CN110777411A - Preparation method of graphene paper-metal composite material - Google Patents
Preparation method of graphene paper-metal composite material Download PDFInfo
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- CN110777411A CN110777411A CN201911109000.4A CN201911109000A CN110777411A CN 110777411 A CN110777411 A CN 110777411A CN 201911109000 A CN201911109000 A CN 201911109000A CN 110777411 A CN110777411 A CN 110777411A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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Abstract
The application discloses a preparation method of a graphene paper-metal composite material, wherein graphene paper is tightly attached to a cathode, the cathode and an anode are immersed in electrolyte, the anode is connected with a power supply anode, and the cathode is connected with a power supply cathode. The metal is adopted in the anode, when the power supply is turned on, the metal in the anode can be electrolyzed to generate metal ions to enter the electrolyte, and a metal coating can be generated on the graphene paper of the cathode, so that the graphene paper and the metal can be compounded.
Description
Technical Field
The application relates to the technical field of graphene-based composite materials, in particular to a preparation method of a graphene paper-metal composite material.
Background
Graphene is currently the thinnest material known in the world and possesses many extremely excellent physical properties, such as: high light transmittance, high thermal conductivity, high electron mobility, low resistivity, hall effect at room temperature, and the like. In the prior art, when multiple layers of graphene are superposed, an agglomeration phenomenon occurs, and a thicker material with low performance cannot be obtained. However, the single-layer/few-layer graphene must be used with the substrate because of its thinness, and the thickness difference between the substrate and the graphene film is very large, so that the thermal deposition and heat dissipation performance of the film are mainly related to the substrate, and it is difficult to effectively improve the thermal deposition and heat dissipation performance. The graphene oxide is a product of graphene after oxidation, and can be prepared into a thicker micron-sized film structure. The reduced graphene oxide is reduced on the basis of graphene oxide, has stable performance and can be applied as a thermal management material. With the development of the preparation technology, the thermal conductivity coefficient of the reduced graphene oxide exceeds that of non-metallic materials such as diamond and GPI films at present, and the reduced graphene oxide has better flexibility. However, the graphene paper has a small thickness, usually less than 100um, due to the limitations of the current process, and therefore, it has low strength, poor impact resistance and limitations in industrial application. On the basis of keeping the excellent thermal conductivity of the original graphene paper, the graphene paper-metal composite material enhances the mechanical properties such as strength, wear resistance and the like, so that the graphene paper-metal composite material has higher practicability.
At present, there are many methods for preparing graphene/graphene paper-metal composite materials, most of which are vapor deposition methods or physical combination methods, such as: the chemical vapor deposition is to take hydrocarbon as a carbon source, simultaneously load pre-plated metal in a quartz boat, put the quartz boat in a reaction chamber, heat the quartz boat to a certain temperature under a protective atmosphere, grow graphene on a metal substrate, and simultaneously deposit the pre-plated metal on the surface of the graphene to form loaded metal graphene. Has higher requirements on raw materials, products and reaction types, and has expensive preparation cost. The thermal evaporation method is to evaporate the evaporated metal in a vacuum chamber by heating and then deposit the evaporated metal on a Si or SiO2 substrate containing graphene, wherein the required environmental condition is vacuum and the experimental condition is high. The hydrothermal method is a synthetic method in which an original mixture is subjected to a chemical reaction in an autoclave at a certain temperature and a certain autogenous pressure of a solution with an aqueous solution as a reaction medium. The hydrothermal reaction process is invisible, the high-pressure kettle has good sealing property and high temperature and high pressure. The methods are complex in preparation process, high in energy consumption, long in time consumption and difficult to industrialize.
Disclosure of Invention
In view of the above-mentioned drawbacks or disadvantages of the prior art, it is desirable to provide a method for preparing a graphene paper-metal composite.
The invention provides a preparation method of a graphene paper-metal composite material, which is characterized by comprising the following steps: preparing electrolyte, and preparing a cathode and an anode, wherein the anode is made of metal, and the cathode is made of metal or other conductive materials; tightly attaching graphene paper to the cathode; immersing both the cathode and the anode in an electrolyte; the anode is connected with the positive pole of the power supply, the cathode is connected with the negative pole of the power supply, and the power supply is started.
Further, the method further comprises the step of covering an insulating film on the graphene paper before the power supply is turned on.
Further, the method also comprises the step of uniformly arranging a plurality of holes on the graphene paper along the contour direction of the graphene paper before the graphene paper is tightly attached to the cathode.
Further, the graphene paper is circular, the holes are formed along the circumference, and the distance between any two adjacent holes in the radial direction and the axial direction is 1 mm.
Further, the method comprises the steps of cleaning the graphene paper after holes are formed in the graphene paper and drying the graphene paper, wherein absolute ethyl alcohol ultrasonic waves are adopted for cleaning the graphene paper.
Further, the method further comprises the step of cleaning the graphene paper and drying the graphene paper before the graphene paper is tightly attached to the cathode, wherein absolute ethyl alcohol ultrasonic waves are adopted for cleaning the graphene paper.
Further, the method further comprises the step of heating the electrolyte in a water bath before turning on the power supply, wherein the heating temperature is 20-100 ℃, and the time for turning on the power supply is after the water temperature is constant.
Further, the electrolyte comprises the following components in percentage by weight: 1-15% of glycerol, 1-15% of triethanolamine, 0.5-6% of tetramethylammonium chloride, 0-2% of acetone and the balance of methanol.
Further, the anode adopts a copper sheet, and the cathode adopts metal or other conductive materials.
Further, the setting current of the power supply is 0.02A-0.5A.
Compared with the prior art, the invention has the following advantages: according to the invention, the graphene paper is tightly attached to the cathode, the cathode and the anode are immersed in the electrolyte, the anode is connected with the anode of the power supply, the cathode is connected with the cathode of the power supply, metal ions generated by electrolysis of metal of the anode enter the electrolyte when the power supply is turned on, and a metal coating is generated on the graphene paper of the cathode, so that the graphene paper and the metal are compounded, the preparation process is simple, the time consumption is short, the energy consumption is low, the coating thickness is easy to control, and the industrialization can be realized.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings in which:
fig. 1 is a flowchart of a method for preparing a graphene paper-metal composite according to an embodiment of the present invention;
fig. 2 is a diagram of a graphene paper-metal composite material formed by graphene paper not covered with an insulating film according to an embodiment of the present invention;
fig. 3 is a diagram of a graphene paper-metal composite material formed by covering an insulating film with graphene paper according to an embodiment of the present invention.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
As mentioned in the background, there are currently more graphene/graphene paper-metal composite preparation methods, most of which are vapor deposition methods or physically combined methods, such as: the chemical vapor deposition is to take hydrocarbon as a carbon source, simultaneously load pre-plated metal in a quartz boat, put the quartz boat in a reaction chamber, heat the quartz boat to a certain temperature under a protective atmosphere, grow graphene on a metal substrate, and simultaneously deposit the pre-plated metal on the surface of the graphene to form loaded metal graphene. Has higher requirements on raw materials, products and reaction types, and has expensive preparation cost. The thermal evaporation method is to evaporate the evaporated metal in a vacuum chamber by heating and then deposit the evaporated metal on a Si or SiO2 substrate containing graphene, wherein the required environmental condition is vacuum and the experimental condition is high. The hydrothermal method is a synthetic method in which an original mixture is subjected to a chemical reaction in an autoclave at a certain temperature and a certain autogenous pressure of a solution with an aqueous solution as a reaction medium. The hydrothermal reaction process is invisible, the high-pressure kettle has good sealing property and high temperature and high pressure. The methods are complex in preparation process, high in energy consumption, long in time consumption and difficult to industrialize.
Therefore, the embodiment of the present application provides a method for preparing a graphene paper-metal composite material, which reduces energy consumption and is frequent in preparing the graphene paper-metal composite material, simplifies a preparation process, enables industrialization of the graphene paper-metal composite material, and is an improvement direction of an existing preparation method.
Referring to fig. 1, a flow chart of a method for preparing a graphene paper-metal composite according to an embodiment of the present application is shown.
In step 110, preparing an electrolyte, and preparing a cathode and an anode, wherein the anode is made of metal, and the cathode is made of metal or other conductive materials;
in step 120, tightly attaching graphene paper to the cathode;
in step 130, immersing both the cathode and the anode in an electrolyte;
in step 140, the anode is connected to the positive pole of the power supply, the cathode is connected to the negative pole of the power supply, and the power supply is turned on.
In step 110, the electrolyte comprises the following components in percentage by weight: 1-15% of glycerol, 1-15% of triethanolamine, 0.5-6% of tetramethylammonium chloride, 0-2% of acetone and the balance of methanol. The anode preferably adopts a copper sheet, and other metals can also be adopted; the cathode is made of metal or other conductive materials, and is not further limited herein. The positions of the cathode and the anode in the electrolyte are not particularly limited, and the anode and the cathode may be arranged in the electrolyte up and down, or left and right.
Before the graphene paper is closely attached to the cathode in step 120, the method further includes uniformly forming a plurality of holes on the graphene paper along the contour direction thereof. The method aims to change the surface roughness of the graphene paper and strengthen the binding capacity. Further, the graphene paper may be circular, and preferably, the holes are arranged along the circumference, and the distance between any two adjacent holes in the radial direction and the axial direction is 1 mm.
Before the graphene paper is tightly attached to the cathode in step 120, the method further includes cleaning the graphene paper and drying, wherein absolute ethyl alcohol ultrasonic waves are adopted for cleaning the graphene paper. If holes are formed in the graphene paper, the steps of cleaning and drying the graphene paper need to be performed after the holes are formed in the graphene paper.
Before the power supply is turned on in step 140, the method further includes covering an insulating film on the graphene paper. If the insulating film is not covered, the metal coating is uniformly covered on the whole graphene paper, if the graphene paper is covered by the insulating film, the coating cannot be generated at the covering position, so that the graphene paper only has the metal coating around the insulating film, and the purpose of controlling the growth of the coating is achieved. Optionally, the insulating film is circular, and the metal plating layer on the graphene paper is concentric.
Before the power supply is turned on in step 140, the method further comprises the step of heating the electrolyte in a water bath, wherein the heating temperature is 20-100 ℃, and the set current of the power supply is 0.02-0.5A after the time of turning on the power supply is constant. In order to ensure that the current of the electrolyte is constant, the resistance is not too large, the electrolyte is prevented from being evaporated too fast, the electrolyte can be properly added in the experiment for keeping the electrolyte sufficient, whether the voltage and the current are normal or not is checked, and the power supply is turned off after a period of time.
When the power supply is turned on, metal on the anode can be electrolyzed to generate metal ions to enter the electrolyte, and a metal coating can be generated on the graphene paper on the cathode, so that the graphene paper and the metal can be compounded. After a period of time, the power supply is turned off, the cathode is taken out of the electrolytic cell, the wafer shown in fig. 2 and 3 is the deposited graphene paper-metal composite material, the metal coating is compact, the graphene and the metal coating are tightly combined, the thickness of the metal coating can be determined according to the electrodeposition time, and the control of the growth area can be realized. The preparation process is simple, the time consumption is short, the energy consumption is low, the thickness of the coating is easy to control, and the industrialization can be realized.
For further understanding of the present invention, the following provides a detailed description of the method for preparing the graphene paper-metal composite material, and the scope of the present invention is not limited by the following examples.
Example 1
And preparing an electrolyte. A1000 ml beaker was taken and about 800ml of organic electrolyte was added. And manufacturing a cathode and an anode.
And cleaning the graphene paper. And removing dust and oil on the graphene paper. Grinding a plurality of pieces of graphene paper with the size of 20mm multiplied by 20mm, ultrasonically cleaning the graphene paper with absolute ethyl alcohol twice, and drying the graphene paper for later use.
Attaching graphene paper on the cathode to ensure that the graphene paper is in close contact with the cathode, and immersing the cathode and the anode into a beaker filled with electrolyte.
Preparing two 15cm long insulated copper wires and a power supply, setting the current of the power supply to be 0.02-0.5A, connecting the anode with the anode of the power supply and connecting the cathode with the cathode of the power supply, and additionally arranging a water bath heating device outside the beaker, wherein the water bath heating device is provided with a cup cover to reduce the evaporation of the electrolyte. The temperature of the heating table is set to be 15-100 ℃, heating is carried out firstly, the water temperature is constant, and then a constant current source power supply is started.
After the electrodeposition is started, in order to ensure that the current of the electrolyte is constant, the resistance is not too large, the electrolyte is prevented from being evaporated too fast, the electrolyte is kept sufficient in the experiment, the electrolyte can be properly added, whether the voltage and the current are normal or not is checked, and the power supply is turned off after a period of time.
And taking the cathode out of the electrolytic cell, drying, and generating and uniformly covering a copper coating on the cathode graphene paper, wherein the thickness of the copper coating can be determined according to the electrodeposition time.
Example 2
And preparing an electrolyte. A1000 ml beaker was taken and about 800ml of organic electrolyte was added. And manufacturing a cathode and an anode.
And cleaning the circular graphene paper. Taking a plurality of graphene paper wafers with the diameter of 2.5cm, polishing two sides of each graphene paper wafer smoothly, uniformly pricking holes on the graphene paper wafers along the circumferential direction by using a fine needle, wherein the distance between every two holes is 1mm, then ultrasonically cleaning the graphene paper wafers twice by using absolute ethyl alcohol, and drying the graphene paper wafers. Adding a proper amount of copper ions into the absolute ethyl alcohol to increase the conductivity.
Graphene paper was attached to the cathode. A copper sheet with the area of 50mm x 50mm is taken to manufacture a cathode, and a circular insulating film is covered in the middle of a certain graphene paper wafer, so that the circular graphene sheet only has a copper coating around, and the coating cannot be generated at the covered part, and the purpose of controlling the growth of the coating is achieved.
Preparing two 15cm long insulated copper wires and a power supply, setting the current to be 0.02-0.5A, connecting the anode with the anode of the power supply, connecting the cathode with the cathode of the power supply, adding a water bath heating device, setting the temperature of a heating table to be 20-100 ℃, heating, and then starting the power supply after the water temperature is constant.
In order to ensure constant current of the electrolytic cell, prevent the resistance from being too large and prevent the electrolyte from evaporating too fast, the electrolyte can be properly added in the experiment in order to keep the electrolyte sufficient, and whether the voltage and the current are normal or not is checked. After a period of time, the power is turned off.
And taking the cathode out of the electrolytic cell, taking out the circular graphene sheet, drying, and if the circular graphene sheet is not covered with the circular insulating film, uniformly covering the whole circular graphene paper with a copper coating, if the circular graphene sheet is covered with the circular insulating film, forming a concentric circle without copper plating in the middle of the circular graphene paper, wherein the copper-plated part is a part except the concentric circle and is a circular ring.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by those skilled in the art that the scope of the invention herein disclosed is not limited to the particular combination of features described above, but also encompasses other arrangements formed by any combination of the above features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (10)
1. A preparation method of a graphene paper-metal composite material is characterized by comprising the following steps:
preparing electrolyte, and preparing a cathode and an anode, wherein the anode is made of metal, and the cathode is made of metal or other conductive materials;
tightly attaching graphene paper to the cathode;
immersing both the cathode and the anode in an electrolyte;
the anode is connected with the positive pole of the power supply, the cathode is connected with the negative pole of the power supply, and the power supply is started.
2. The method of claim 1, further comprising covering the graphene paper with an insulating film before turning on the power supply.
3. The method of preparing a graphene paper-metal composite according to claim 2, further comprising uniformly providing a plurality of holes on the graphene paper along the contour direction thereof before the graphene paper is closely attached to the cathode.
4. The method of preparing a graphene paper-metal composite according to claim 3, wherein the graphene paper is circular, the plurality of holes are arranged along a circumference, and a distance between any two adjacent holes in a radial direction and an axial direction is 1 mm.
5. The method for preparing the graphene paper-metal composite material according to claim 3 or 4, further comprising cleaning the graphene paper after the graphene paper is provided with the holes and drying, wherein absolute ethyl alcohol ultrasonic waves are adopted for cleaning the graphene paper.
6. The method for preparing the graphene paper-metal composite material according to claim 1, further comprising cleaning the graphene paper and drying the graphene paper before the graphene paper is tightly attached to the cathode, wherein absolute ethyl alcohol ultrasonic waves are adopted for cleaning the graphene paper.
7. The preparation method of the graphene paper-metal composite material according to claim 1, further comprising heating the electrolyte in a water bath before turning on the power supply, wherein the heating temperature is 20-100 ℃, and the time when the power supply is turned on is after the water temperature is constant.
8. The preparation method of the graphene paper-metal composite material according to claim 1, wherein the electrolyte comprises the following components in percentage by weight: 1-15% of glycerol, 1-15% of triethanolamine, 0.5-6% of tetramethylammonium chloride, 0-2% of acetone and the balance of methanol.
9. The method for preparing the graphene-metal composite material according to claim 1, wherein the anode is made of a copper sheet, and the cathode is made of metal or other conductive materials.
10. The method for preparing the graphene paper-metal composite material according to claim 1, wherein the set current of the power supply is 0.02A-0.5A.
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Cited By (1)
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