High-conductivity copper-based graphene composite wire preparation system and method

Abstract

A high-conductivity copper-based graphene composite wire preparation system comprises a reel-to-reel graphene growth device and a graphite winding device which are arranged in a sealed space, the sealed space is provided with an air inlet and an air outlet, and the interior of the sealed space is a controlled gas environment; the roll-to-roll graphene growth device comprises a pure copper core rolling rod, a tension controller and a quartz plate, a copper foil graphite belt provided with a graphite layer is mounted on the tension controller, and the rolled copper foil belts are separated by the graphite belt; the pure copper core rolling rod is used for rolling a copper foil belt, and a quartz plate for supporting a copper foil graphite belt is arranged between the pure copper core rolling rod and the tension controller; winding the separated graphite layer through a graphite winding device; the device further comprises a hot extrusion device, and the hot extrusion device extrudes the rolled copper foil at high temperature and high pressure. The problems of high temperature control difficulty and copper foil adhesion in the prior art can be effectively solved.

Description

Technical Field

[0001] The invention relates to the field of preparation and processing of metal composite materials, and in particular to a method for preparing a high-conductivity copper-based graphene composite wire. Background Art

[0002] Room temperature graphene has great application potential in the field of metal composite materials due to its excellent electrical conductivity, thermal conductivity and mechanical properties, especially in improving the mechanical and electrical conductivity of graphene copper composite materials. However, although the existing CVD technology can produce high-quality graphene films, it faces challenges such as complex equipment, low yield and high cost in the preparation of graphene composite wires, which seriously limits its large-scale industrial production and application. The CVD process has high requirements for precise control of temperature, atmosphere and deposition rate, and has a long growth cycle, making it difficult to achieve continuous production, which restricts the promotion and application of graphene copper composite wires in the industrial field.

[0003] In the preparation of graphene copper composite wire, the main technical challenges are as follows: (1) The roll-to-roll technology has great difficulty in temperature control: The roll-to-roll process requires the uniform growth of graphene on the surface of the continuously moving copper foil, which places extremely high demands on temperature control. In the prior art (such as CN202223063256.6, CN202120609760.8), the high thermal conductivity and continuous movement of copper foil make it difficult to maintain temperature uniformity, resulting in unstable graphene quality. In addition, copper foil is prone to oxidation and adhesion at high temperatures, which further increases the complexity of the process and makes temperature control a bottleneck problem for achieving high-quality graphene growth. (2) Limitations of CVD technology for preparing composite wires: Traditional CVD technology is inefficient in preparing graphene composite wires, and high temperature has a significant effect on the mechanical properties of the wire. The CVD process is usually carried out at a high temperature of more than 900°C, which will cause the grains of the copper wire to grow and soften, significantly weakening its strength, toughness and durability. At the same time, the complex shape of the wire makes it difficult to achieve uniform heating and gas distribution in the CVD reaction chamber, resulting in uneven graphene coverage and quality fluctuations. High temperature treatment not only damages the mechanical properties of the wire, but also reduces production efficiency, becoming a major bottleneck for large-scale industrial production. Summary of the invention

[0004] In view of the above-mentioned defects, the purpose of the present invention is to propose a system for efficiently preparing graphene copper composite wires, which can effectively overcome the problems of difficult temperature control and copper foil adhesion in the prior art.

[0005] To achieve this object, the present invention adopts the following technical solutions:

[0006] A high-conductivity copper-based graphene composite wire preparation system, comprising a roll-to-roll graphene growth device and a graphite winding device arranged in a sealed space, wherein the sealed space is provided with an air inlet and an air outlet, and the sealed space is a controlled gas environment;

[0007] The roll-to-roll graphene growth device comprises a pure copper core winding rod, a tension controller and a quartz plate, wherein a copper foil graphite tape provided with a graphite layer is installed on the tension controller, and the rolled copper foil tapes are separated by the graphite tapes;

[0008] The copper foil strip is rolled up by a pure copper core winding rod, and a quartz plate for holding up the copper foil graphite strip is arranged between the pure copper core winding rod and the tension controller; the separated graphite layer is rolled up by a graphite winding device;

[0009] It also includes a hot extrusion device, which extrude the rolled copper foil at high temperature and high pressure.

[0010] Preferably, the controlled gas environment in the sealed space is argon or hydrogen.

[0011] A method for preparing a high-conductivity copper-based graphene composite wire system comprises the following steps:

[0012] Step 1, equipment preparation and atmosphere control; connect the roll-to-roll graphene growth device, graphite winding device 7 and hot extrusion device into an integrated production line; ensure that the CVD growth device is fully enclosed, and fill it with argon gas with a purity of 99.99% as a protective atmosphere to maintain a non-oxidizing environment in the reaction zone; set the atmosphere pressure in the system to 10Pa to ensure a stable atmosphere environment in the equipment, prevent copper foil oxidation and ensure high-quality growth of graphene.

[0013] Step 2: Isolate the copper foil feed from the graphite paper; use a high-purity copper foil with a width of 100 mm and a thickness of 20 μm as the substrate, and introduce the copper foil roll into the CVD reaction area through the feeding mechanism; set a graphite paper isolation layer in the copper foil unwinding area to ensure that the copper foil does not adhere at high temperature, and the chemical inertness of the graphite paper ensures that it will not affect the quality of graphene growth;

[0014] Step 3: Roll-to-roll CVD graphene growth; in the CVD reaction zone, the copper foil continuously passes through the reaction zone at a speed of 0.1 cm / min under the protection of argon to ensure uniform growth; gas flow control: methane is introduced as the carbon source gas with a flow rate of 5 sccm, and hydrogen is introduced as the reducing gas with a flow rate of 20 sccm to maintain the chemical activity of the growth environment; the reaction temperature is set to 650°C to ensure the formation of high-quality single-layer to a small number of multi-layer graphene films on the surface of the copper foil;

[0015] Step 4: Copper foil rolling: The grown graphene copper foil is rolled together with the copper rod at the rolling device. A copper rod with a diameter of 20 mm is used as the core material, and the graphene copper foil is tightly rolled on the copper rod at a winding speed of 0.1 cm / min to ensure that the graphene layer is evenly attached and free of bubbles.

[0016] Step 5: hot extrusion treatment: the rolled copper coil is directly sent to the hot extrusion device for treatment; the extrusion temperature is set to 850°C and the extrusion ratio is 25; through hot extrusion, the graphene and the copper matrix are further combined under high temperature and high pressure, which significantly improves the density and uniformity of the composite material, and improves its conductivity and mechanical properties.

[0017] Step 6: After extrusion, the wire is quickly cooled to room temperature by water cooling to form a high-density, high-conductivity graphene copper composite wire.

[0018] One of the above technical solutions includes the following beneficial effects: 1. High-efficiency anti-oxidation and temperature control: The fully enclosed gas environment design prevents the copper foil from oxidizing at high temperatures, ensures the stability and uniformity of graphene growth, improves the growth quality, and simplifies system maintenance. 2. Integrated hot extrusion process: After graphene grows, it is directly rolled up and hot-extruded to improve the density of the composite material and the uniformity of graphene dispersion, greatly enhancing the conductivity and mechanical properties of the material. 3. Large-scale production based on CVD technology: By combining the roll-to-roll system with atmosphere control, the continuity and efficiency of the CVD process are achieved, breaking through the bottleneck of low yield and high cost of traditional CVD technology, and successfully realizing the large-scale production of graphene copper composite materials, laying a solid foundation for the large-scale application of high-performance conductive materials in the industrial field. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic diagram of the overall system of one embodiment of the present invention.

[0020] Among them: 1-graphene copper roll, 2-pure copper core roll rod, 3-CVD graphene copper foil, 4-quartz plate, 5-pure copper foil graphite roll, 6-air inlet valve, 7-tension controller, 8-graphite roll, 9-tension controller, 10-air outlet. DETAILED DESCRIPTION

[0021] Embodiments of the present invention are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and cannot be understood as limiting the present invention.

[0022] As shown in the figure, a high-conductivity copper-based graphene composite wire preparation system includes a roll-to-roll graphene growth device and a graphite winding device 7 arranged in a sealed space, and the sealed space is provided with an air inlet 6 and an air outlet 10, and the sealed space is a controlled gas environment;

[0023] The roll-to-roll graphene growth device comprises a pure copper core winding rod 2, a tension controller 9 and a quartz plate 4, wherein a copper foil graphite tape 5 provided with a graphite layer is installed on the tension controller 9, and the rolled copper foil tapes are separated by graphite tapes;

[0024] The copper foil strip is rolled up by the pure copper core winding rod 2, and a quartz plate for holding up the copper foil graphite strip is arranged between the pure copper core winding rod 2 and the tension controller 9; the separated graphite layer is rolled up by the graphite winding device 7;

[0025] It also includes a hot extrusion device, which extrude the rolled copper foil at high temperature and high pressure.

[0026] Efficient anti-oxidation and temperature control: The fully enclosed gas environment design prevents copper foil from oxidizing at high temperatures, ensures the stability and uniformity of graphene growth, improves growth quality, and simplifies system maintenance. Integrated hot extrusion process: After graphene grows, it is directly rolled up and hot-extruded to improve the density of the composite material and the uniformity of graphene dispersion, greatly enhancing the conductivity and mechanical properties of the material. Large-scale production based on CVD technology: By combining the roll-to-roll system with atmosphere control, the continuity and efficiency of the CVD process are achieved, breaking through the bottleneck of low yield and high cost of traditional CVD technology, and successfully realizing the large-scale production of graphene copper composite materials, laying a solid foundation for the large-scale application of high-performance conductive materials in the industrial field. As can be seen from the figure, the tension controller 9 is rolled with a copper foil graphite strip 5, which becomes a CVD graphene copper foil 3 in a sealed space, and finally the CVD graphene copper foil 3 is rolled on a pure copper core winding rod 2 to become a graphene copper roll 1.

[0027] Wherein, the controlled gas environment in the sealed space is argon or hydrogen.

[0028] Ensure that the copper foil is not oxidized during the graphene growth process, ensuring the high-quality growth of the graphene film.

[0029] A method for preparing a high-conductivity copper-based graphene composite wire system comprises the following steps:

[0030] Step 1, equipment preparation and atmosphere control; connect the roll-to-roll graphene growth device, graphite winding device 7 and hot extrusion device into an integrated production line; ensure that the CVD growth device is fully enclosed, and fill it with argon gas with a purity of 99.99% as a protective atmosphere to maintain a non-oxidizing environment in the reaction zone; set the atmosphere pressure in the system to 10Pa to ensure a stable atmosphere environment in the equipment, prevent copper foil oxidation and ensure high-quality growth of graphene.

[0031] Step 2: Isolate the copper foil feed from the graphite paper; use a high-purity copper foil with a width of 100 mm and a thickness of 20 μm as the substrate, and introduce the copper foil roll into the CVD reaction area through the feeding mechanism; set a graphite paper isolation layer in the copper foil unwinding area to ensure that the copper foil does not adhere at high temperature, and the chemical inertness of the graphite paper ensures that it will not affect the quality of graphene growth;

[0032] Step 3: Roll-to-roll CVD graphene growth; in the CVD reaction zone, the copper foil continuously passes through the reaction zone at a speed of 0.1 cm / min under the protection of argon to ensure uniform growth; gas flow control: methane is introduced as the carbon source gas with a flow rate of 5 sccm, and hydrogen is introduced as the reducing gas with a flow rate of 20 sccm to maintain the chemical activity of the growth environment; the reaction temperature is set to 650°C to ensure the formation of high-quality single-layer to a small number of multi-layer graphene films on the surface of the copper foil;

[0033] Step 4: Copper foil rolling: The grown graphene copper foil is rolled together with the copper rod at the rolling device. A copper rod with a diameter of 20 mm is used as the core material, and the graphene copper foil is tightly rolled on the copper rod at a winding speed of 0.1 cm / min to ensure that the graphene layer is evenly attached and free of bubbles.

[0034] Step 5: hot extrusion treatment: the rolled copper coil is directly sent to the hot extrusion device for treatment; the extrusion temperature is set to 850°C and the extrusion ratio is 25; through hot extrusion, the graphene and the copper matrix are further combined under high temperature and high pressure, which significantly improves the density and uniformity of the composite material, and improves its conductivity and mechanical properties.

[0035] Step 6: After extrusion, the wire is quickly cooled to room temperature by water cooling to form a high-density, high-conductivity graphene copper composite wire.

[0036] Example 2

[0037] Step 1: Equipment preparation and atmosphere control. Connect the roll-to-roll CVD graphene growth device, winding device and hot extrusion device into an integrated production line. Ensure that the CVD growth device is fully enclosed and filled with 99.99% pure argon as a protective atmosphere to maintain a non-oxidizing environment in the reaction area. Set the atmosphere pressure in the system to 10Pa to ensure a stable atmosphere in the equipment, prevent copper foil oxidation and ensure high-quality graphene growth.

[0038] Step 2: Copper foil feeding and graphite paper isolation. Use high-purity copper foil with a width of 100 mm and a thickness of 25 μm as the substrate, and introduce the copper foil roll into the CVD reaction area through the feeding mechanism. Set a graphite paper isolation layer in the copper foil unwinding area to ensure that the copper foil does not stick at high temperatures, and the chemical inertness of the graphite paper ensures that it will not affect the quality of graphene growth.

[0039] Step 3: Roll-to-roll CVD graphene growth. In the CVD reaction zone, the copper foil continuously passes through the reaction zone at a speed of 0.5 cm / min under the protection of argon to ensure uniform growth. Gas flow control: methane (CH4) is introduced as the carbon source gas with a flow rate of 1 sccm, and hydrogen (H2) is introduced as the reducing gas with a flow rate of 10 sccm to maintain the chemical activity of the growth environment. The reaction temperature is set to 900°C to ensure the formation of a high-quality single-layer graphene film on the surface of the copper foil.

[0040] Step 4: Copper foil rolling. The grown graphene copper foil is rolled up with the copper rod at the rolling device. A copper rod with a diameter of 20 mm is used as the core material. The graphene copper foil is tightly rolled up on the copper rod at a winding speed of 0.5 cm / min to ensure that the graphene layer is evenly attached and free of bubbles. The diameter of the copper roll is 100 mm.

[0041] Step 5: Hot extrusion treatment. The rolled copper coil is directly sent to the hot extrusion device for treatment. The extrusion temperature is set to 650°C and the extrusion ratio is 25. Through hot extrusion, graphene and copper matrix are further combined under high temperature and high pressure, which improves the density and uniformity of the composite material and its conductivity and mechanical properties.

[0042] Step 6: After extrusion, the wire is quickly cooled to room temperature by water cooling to form a high-density, high-conductivity graphene copper composite wire.

[0043] The conductivity of the graphene copper rod after extrusion was tested using the four-probe test method and the test result was 105.8% IACS, which is significantly better than pure copper wire. The mechanical properties test results show that the tensile strength of the composite material is more than 15% higher than that of the copper wire without graphene.

[0044] Example 3

[0045] Step 1: Equipment preparation and atmosphere control. Connect the roll-to-roll CVD graphene growth device, winding device and hot extrusion device into an integrated production line. Ensure that the CVD growth device is fully enclosed and filled with 99.99% pure argon as a protective atmosphere to maintain a non-oxidizing environment in the reaction area. Set the atmosphere pressure in the system to 10Pa to ensure a stable atmosphere in the equipment, prevent copper foil oxidation and ensure high-quality graphene growth.

[0046] Step 2: Copper foil feeding and graphite paper isolation. Use high-purity copper foil with a width of 100 mm and a thickness of 10 μm as the substrate, and introduce the copper foil roll into the CVD reaction area through the feeding mechanism. Set a graphite paper isolation layer in the copper foil unwinding area to ensure that the copper foil does not stick at high temperatures, and the chemical inertness of the graphite paper ensures that it will not affect the quality of graphene growth.

[0047] Step 3, roll-to-roll CVD graphene growth. In the CVD reaction zone, the copper foil continuously passes through the reaction zone at a speed of 0.1cm / min under the protection of argon to ensure uniform growth. Gas flow control: methane (CH4) is introduced as the carbon source gas with a flow rate of 50sccm, and hydrogen (H2) is introduced as the reducing gas with a flow rate of 50sccm to maintain the chemical activity of the growth environment. The reaction temperature is set to 950°C to ensure the formation of high-quality single-layer to small-volume multi-layer graphene films on the surface of the copper foil. The diameter of the copper roll is 100mm.

[0048] Step 4: Copper foil winding. The grown graphene copper foil is rolled up with the copper rod at the winding device. A copper rod with a diameter of 10 mm is used as the core material, and the graphene copper foil is tightly wound on the copper rod at a winding speed of 0.1 cm / min to ensure that the graphene layer is evenly attached and free of bubbles.

[0049] Step 5: Hot extrusion treatment. The rolled copper coil is directly sent to the hot extrusion device for processing. The extrusion temperature is set to 450°C and the extrusion ratio is 25. Through hot extrusion, graphene and copper matrix are further combined under high temperature and high pressure, which improves the density and uniformity of the composite material and improves its conductivity and mechanical properties.

[0050] Step 6: After extrusion, the wire is quickly cooled to room temperature by water cooling to form a high-density, high-conductivity graphene copper composite wire.

[0051] The conductivity of the graphene copper rod after extrusion was tested using the four-probe test method and the test result was 110.5% IACS, which is significantly better than pure copper wire. The mechanical properties test results show that the tensile strength of the composite material is more than 30% higher than that of the copper wire without graphene.

[0052] The technical principle of the present invention is described above in conjunction with specific embodiments. These descriptions are only for explaining the principle of the present invention and cannot be interpreted as limiting the scope of protection of the present invention in any way. Based on the explanations herein, those skilled in the art can associate other specific implementations of the present invention without paying creative labor, and these methods will fall within the scope of protection of the present invention.

Claims

1. A system for preparing a highly conductive copper-based graphene composite wire, characterized in that: It comprises a roll-to-roll graphene growth device and a graphite winding device arranged in a sealed space, wherein the sealed space is provided with an air inlet and an air outlet, and the sealed space is a controlled gas environment; The roll-to-roll graphene growth device comprises a pure copper core winding rod, a tension controller and a quartz plate, wherein a copper foil graphite tape provided with a graphite layer is installed on the tension controller, and the rolled copper foil tapes are separated by the graphite tapes; The copper foil strip is rolled up by a pure copper core winding rod, and a quartz plate for holding up the copper foil graphite strip is arranged between the pure copper core winding rod and the tension controller; the separated graphite layer is rolled up by a graphite winding device; It also includes a hot extrusion device, which extrude the rolled copper foil at high temperature and high pressure.

2. The high-conductivity copper-based graphene composite wire preparation system according to claim 1, characterized in that: The controlled gas environment in the sealed space is argon or hydrogen.

3. A method for preparing a highly conductive copper-based graphene composite wire system according to claim 1-2, characterized in that: The steps include: Step 1, equipment preparation and atmosphere control; connect the roll-to-roll graphene growth device, graphite winding device 7 and hot extrusion device into an integrated production line; ensure that the CVD growth device is fully enclosed, and fill it with argon gas with a purity of 99.99% as a protective atmosphere to maintain a non-oxidizing environment in the reaction zone; set the atmosphere pressure in the system to 10Pa to ensure a stable atmosphere environment in the equipment, prevent copper foil oxidation and ensure high-quality growth of graphene. Step 2: Isolate the copper foil feed from the graphite paper; use a high-purity copper foil with a width of 100 mm and a thickness of 20 μm as the substrate, and introduce the copper foil roll into the CVD reaction area through the feeding mechanism; set a graphite paper isolation layer in the copper foil unwinding area to ensure that the copper foil does not adhere at high temperature, and the chemical inertness of the graphite paper ensures that it will not affect the quality of graphene growth; Step 3: Roll-to-roll CVD graphene growth; in the CVD reaction zone, the copper foil continuously passes through the reaction zone at a speed of 0.1 cm / min under the protection of argon to ensure uniform growth; gas flow control: methane is introduced as the carbon source gas with a flow rate of 5 sccm, and hydrogen is introduced as the reducing gas with a flow rate of 20 sccm to maintain the chemical activity of the growth environment; the reaction temperature is set to 650°C to ensure the formation of high-quality single-layer to a small number of multi-layer graphene films on the surface of the copper foil; Step 4: Copper foil rolling: The grown graphene copper foil is rolled together with the copper rod at the rolling device. A copper rod with a diameter of 20 mm is used as the core material, and the graphene copper foil is tightly rolled on the copper rod at a winding speed of 0.1 cm / min to ensure that the graphene layer is evenly attached and free of bubbles. Step 5: hot extrusion treatment: the rolled copper coil is directly sent to the hot extrusion device for treatment; the extrusion temperature is set to 850°C and the extrusion ratio is 25; through hot extrusion, the graphene and the copper matrix are further combined under high temperature and high pressure, which significantly improves the density and uniformity of the composite material, and improves its conductivity and mechanical properties. Step 6: After extrusion, the wire is quickly cooled to room temperature by water cooling to form a high-density, high-conductivity graphene copper composite wire.

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