vacuum-filtering, and collecting the P-GNPs@N-PE microspheres;
placing the P-GNPs@N-PE microspheres in a mold, performing hot pressing treatment, and performing secondary pressing treatment to obtain a graphene/polyethylene composite material;
the preparation method of the positively charged coated graphene P-GNPs comprises the following steps:
dispersing graphene nano-sheets in a tetramethyl ammonium hydroxide aqueous solution in an ultrasonic manner, dropwise adding a polydiallyl dimethyl ammonium chloride aqueous solution, and continuously stirring for 6-18 hours;
centrifuging the stirred solution;
washing the centrifuged precipitate with absolute ethyl alcohol for several times to obtain graphene nanoplatelets P-GNPs coated with polydiallyl dimethyl ammonium chloride positive charges;
the preparation of the negatively charged coated polyethylene N-PE comprises the following steps:
ultrasonically dispersing polyethylene powder into a sodium polystyrene sulfonate aqueous solution, and stirring;
centrifuging the stirred mixture;
washing the centrifuged precipitate with absolute ethyl alcohol for several times to obtain polyethylene powder N-PE coated with negative charges of sodium polystyrene sulfonate.
2. The method for preparing a graphene/polyethylene composite material according to claim 1, wherein the rotational speed of the centrifugal treatment is 1000rpm to 4000rpm.
3. The method for preparing graphene/polyethylene composite material according to claim 1, wherein in the step of preparing positive charge coated graphene P-GNPs:
the mass volume ratio of the graphene nano-sheets to the tetramethyl ammonium hydroxide aqueous solution is 1 (300-600), and the mass volume unit is g/mL;
the molar concentration of the tetramethylammonium hydroxide aqueous solution is 0.05-0.15mol/L.
4. The method for preparing graphene/polyethylene composite material according to claim 1, wherein in the step of preparing positive charge coated graphene P-GNPs: the volume ratio of the tetramethyl ammonium hydroxide aqueous solution to the polydiallyl dimethyl ammonium chloride aqueous solution is (20-40): 1.
5. the method for preparing graphene/polyethylene composite material according to claim 1, wherein in the step of preparing positive charge coated graphene P-GNPs: the mass fraction of the polydiallyl dimethyl ammonium chloride aqueous solution is 10-20wt%.
6. The method of preparing a graphene/polyethylene composite material according to claim 1, wherein in the step of preparing a negatively charged coated polyethylene N-PE:
the stirring speed is 300-600rpm;
the stirring time is 12-18h.
7. The method of preparing a graphene/polyethylene composite material according to claim 6, wherein in the step of preparing a negatively charged coated polyethylene N-PE:
the rotational speed of the centrifugal treatment is 1000-2000rpm.
8. The method of preparing a graphene/polyethylene composite material according to claim 1, wherein in the step of preparing a negatively charged coated polyethylene N-PE:
the mass volume ratio of the polyethylene powder to the polystyrene sodium sulfonate aqueous solution is 1 (100-400), and the mass volume unit is g/mL;
the mass fraction of the sodium polystyrene sulfonate aqueous solution is 0.5-1.5wt%.
9. The preparation method of the graphene/polyethylene composite material according to claim 1, wherein the mass ratio of the P-GNPs to the N-PE is (1-4): (16-19).
10. The preparation method of the graphene/polyethylene composite material according to claim 1 or 9, wherein the mass ratio of the P-GNPs to the N-PE is 1:4.
11. the method for preparing a graphene/polyethylene composite material according to claim 1, wherein the hot and cold pressing pressures are 10 to 20 MPa; the hot pressing temperature is set to 130-140 ℃ and the hot pressing time is 5-20 min; the cold pressing temperature is room temperature, and the cold pressing time is 5-20 min.
12. The method for preparing a graphene/polyethylene composite material according to claim 1, wherein in the step of ultrasonically dispersing P-GNPs and N-PE in absolute ethanol and stirring:
the stirring speed is 300-600rpm; the stirring time is 6-18 h.
13. A graphene/polyethylene composite material, characterized in that it is prepared by the preparation method of the graphene/polyethylene composite material according to any one of claims 1 to 12.
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| CN107236165B (en) * | 2017-07-13 | 2019-02-26 | 上海通茗检测技术服务有限公司 | A kind of rubber/graphene composite material preparation method with isolation structure |
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