CN114507791A - Production method and equipment of graphene metal conductive material - Google Patents
Production method and equipment of graphene metal conductive material Download PDFInfo
- Publication number
- CN114507791A CN114507791A CN202210095786.4A CN202210095786A CN114507791A CN 114507791 A CN114507791 A CN 114507791A CN 202210095786 A CN202210095786 A CN 202210095786A CN 114507791 A CN114507791 A CN 114507791A
- Authority
- CN
- China
- Prior art keywords
- graphene
- conductive material
- die
- metal
- integrated growth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of graphene metal material preparation, and discloses a production method and equipment of a graphene metal conductive material. The equipment comprises an integrated growth mould pressing cavity and a pipeline system communicated with the integrated growth mould pressing cavity, wherein a heating system, a clamp and a mould are arranged in the integrated growth mould pressing cavity, the mould comprises a male mould and a female mould which can move vertically, and the clamp is positioned between the male mould and the female mould. According to the invention, the graphene growing step and the compression molding step are carried out in the same chamber, so that the metal foil/plate with the graphene is prevented from contacting air before compression molding, the influence of moisture, impurities and oxygen in the air on the metal foil/plate with the graphene is avoided, the conductivity of the graphene metal conductive material is improved, and the quality of the graphene metal conductive material is improved.
Description
Technical Field
The invention relates to the technical field of preparation of graphene metal materials, in particular to a production method and equipment of a graphene metal conductive material.
Background
Under conventional conditions, pure silver has the best conductive performance, but is expensive and difficult to apply on a large scale, and the electron mobility of the graphene material can reach 2 x 105cm2V s has excellent electrical properties, but the cost is lower than that of pure silver. Therefore, the graphene-based composite material is available, so that the material with both cost and performance can be obtained greatly. This has prompted intensive research into graphene-based composites and their preparation.
At present, researchers prepare graphene metal conductive materials from metal powder with graphene through a hot press molding process, so that the conductivity can be improved to a certain extent. However, since the graphene is in a discrete distribution state in the composite material, continuity cannot be formed, and the conductivity of the prepared graphene metal conductive material is improved to a limited extent. The preparation method needs to be implemented in multiple steps, firstly growing graphene on metal powder and a carbon source in one device, taking out the metal powder with the graphene after cooling, then transferring the metal powder into another device for hot press molding, and then taking out the metal powder after cooling to obtain the graphene metal conductive material. In the preparation process of the graphene metal conductive material, multiple times of heating and cooling are needed, energy is consumed, the cost is high, the number of production steps is large, and the performance of the obtained graphene metal conductive material cannot reach the expectation.
Disclosure of Invention
In view of the above disadvantages of the prior art, an object of the present invention is to provide a method and an apparatus for producing a graphene metal conductive material, which are used to solve the problems of energy consumption and more production steps in the preparation of the graphene metal conductive material in the prior art.
In order to achieve the above and other related objects, the present invention provides a method for producing a graphene metallic conductive material, including a graphene growing step and a compression molding step, wherein the graphene growing step and the compression molding step are performed in the same chamber.
Optionally, in the graphene growing step, the temperature in the chamber is 500-1200 ℃.
Optionally, in the graphene growing step, the chamber is vacuumized in advance, so that the pressure P in the chamber satisfies the following condition: p is more than 0 and less than or equal to 100 KPa.
Optionally, in the graphene growing step, the metal material for growing graphene is selected from one of copper, silver, gold, palladium, nickel, tungsten, aluminum, iron, and an alloy.
Optionally, in the graphene growing step, the metal material for growing graphene is a metal foil/plate.
Optionally, in the graphene growing step, the temperature in the chamber is 800-1200 ℃.
Optionally, in the graphene growing step, the chamber is vacuumized in advance, so that the pressure P in the chamber satisfies the following condition: p is more than 0 and less than or equal to 10 a.
Optionally, the thickness of the metal material is 3 μm to 100 mm.
Optionally, the graphene grown on the metal material is 1-5 layers.
Optionally, in the compression molding step, the compression temperature of the mold is 500-1200 ℃.
Optionally, in the compression molding step, the mold pressing pressure is greater than 0 and equal to or less than 100 MPa.
The invention also provides the graphene metal conductive material prepared by the production method.
The invention also provides production equipment used in the production method of the graphene metal conductive material, which comprises an integrated growth and mould pressing cavity and a pipeline system, wherein the pipeline system is communicated with the integrated growth and mould pressing cavity; and a cooling jacket is arranged on the outer wall of the integrated growth die pressing cavity.
Optionally, the clamp is a retractable clamp, which is compressed in the compression molding step.
Optionally, the telescopic clamp includes more than four suspension portions, each suspension portion includes a plurality of first rods and a plurality of second rods, a central portion of each first rod is hinged to a central portion of each second rod, top ends and bottom ends of the first rods are respectively hinged to end portions of the vertically adjacent second rods, and top ends and bottom ends of the second rods are respectively hinged to end portions of the vertically adjacent first rods.
Optionally, the jig is removably attached within the integrated growth die cavity.
Optionally, a top die-pressing jacking mechanism for driving the male die is arranged outside the integrated growth die-pressing cavity; or, a top die-pressing jacking mechanism for driving the male die and a bottom die-pressing jacking mechanism for driving the female die are arranged outside the integrated growth die-pressing cavity.
As described above, the method and apparatus for producing a graphene metal conductive material of the present invention have the following beneficial effects:
1) according to the invention, the graphene growing step and the compression molding step are carried out in the integrated growth molding cavity, so that the graphene metal conductive material can be obtained by compression molding after the graphene grows on the metal material, the metal material with the graphene growing is prevented from being transferred between devices, the operation steps are reduced, the heating and cooling times are reduced, the energy is saved, the possibility of oxidation and pollution of the composite material is greatly reduced, and the conductivity of the graphene metal conductive material is improved.
2) According to the invention, the metal foil/plate is used as the growth substrate of the graphene, the obtained graphene is continuous and stable, the quality is excellent, and compared with the graphene metal conductive material obtained by taking metal powder as the growth substrate, the graphene metal conductive material provided by the invention can effectively improve the conductivity of the graphene metal conductive material.
3) The production equipment of the graphene metal conductive material can realize that the graphene growth step and the compression molding step are carried out in the same cavity, in addition, the clamp in the integrated growth compression molding cavity is a telescopic clamp, the telescopic clamp is compressed in the compression molding step, the distance between two adjacent metal foils/plates is gradually reduced in the compression process of the telescopic clamp, but the metal foils/plates cannot be subjected to the compression force, compared with a non-telescopic common clamp, the production equipment of the graphene metal conductive material greatly reduces the tensile deformation amount of the metal foils/plates due to the fact that the metal foils/plates are fixed on the common clamp when the metal foils/plates are subjected to the compression force of a mold in the compression molding step, thereby greatly reducing the friction degree of the metal foils/plates due to the tensile deformation, and finally greatly reducing the damage degree of the graphene structure grown on the surfaces of the metal foils/plates, thereby further improving the conductivity of the graphene metal conductive material.
Drawings
Fig. 1 is a front view of a production apparatus for a graphene metal conductive material in embodiment 1 of the present invention;
fig. 2 is a half sectional view of a production apparatus for a graphene metal conductive material in embodiment 1 of the present invention;
fig. 3 is a schematic structural view of a metal copper foil hung on a hanging part in example 1 of the present invention;
FIG. 4 is a schematic view showing a compressed suspension part according to embodiment 1 of the present invention;
fig. 5 is a half sectional view of a production apparatus for a graphene metal conductive material in embodiment 2 of the present invention;
fig. 6 is a production flow chart of a method for producing a graphene metal conductive material in embodiment 1 of the present invention.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the description of the present invention. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The invention provides a production method of a graphene metal conductive material, which comprises a graphene growing step and a compression molding step, wherein the graphene growing step and the compression molding step are carried out in the same chamber.
In the graphene growth step, a chamber is vacuumized in advance, so that the pressure P in the chamber meets the following conditions: p is more than 0 and less than or equal to 100 KPa; the temperature in the cavity is 500-1200 ℃.
In the graphene growing step, the metal material for growing the graphene is selected from one of copper, silver, gold, palladium, nickel, tungsten, aluminum, iron and alloy, the metal material for growing the graphene is a metal foil/plate, the thickness of the metal material is 3 mu m-100 mm, and the graphene grown on the metal material is 1-5 layers.
In the graphene growing step, a carbon source for growing graphene is selected from one of a gaseous carbon source, a solid carbon source and a liquid carbon source, the gaseous carbon source is selected from one of methane and acetylene, and the solid carbon source is selected from one of polymethyl methacrylate and polystyrene.
In the compression molding step, the compression temperature of the mold is 500-1200 ℃, and the compression pressure of the mold is more than 0 and less than or equal to 100 MPa.
The invention also provides the graphene metal conductive material prepared by the production method.
The invention also provides production equipment used in the production method of the graphene metal conductive material, which comprises an integrated growth mould pressing cavity and a pipeline system, wherein the pipeline system is communicated with the integrated growth mould pressing cavity. The integrated growth mould pressing chamber is internally provided with a heating system, a mould and a clamp for fixing the metal foil/plate, the mould comprises a male mould and a female mould, and the outside of the integrated growth mould pressing chamber is provided with a bottom mould pressing jacking mechanism for driving the female mould. The clamp is positioned between the male die and the female die.
The pipeline system comprises a special gas pipeline, a backfill pipeline and a vacuum pipeline, wherein valves and flow controllers are respectively arranged on the special gas pipeline and the backfill pipeline, and a vacuum valve and a vacuum pressure gauge are arranged on the vacuum pipeline.
The heating system is used for heating the integrated growth and mould pressing cavity and comprises a heating assembly, a temperature sensor and a controller.
Be equipped with the cavity in the lateral wall of integration growth mould pressing cavity, the cavity intercommunication has inlet tube and outlet pipe for lower the temperature to integration growth mould pressing cavity. The outer side wall of the integrated growth die pressing cavity is wrapped with the heat preservation layer and the cooling jacket, and the heat overflowing from the integrated growth die pressing cavity is cooled, so that the outside of the production equipment is kept in a state of 25-30 ℃.
The side wall of the integrated growth mould pressing cavity is provided with a feeding hole and a discharging hole, and the feeding hole and the discharging hole are rotatably connected with a sealing door used for sealing the feeding hole and the discharging hole.
In another embodiment of the present invention, the clamp is a telescopic clamp, the telescopic clamp is compressed in the compression molding step, the telescopic clamp includes more than four suspension portions, each suspension portion includes a plurality of first rods and a plurality of second rods, a central portion of each first rod is hinged to a central portion of each second rod, top ends and bottom ends of the first rods are respectively hinged to end portions of the vertically adjacent second rods, and top ends and bottom ends of the second rods are respectively hinged to end portions of the vertically adjacent first rods.
In another embodiment of the invention, the clamp is detachably connected in the integrated growth die pressing chamber, the top end of the clamp is fixedly connected with the T-shaped slide block, and the top wall of the integrated growth die pressing chamber is provided with a T-shaped sliding groove for the T-shaped slide block to horizontally slide.
In another embodiment of the invention, a top die pressing jacking mechanism for driving the male die is arranged outside the integrated growth die pressing cavity.
The present invention will be described in detail below with reference to specific exemplary embodiments. It should also be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention, and that numerous insubstantial modifications and adaptations of the invention described above will occur to those skilled in the art. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Reference numerals in the drawings of the specification include: the device comprises a frame 100, an integrated growth die pressing chamber 200, a heating assembly 201, a male die 202, a female die 203, a top die pressing jacking mechanism 204, a bottom die pressing jacking mechanism 205, a cavity 210, a cooling jacket 220, a sealing door 230, an observation window 231, a pipeline system 300, a special air pipeline 301, a backfill pipeline 302, a vacuum pipeline 303, a hanging part 400, a first rod 401, a second rod 402, a fixing plate 403, a T-shaped sliding block 404 and a metal copper foil 500.
Example 1
This embodiment is substantially as shown in fig. 1 and 2: the utility model provides a production facility of graphite alkene metal conducting material, includes frame 100, fixedly connected with integration growth mould pressing cavity 200 on frame 100, in this embodiment, integration growth mould pressing cavity 200 passes through bolt fixed mounting on frame 100. The integrated growth molding cavity 200 is communicated with a pipeline system 300, specifically, the pipeline system 300 comprises a special gas pipeline 301, a backfill pipeline 302 and a vacuum pipeline 303, valves and flow controllers are mounted on the special gas pipeline 301 and the backfill pipeline 302, a vacuum valve and a vacuum pressure gauge are mounted on the vacuum pipeline 303, and a vacuum pump is communicated with one end of the vacuum pipeline 303 far away from the integrated growth molding cavity 200.
The integrated growth-molding chamber 200 is provided with a heating system, a mold, and a fixture for fixing the metal foil/plate. Heating system includes heating element 201, temperature sensor and controller, and heating element 201 is used for the intracavity intensification of integration growth mould pressing cavity 200, and temperature sensor is used for monitoring the temperature in the integration growth mould pressing cavity 200 to convert temperature signal into the signal of telecommunication and transmit the controller, the controller control heating element 201 opens and close. Since it is the prior art to detect signals by using the sensor and transmit the related signals to the controller, and the controller controls the actuator to execute actions according to the received signals, the details are not described herein. In this embodiment, the heating element 201 is a resistance wire heater.
The mold comprises a male mold 202 and a female mold 203, and a top molding jacking mechanism 204 for driving the male mold 202 and a bottom molding jacking mechanism 205 for driving the female mold 203 are arranged outside the integrated growth molding chamber 200. In this embodiment, the top molding jacking mechanism 204 and the bottom molding jacking mechanism 205 both employ hydraulic cylinders, and the top molding jacking mechanism 204 and the bottom molding jacking mechanism 205 are both fixedly mounted on the rack 100 through bolts.
The fixture is a telescopic fixture, the telescopic fixture is compressed in the die assembly process, the telescopic fixture comprises more than four hanging parts 400, in the embodiment, the number of the hanging parts 400 is four, the four hanging parts 400 are distributed on the left side and the right side in the integrated growth die pressing cavity 200 in a pairwise manner, and the two hanging parts 400 located on the same side are arranged in order in the horizontal longitudinal direction. As shown in fig. 3, each of the suspending portions 400 includes a plurality of first rods 401 and a plurality of second rods 402, a central portion of each of the first rods 401 is hinged to a central portion of each of the second rods 402, top and bottom ends of each of the first rods 401 are hinged to ends of vertically adjacent second rods 402, and top and bottom ends of each of the second rods 402 are hinged to ends of vertically adjacent first rods 401. The top end of the hanging part 400 is provided with a fixing plate 403, the top ends of the first rod 401 and the second rod 402 which are positioned at the top are horizontally and slidably connected on the fixing plate 403, and the fixing plate 403 is fixedly installed on the top wall of the integrated growth molding chamber 200 through screws. In this embodiment, the number of the first rods 401 and the second rods 402 is eighteen, and those skilled in the art can select an appropriate number of the first rods 401 and the second rods 402 to assemble the retractable clamp according to actual requirements.
The side wall of the integrated growth mold pressing cavity 200 is provided with a cavity 210, and the cavity 210 is communicated with a water inlet pipe and a water outlet pipe for cooling the integrated growth mold pressing cavity 200. The outer side wall of the integrated growth die pressing cavity 200 is wrapped with the heat preservation layer and the cooling jacket 220, the heat preservation layer is used for reducing heat dissipation in the integrated growth die pressing cavity 200, the cooling jacket 220 is used for cooling heat overflowing from the integrated growth die pressing cavity 200, and the outside of the production equipment is kept in a state of 25-30 ℃.
The side wall of the integrated growth mold pressing cavity 200 is provided with an upper material opening and a lower material opening, the upper material opening and the lower material opening are rotatably connected with a sealing door 230 used for sealing the upper material opening and the lower material opening, and an observation window 231 is arranged on the sealing door 230.
A method for producing a graphene metal conductive material by using the production equipment for a graphene metal conductive material, as shown in fig. 6, includes the following steps:
s1, placing the metal material in the integrated growth die pressing chamber: the suspension part 400 is stretched by pulling the suspension part 400 downward, the suspension part 400 is thinned while the suspension part 400 is stretched because the first rod 401 and the second rod 402 are hinged to each other, the edge portion of the metal copper foil 500 (17 metal copper foils 500 in this embodiment) for growing graphene is perforated, after the perforation, the hole of the 17 metal copper foils 500 is perforated through the thinned suspension part 400, the 17 metal copper foils 500 are separated and supported between the suspension parts 400 by using an auxiliary tool, each metal copper foil 500 is respectively positioned at the hinge point of the central portion of the corresponding first rod 401 and the second rod 402, the auxiliary tool comprises a vertical plate and an insert plate, the vertical plate is provided with a plurality of slots for inserting the insert plate horizontally, after the metal copper foils 500 are separated upward, the insert plate is inserted into the corresponding slots, thereby supporting the metal copper foils 500, and making the metal copper foils 500 flush with the central portions of the corresponding first rod 401 and second rod 402, so, after separating 17 metal copper foils 500 (namely 17 metal copper foils 500 all level with the pin joint of the first pole 401 that corresponds and second pole 402 central part mutually), the application of force makes linkage 400 compress, its length shortens, thereby make the bottom interval grow (the bottom interval is greater than the aperture of metal copper foil 500) of first pole 401 and second pole 402, thereby hang metal copper foil 500 on linkage 400, take out appurtenance at last, accomplish the operation of putting into metal copper foil 500 integration chamber, there is the interval between two adjacent metal copper foils 500 can not contact, as shown in fig. 3 after metal copper foil 500 hangs. Subsequently, the sealing door 230 of the upper and lower ports is closed. In this example, the thickness of the metal copper foil 500 was 25 μm.
S2, adjusting parameters in the integrated growth die pressing chamber: and starting a vacuum pump, pumping out air in the integrated growth and mould pressing cavity 200 through a vacuum pipeline 303, enabling the air pressure in the integrated growth and mould pressing cavity 200 to reach 20Pa, then closing a vacuum valve, and stopping the vacuum pump. Then, the valve on the backfill pipeline 302 is opened, the protective gas (in this embodiment, the protective gas is argon, and the flow rate of the argon is 350sccm) enters the integrated growth and mold-pressing chamber 200, and after the internal pressure of the integrated growth and mold-pressing chamber 200 is restored to the normal pressure, the vacuum valve is opened, so that the redundant argon is discharged through the vacuum pipeline 303, and the inside of the integrated growth and mold-pressing chamber 200 is in a micro-positive pressure state. Then, the heating system is started, and the heating assembly 201 is powered on to heat the integrated growth and die pressing chamber 200, so that the temperature in the integrated growth and die pressing chamber 200 is increased to 1020 ℃. When the temperature in the integrated growth and mold pressing chamber 200 reaches 1020 ℃, the temperature sensor converts the temperature signal into an electric signal and transmits the electric signal to the controller, and the controller controls the heating assembly 201 to stop working.
S3, graphene growth: introducing process gas (in the embodiment, the process gas refers to methane and hydrogen, the flow rate of the methane is 25sccm, and the flow rate of the hydrogen is 55sccm) into the integrated growth and die pressing chamber 200 through a special gas pipeline 301, keeping the input of argon during the introduction of the process gas, and starting a heating system to raise the temperature in the integrated growth and die pressing chamber 200 to 1060 ℃ for graphene growth.
S4, compression molding: after the graphene growth is completed, the valve on the special gas pipeline 301 is closed, argon is continuously introduced into the integrated growth molding cavity 200 through the backfill pipeline 302, and the heating system is closed. After the heating system is closed, the temperature in the integrated growth and press molding chamber 200 is reduced, the temperature of the mold is also reduced, when the temperature of the mold is 900 ℃, the bottom press molding jacking mechanism 205 drives the female mold 203 to move upwards, the female mold 203 abuts against the bottom end of the hanging part 400, upward thrust is applied to the hanging part 400, so that the hanging part 400 is compressed (namely a clamp is compressed), the metal copper foil 500 hung on the hanging part 400 moves accordingly, the distance between two adjacent metal copper foils 500 is gradually reduced until the hanging part 400 is compressed to the limit (as shown in fig. 4), the top press molding jacking mechanism 204 drives the male mold 202 to move downwards, the male mold 202 and the female mold 203 are closed, the metal copper foil 500 is pressed, and the press pressure of the mold is 30 MPa. After the male mold 202 and the female mold 203 are closed, the metal copper foil 500 is cut off so that the metal copper foil 500 is separated from the hanging part 400.
In the compression molding process, since the hanging part 400 can be compressed, the female die 203 does not contact the metal copper foil 500 at the bottom layer initially, so that the metal copper foil 500 is not subjected to tensile deformation due to the acting force applied to the metal copper foil 500, and the phenomenon of friction between two adjacent metal copper foils 500 due to the tensile deformation does not exist, only after the hanging part 400 is compressed to the utmost, in the process of closing the male mold 202 moving downward and the female mold 203, a pressing force is applied to the metallic copper foil 500, therefore, in the step, the amount of the metal foil/plate which is stretched and deformed because of being fixed on a common clamp is greatly reduced, therefore, the friction degree between the metal foils/plates caused by tensile deformation is greatly reduced, and finally, the damage degree of the graphene structure grown on the surfaces of the metal foils/plates is greatly reduced, so that the conductivity of the graphene metal conductive material is further ensured.
S5, taking materials: after compression molding, top mould pressing climbing mechanism 204 drives public mould 202 rebound and resets, and bottom mould pressing climbing mechanism 205 drives master model 203 rebound and resets, simultaneously, utilizes the inlet tube to continuous input cooling water in the cavity 210 of integration growth mould pressing cavity 200 lateral wall, flows out from the outlet pipe after the cooling water absorbs the heat to the realization is to the cooling of integration growth mould pressing cavity 200. After the temperature of the integrated growth and mold pressing chamber 200 is reduced to room temperature, the sealing door 230 is opened, the graphene metallic copper conductive material is taken out through the upper and lower material openings, finally, the valve on the backfill pipeline 302 is closed, and the input of argon gas is stopped.
Example 2
The present embodiment is different from embodiment 1 in that: in step S4, the mold press bonding pressure is 40 MPa.
Example 3
The present embodiment is different from embodiment 1 in that: in this embodiment, the fixture is detachably connected to the integrated growth cavity, specifically, as shown in fig. 5, a T-shaped slider 404 is welded to the top end of the fixing plate 403, and a T-shaped chute for the T-shaped slider 404 to horizontally slide is formed in the top wall of the integrated growth cavity.
In this embodiment, the horizontal sliding connection of linkage 400 is in T type spout through T type slider 404 to realize linkage 400 can dismantle in integration growth mould pressing cavity 200, so that the user with linkage 400 roll-off integration growth mould pressing cavity 200 or take out integration growth mould pressing cavity 200, carry out metal copper foil 500's suspension outside integration growth mould pressing cavity 200, operating space is bigger, it is more convenient to operate.
Comparative example
This comparative example differs from example 1 in that: the comparative example adopts the same technological parameters to grow the graphene on the metal copper foil in the graphene growth equipment, then the metal copper foil is taken out after cooling to obtain the metal copper foil with the graphene, the metal copper foil is placed for 8 hours in a natural environment (simulating the production mode that the metal copper foil with the graphene is firstly prepared in the prior art and is stored for a period of time and then is subjected to roll forming), and then 17 pieces of the metal copper foil with the graphene are subjected to mould pressing according to the same compression molding technological parameters as the embodiment 1 to obtain the graphene metal copper conductive material.
Experimental example 1
For the graphene metallic copper conductive materials in the embodiments 1, 2, 3 and the comparative examples, the conductivity of the composite material is determined according to the "metallic material resistivity measurement method (GB/T351-.
TABLE 1 composite conductivity
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Conductivity (S/m) | 66.7×106 | 68.5×106 | 66.4×106 | 57.6×106 |
Experimental example 2
According to the production methods of the embodiment 1 and the comparative example, three times of production are performed to obtain graphene metallic copper conductive materials with different production batches, the conductivity of the graphene metallic copper conductive materials with different production batches is measured according to the metal material resistivity measurement method (GB/T351-.
Table 2 conductivity of graphene metallic copper conductive material of different production batches
As can be seen from table 1, the conductivity of the graphene metallic copper conductive material in examples 1 to 3 is significantly higher than that of the graphene metallic copper conductive material in the comparative example, which shows that the present invention can significantly improve the conductivity of the graphene metallic conductive material. Moreover, as can be seen from table 2, the standard deviation of example 1 is smaller than that of the comparative example, which indicates that in example 1, the stability between different production batches of graphene metal conductive materials is better, that is, the present invention can avoid adverse effects of external environments on the composite material, and the production quality of the graphene metal conductive material in the present invention is more stable.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A production method of a graphene metal conductive material comprises a graphene growth step and a compression molding step, and is characterized in that: the graphene growing step and the compression molding step are performed in the same chamber.
2. The method for producing a graphene metal conductive material according to claim 1, characterized in that: in the graphene growing step, the temperature in the cavity is 500-1200 ℃;
and/or in the graphene growing step, vacuumizing the chamber in advance to enable the air pressure P in the chamber to meet the following conditions: p is more than 0 and less than or equal to 100 KPa;
and/or, in the graphene growing step, the metal material for growing the graphene is selected from one of copper, silver, gold, palladium, nickel, tungsten, aluminum, iron and alloy;
and/or, in the graphene growing step, the metal material for growing the graphene is a metal foil/plate.
3. The method for producing a graphene metal conductive material according to claim 2, characterized in that: in the graphene growing step, the temperature in the cavity is 800-1200 ℃;
and/or in the graphene growing step, vacuumizing the chamber in advance to enable the air pressure P in the chamber to meet the following conditions: p is more than 0 and less than or equal to 10 Pa;
and/or the thickness of the metal material is 3 mu m-100 mm;
and/or the graphene growing on the metal material is 1-5 layers.
4. The method for producing a graphene metal conductive material according to claim 1, characterized in that: in the compression molding step, the compression temperature of the mold is 500-1200 ℃;
and/or in the compression molding step, the compression pressure of the mold is more than 0 and less than or equal to 100 MPa.
5. A graphene metal conductive material produced by the production method according to any one of claims 1 to 4.
6. A production apparatus of a graphene metal conductive material used for the production method according to any one of claims 1 to 4, characterized in that: the integrated growth die pressing device comprises an integrated growth die pressing cavity and a pipeline system, wherein the pipeline system is communicated with the integrated growth die pressing cavity, a heating system, a die and a clamp for fixing a metal foil/plate are arranged in the integrated growth die pressing cavity, the die comprises a male die and a female die, and the clamp is positioned between the male die and the female die; and a cooling jacket is arranged on the outer wall of the integrated growth die pressing cavity.
7. The apparatus for producing a graphene metallic conductive material according to claim 6, wherein: the clamp is a telescopic clamp, and the telescopic clamp is compressed in the compression molding step.
8. The apparatus for producing a graphene metallic conductive material according to claim 7, wherein: the telescopic clamp comprises more than four suspension parts, each suspension part comprises a plurality of first rods and a plurality of second rods, the center parts of the first rods are hinged to the center parts of the second rods, the top ends and the bottom ends of the first rods are hinged to the end parts of the vertically-adjacent second rods respectively, and the top ends and the bottom ends of the second rods are hinged to the end parts of the vertically-adjacent first rods respectively.
9. The apparatus for producing a graphene metallic conductive material according to claim 6, wherein: the clamp is detachably connected in the integrated growth die pressing cavity.
10. The apparatus for producing a graphene metallic conductive material according to claim 6, wherein: a top die pressing jacking mechanism for driving the male die is arranged outside the integrated growth die pressing cavity;
or, a top die-pressing jacking mechanism for driving the male die and a bottom die-pressing jacking mechanism for driving the female die are arranged outside the integrated growth die-pressing cavity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210095786.4A CN114507791B (en) | 2022-01-26 | 2022-01-26 | Production method and equipment of graphene metal conductive material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210095786.4A CN114507791B (en) | 2022-01-26 | 2022-01-26 | Production method and equipment of graphene metal conductive material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114507791A true CN114507791A (en) | 2022-05-17 |
| CN114507791B CN114507791B (en) | 2022-09-23 |
Family
ID=81549677
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210095786.4A Active CN114507791B (en) | 2022-01-26 | 2022-01-26 | Production method and equipment of graphene metal conductive material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114507791B (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060288927A1 (en) * | 2005-06-24 | 2006-12-28 | Robert Chodelka | System and high pressure, high temperature apparatus for producing synthetic diamonds |
| CN103345979A (en) * | 2013-06-27 | 2013-10-09 | 中国科学院微电子研究所 | Preparation method of graphene conductive film |
| CN106868715A (en) * | 2016-12-31 | 2017-06-20 | 南京新月材料科技有限公司 | A kind of preparation method of compression molding Graphene non-woven fabrics |
| CN109306466A (en) * | 2017-07-28 | 2019-02-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method of semiconductor material |
| CN109811175A (en) * | 2019-03-26 | 2019-05-28 | 重庆大学 | A kind of graphene-method of manufacturing carbon/carbon-copper composite material |
| CN209242684U (en) * | 2018-11-09 | 2019-08-13 | 北京石墨烯研究院 | Utilize the carrier of CVD method growth graphene film |
| CN111485224A (en) * | 2019-01-29 | 2020-08-04 | 北京石墨烯研究院 | Chemical vapor deposition apparatus |
| CN112746262A (en) * | 2019-10-29 | 2021-05-04 | 北京石墨烯研究院 | Graphene composite metal foil and double-sided growth method and device thereof |
| CN113445030A (en) * | 2020-03-25 | 2021-09-28 | 北京石墨烯研究院 | Method for improving cleanliness of graphene film |
| CN113718230A (en) * | 2020-05-26 | 2021-11-30 | 北京石墨烯研究院 | Chemical vapor deposition device and method for preparing graphene film |
| CN113909476A (en) * | 2020-07-10 | 2022-01-11 | 上海新池能源科技有限公司 | Method for growing graphene on structured copper base, cable core material and preparation method thereof |
-
2022
- 2022-01-26 CN CN202210095786.4A patent/CN114507791B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060288927A1 (en) * | 2005-06-24 | 2006-12-28 | Robert Chodelka | System and high pressure, high temperature apparatus for producing synthetic diamonds |
| CN103345979A (en) * | 2013-06-27 | 2013-10-09 | 中国科学院微电子研究所 | Preparation method of graphene conductive film |
| CN106868715A (en) * | 2016-12-31 | 2017-06-20 | 南京新月材料科技有限公司 | A kind of preparation method of compression molding Graphene non-woven fabrics |
| CN109306466A (en) * | 2017-07-28 | 2019-02-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method of semiconductor material |
| CN209242684U (en) * | 2018-11-09 | 2019-08-13 | 北京石墨烯研究院 | Utilize the carrier of CVD method growth graphene film |
| CN111485224A (en) * | 2019-01-29 | 2020-08-04 | 北京石墨烯研究院 | Chemical vapor deposition apparatus |
| CN109811175A (en) * | 2019-03-26 | 2019-05-28 | 重庆大学 | A kind of graphene-method of manufacturing carbon/carbon-copper composite material |
| CN112746262A (en) * | 2019-10-29 | 2021-05-04 | 北京石墨烯研究院 | Graphene composite metal foil and double-sided growth method and device thereof |
| CN113445030A (en) * | 2020-03-25 | 2021-09-28 | 北京石墨烯研究院 | Method for improving cleanliness of graphene film |
| CN113718230A (en) * | 2020-05-26 | 2021-11-30 | 北京石墨烯研究院 | Chemical vapor deposition device and method for preparing graphene film |
| CN113909476A (en) * | 2020-07-10 | 2022-01-11 | 上海新池能源科技有限公司 | Method for growing graphene on structured copper base, cable core material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114507791B (en) | 2022-09-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114507791B (en) | Production method and equipment of graphene metal conductive material | |
| CN217047854U (en) | Preparation device of graphene metal laminated composite material | |
| CN216832370U (en) | Integrated production device for graphene metal conductive material | |
| CN111139453B (en) | Preparation method of high-conductivity copper/graphene composite material | |
| CN216801533U (en) | A growth forging and pressing integration equipment for preparing graphite alkene metal composite | |
| CN216828449U (en) | Growth forging and pressing split type equipment for preparing graphene metal composite material | |
| CN116718012A (en) | Multifunctional sintering furnace for graphene heat conducting film production | |
| CN218286837U (en) | Induction hot-press forming device | |
| CN104438425B (en) | Method for preparing buses for electrical engineering through taking high-quality aluminum ingots as raw material | |
| CN115214179A (en) | Induction hot press molding device | |
| CN212310613U (en) | New energy automobile battery case stamping die | |
| CN114433628B (en) | Graphene reinforced high-conductivity metal material growth and rolling integrated method and device | |
| CN201514855U (en) | Sample line straightening device of transposed conductor | |
| CN104307916B (en) | Preparation method of aluminum and aluminum alloy bus | |
| CN109940056B (en) | High-efficient multi-functional self-heating equal channel extrusion device | |
| CN112547830A (en) | Manufacturing method of oversized U-shaped copper bar and continuous extrusion die thereof | |
| CN202534443U (en) | Twisting mold of metal wire for cable | |
| CN219454619U (en) | Heating and pressurizing electrode of sintering equipment for graphene heat-conducting film production | |
| CN107824629B (en) | A kind of vacuum hot-pressing process of silver-bearing copper composite band | |
| CN114433763B (en) | Folding forging method and device for high-conductivity graphene metal composite material | |
| CN209888228U (en) | Electrode paste forming device | |
| CN221046961U (en) | Extrusion molding die | |
| CN218159657U (en) | High-temperature-resistant copper rod suitable for non-ferrous metal rolled products | |
| CN217665700U (en) | Carbon steel three-way pipe forming device | |
| CN219335542U (en) | Burst-proof die for stretching battery box body |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |