Manufacturing process of graphene heat dissipation film coil material

A continuous manufacturing process for graphene dissipation film coils addresses the inefficiencies of existing methods by achieving stable and efficient production with improved thermal conductivity, suitable for industrial automation.

JP7625765B2Active Publication Date: 2025-02-03ZHEJIANG DAOMING SUPERCONDUCTOR TECH CO LTD
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Patent Information

Application Number
JP2024518764
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2022-03-04
Filing Date
2022-12-08
Publication Date
2025-02-03
Estimated Expiration
2042-12-08

AI Technical Summary

Technical Problem

The current manufacturing process for graphene heat dissipation membranes is not continuous, leading to high molding costs, complex production processes, and high labor costs, making it unsuitable for industrial automation.

Method used

A continuous manufacturing process for graphene dissipation film coils involving steps such as dispersing graphene oxide in water, adjusting pH, homogenizing and foaming, applying the graphene oxide solution on a substrate, rolling, and subjecting it to low-temperature and carbonization processes to achieve a thermal conductivity of 800-2000 W·m/k.

Benefits of technology

The process results in a stable, efficient, and cost-effective production of graphene dissipation coils with enhanced thermal conductivity, suitable for industrial automation.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The manufacturing process for a graphene heat dissipation film coil material includes the steps of: step S1 of preparing a graphene oxide dispersion using a graphene oxide cake; step S2 of performing homogenization and degassing treatment; step S3 of applying the graphene oxide slurry onto a substrate with a coater, then performing peeling and slitting treatment to obtain a pretreated graphene film, which is then wound up to obtain a tight pretreated graphene film tight coil material (1); step S4 of putting the pretreated graphene film tight coil material (1) into an unwinding mechanism to perform unwinding treatment to obtain a pretreated graphene film loose coil material (2); step S5 of performing low-temperature treatment, carbonization treatment, and graphitization treatment on the pretreated graphene film loose coil material (2) to obtain a graphene foam film coil material; and step S6 of performing single-layer roll pressing or multi-layer roll pressing on the graphene foam film coil material to obtain a graphene heat dissipation coil material.
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Description

[Technical field]

[0001] The present invention relates to the technical field of graphene, and in particular to a manufacturing process for graphene heat dissipation film coil material. [Background technology]

[0002] Thermally conductive heat dissipation films are currently widely used in many fields, including electronics, communications, aviation, and defense and military industries. Among them, graphene heat dissipation films are widely used due to their advantages such as high thermal conductivity, light weight, and small size, and are quickly replacing traditional materials.

[0003] The current mainstream manufacturing method of graphene heat dissipation film is the coating heat treatment method. The process flow of the coating heat treatment method includes the steps of slurry preparation, coating, removal of foreign matter, heat treatment, rolling, etc., and then cutting into sheets and carrying out subsequent processing. However, this manufacturing process is not continuous and can only produce graphene sheets, so the subsequent die-cutting costs are high, the production process is complicated, the labor costs are high, and the demand for industrial automation production cannot be met, which is disadvantageous to the popularization of graphene heat dissipation film.

[0004] Based on the above current situation, a continuous manufacturing process for graphene heat dissipation film suitable for industrial production needs to be optimized. Summary of the Invention [Problem to be solved by the invention]

[0005] The present invention provides a new graphene heat dissipation film coil material manufacturing process to address the defects existing in the prior art, such as the graphene heat dissipation film manufacturing process can only produce graphene sheets, resulting in high subsequent die-cutting costs, complicated production processes, high labor costs, and inability to meet the demands of industrialized automated production. [Means for solving the problem]

[0006] In order to solve the above technical problems, the present invention is achieved by the following technical solutions.

[0007] A manufacturing process for a graphene heat dissipation film coil material, comprising: Step S1 of dispersing the graphene oxide cake in deionized water to prepare a 3 wt% to 6 wt% graphene oxide dispersion; Step S2 of slowly injecting ammonia water into the graphene oxide dispersion until the pH value of the graphene oxide dispersion becomes 6 to 10, and then performing homogenization and degassing treatment to obtain a graphene oxide slurry having a particle size controlled in the range of 0.5 μm to 3 μm and a viscosity of 15000 to 60000 Pa / s; A step S3 of preparing a substrate, applying the graphene oxide slurry onto the substrate with a coater while controlling the coating thickness to 0.1 to 0.5 mm, drying the substrate in an environment of 40 to 85° C., and then performing peeling and slitting to obtain a pretreated graphene film, and winding the pretreated graphene film with a winding mechanism while controlling the winding rotation speed to 0.5 to 2.5 m / min and the winding tension to 20 to 200 N to form a tight pretreated graphene film tight coil material; Step S4 of placing the pretreated graphene film tight coil material in a rewinding mechanism, controlling the rotation speed of the rewinding mechanism to less than 30 m / min and the winding tension to 30 N or less to perform an rewinding process, thereby obtaining a pretreated graphene film loose coil material having a predetermined tension; Step S5: subjecting the pretreated graphene film loose coil material to low-temperature treatment in an environment of 200°C to 450°C for 12 to 200 hours, then subjecting it to carbonization treatment in an environment of 1400°C or less for 10 to 50 hours, and finally subjecting it to graphitization treatment in an environment of 3200°C or less for 10 to 50 hours to obtain a graphene foam film coil material; and step S6 of subjecting the graphene foam film coil material to single-layer roll pressing or multi-layer roll pressing by the action of a pressing roll with a pressure of 1 T to 5 T to obtain a graphene heat dissipation coil material having a thermal conductivity of 800 to 2000 w·m / K.

[0008] In step S1, the weight percentage of the graphene oxide dispersion is controlled to facilitate controlling the subsequent viscosity.

[0009] In step S2, when the pH value of the graphene oxide dispersion exceeds 11, the graphene oxide GO is easily reduced, resulting in aggregation. Therefore, in the present invention, the pH value is adjusted to a range of 6 to 10 by adding ammonia water to negatively charge the graphene oxide, and by combining this with homogenization and degassing treatment, the dispersion effect of the graphene oxide dispersion can be effectively enhanced.

[0010] In addition, the homogenization treatment crushes large particles in the graphene oxide dispersion into small particles, resulting in a graphene oxide dispersion with a uniform particle size and good dispersion effect, which is also advantageous for improving the stability of the product.

[0011] In step S4, the graphene film dissipates heat and releases a large amount of gas while expanding during the high-temperature treatment, and the unwinding process creates a suitable gap between adjacent film layers of the pre-treated graphene film loose coil material, which is advantageous for improving heat dissipation and breathability.

[0012] In step S5, low-temperature treatment can remove water and most oxygen-containing functional groups and prevent explosion, and carbonization and graphitization can improve thermal conductivity (thermal diffusion coefficient).

[0013] In step S6, the roll press can increase the density of the graphene heat dissipation coil material and improve its thermal conductivity.

[0014] The manufacturing process of the present invention can produce a graphene heat dissipation film coil material with stable continuous dispersion, and the process stability is good, and the production efficiency is significantly improved and the cost is reduced.

[0015] Preferably, in the manufacturing process of the graphene heat dissipation film coil material described above, in step S4, a coating pre-lamination process is performed using a pre-lamination mechanism before performing a rewinding process on the pre-treated graphene film tight coil material, the pre-lamination mechanism including a pay-out roll group, an adhesive containing tube group, and a take-up roll, and the coating pre-lamination process step includes step S4-1 of attaching a plurality of pre-treated graphene film tight coil materials to the pay-out roll group, setting the rotation speed of the pay-out roll group to 1 to 5 m / min, setting the rotation speed of the take-up roll to 1 to 5 m / min, and controlling the winding tension to 5 to 500 N; and step S4-2 of putting an adhesive into an adhesive containing tube group, uniformly applying the adhesive to the surface of the pretreated graphene film tight coil material in the adhesive containing tube group to form an adhesive layer, and then drying the adhesive layer in an environment of 20 to 60° C. for 3 to 48 minutes to make the dry thickness of the adhesive layer 2 to 20 μm.

[0016] In order to produce thicker graphene coil material and avoid layer separation during rolling, In step S4-1, the pre-lamination mechanism can rapidly increase the thickness of the coil material by laminating multiple pre-treated graphene film tight coil materials.

[0017] In step S4-2, multiple pre-treated graphene film tight coil materials are adhered together with an adhesive to increase the thickness and prevent layer separation.

[0018] Preferably, in the above-mentioned manufacturing process of the graphene heat dissipation film coil material, the adhesive includes one or more of epoxy resin, phenol resin, acrylic resin, polyvinyl alcohol resin, polyethylene glycol aqueous resin, and polyurethane resin.

[0019] In the present invention, the adhesive manufactured using the above-mentioned materials has excellent adhesion effect, and ensures the adhesion effect of the pretreated graphene film tight coil material.

[0020] Preferably, in the above-mentioned graphene heat dissipation film coil material manufacturing process, a hole-making process is performed on the pretreated graphene film tight coil material after the coating pre-lamination process, and the pretreated graphene film tight coil material is provided with microholes having a hole diameter of 10 to 500 μm at a rate of 2000 to 100000 pieces / m 2 Open with a distribution density of .

[0021] The purpose of the hole-forming treatment on the pre-treated graphene film tight coil material is to facilitate the release of gases such as water and carbon dioxide during high-temperature treatment, to uniformly foam the film material, and to facilitate degassing during the subsequent rolling.

[0022] Preferably, in the above-mentioned manufacturing process of the graphene heat dissipation film coil material, the pretreated graphene film tight coil material that has been subjected to the hole-forming treatment is cured in an environment of 50° C. to 150° C. for 3 to 10 hours.

[0023] The curing process can sufficiently dry the pre-lamination adhesive and remove some water and oxygen-containing functional groups to prevent explosion during high-temperature processing.

[0024] Preferably, in the manufacturing process of the graphene heat dissipation film coil material described above, in step S6, a post-lamination roll press mechanism is used for the multi-layer roll press, and the post-lamination roll press mechanism includes 2 to 5 pulling rolls and a winding round roll, the rotation speed of the pulling roll is set to 1 to 5 m / min, the rotation speed of the winding round roll is set to 1 to 5 m / min, and the winding tension is controlled to 5 to 200 N.

[0025] The post-lamination roll press can produce graphene thermal conductive films of various thicknesses by rolling and integrating multiple layers of graphene films.

[0026] Preferably, in the above-mentioned manufacturing process for the graphene heat dissipation film coil material, the pretreated graphene film tight coil material has a width of 10 cm to 70 cm and a length of 30 m to 200 m.

[0027] Preferably, in the above-mentioned manufacturing process for the graphene heat dissipation film coil material, a gap D between adjacent film layers in the pretreated graphene film loose coil material is 2 to 9 times the film layer thickness.

[0028] In the pre-treated graphene film loose coil material, if the gap D is too small, it is difficult to dissipate heat and release gas, and explosions are likely to occur; if the gap D is too large, the amount of material loaded at high temperatures will be greatly reduced, and the cost will increase; therefore, the above parameters used in the present invention are suitable for industrial mass production.

[0029] Preferably, in the above-mentioned manufacturing process of the graphene heat dissipation film coil material, in the homogenization treatment of step S2, the homogenization pressure is 30 to 150 MPa, and the temperature is controlled to 10° C. to 50° C., and in the degassing treatment, the degree of vacuum is maintained at 1 KPa to 10 KPa.

[0030] The above homogenization pressure and temperature parameters used in the homogenization process according to the present invention can more reliably control the uniformity of the particle size of the graphene oxide slurry, and can provide a graphene oxide slurry with a particle size of 0.5 μm to 3 μm, which is advantageous in providing optimal thermal conductivity to the final manufactured product.

[0031] Preferably, in the manufacturing process of the above-mentioned graphene heat dissipation film coil material, in step S6, the multi-layer roll press includes a payout section, a first precision press section, a second precision press section, a third precision press section, a fourth precision press section and a winding section, the payout section and the winding section are all equipped with a tension control unit and a tension amplifier, the first precision press section, the second precision press section, the third precision press section and the fourth precision press section are all equipped with a pressure control unit, a pressure sensor, a linear speed control unit and a speedometer, and the tension control unit, pressure control unit and linear speed control unit are all connected to a PLC central processing unit.

[0032] The multi-layer roll press can produce graphene heat dissipation film coil materials of various thicknesses, and can even produce extremely thick graphene heat dissipation film coil materials (25 μm or more). However, the thicker the coil material, the more important the pressure and speed of the roll press become, which determines the quality of the coil material.

[0033] The multi-stage roll press is divided into the first, second, third and fourth precision press sections, which can not only fully degas the graphene foam coil material, but also effectively improve the density of the coil material and significantly increase the thermal conductivity. The multi-stage roll press can also improve the automation efficiency, facilitate continuous production and increase efficiency. [Brief description of the drawings]

[0034] [Figure 1] FIG. 2 is a schematic diagram showing the structure of a pretreated graphene film tight coil material according to the present invention. [Diagram 2] FIG. 2 is a schematic diagram of the structure of a pretreated graphene film loose coil material in the present invention. [Diagram 3] FIG. 2 is a structural schematic diagram of a pre-lamination mechanism in the present invention. [Figure 4] FIG. 2 is a structural schematic diagram of a post-lamination roll press mechanism in the present invention. [Diagram 5] 1 is a flowchart of a multi-layer roll press according to the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0035] The present invention will be described in further detail below with reference to FIGS. 1 to 5 and specific embodiments, but the present invention is not limited thereto. EXAMPLES

[0036] The manufacturing process of the graphene heat dissipation film coil material includes the following steps S1 to S6.

[0037] S1: Disperse the graphene oxide cake in deionized water to prepare a 3 wt% graphene oxide dispersion.

[0038] S2: Ammonia water is slowly injected into the graphene oxide dispersion until the pH value of the graphene oxide dispersion reaches 6, and then homogenization and degassing treatment are performed to obtain a graphene oxide slurry with a particle size controlled in the range of 0.5 μm to 3 μm and a viscosity of 15,000 Pa / s.

[0039] S3: Prepare a substrate, coat the graphene oxide slurry onto the substrate using a coater while controlling the coating thickness to 0.1 mm, then dry in an environment of 40°C, and then perform peeling and slitting to obtain a pretreated graphene film. The pretreated graphene film is wound up using a winding mechanism while controlling the winding speed to 0.5 m / min and the winding tension to 20 N, to form a tight pretreated graphene film tight coil material 1.

[0040] S4: The pretreated graphene film tight coil material 1 is placed in a rewinding mechanism, and an rewinding process is performed by controlling the rotation speed of the rewinding mechanism to less than 30 m / min and the winding tension to 30 N or less, to obtain a pretreated graphene film loose coil material 2 having a predetermined tension.

[0041] S5: The pretreated graphene film loose coil material 2 is subjected to low-temperature treatment in an environment of 200°C for 12 hours, then carbonized in an environment of 1400°C or less for 10 hours, and finally graphitized in an environment of 3200°C or less for 10 hours to obtain a graphene foam film coil material.

[0042] S6: The graphene foam film coil material is subjected to single-layer roll pressing or multi-layer roll pressing by the action of a pressing roll with a pressure of 1 T to obtain a graphene heat dissipation coil material with a thermal conductivity of 800 w·m / K.

[0043] Preferably, in step S4, before performing an unwinding process on the pretreated graphene film tight coil material 1, a coating pre-lamination process is performed using a pre-lamination mechanism 3, the pre-lamination mechanism 3 including a pay-out roll group 31, an adhesive containing tube group 32, and a take-up roll 33, and the coating pre-lamination process step includes the following steps S4-1 and S4-2.

[0044] S4-1: A plurality of pretreated graphene film tight coil materials 1 are attached to the unwinding roll group 31, the rotation speed of the unwinding roll group 31 is set to 1 m / min, the rotation speed of the winding roll 33 is set to 1 m / min, and the winding tension is controlled to 5 N.

[0045] S4-2: Put adhesive into the adhesive containing tube group 32, and apply the adhesive evenly to the surface of the pretreated graphene film tight coil material 1 through the adhesive containing tube group 32 to form an adhesive layer, and then dry it in an environment of 20°C for 3 minutes to make the dry thickness of the adhesive layer 2 μm.

[0046] Preferably, the adhesive comprises one or more of the following: epoxy resin, phenolic resin, acrylic resin, polyvinyl alcohol resin, polyethylene glycol water-based resin, polyurethane resin.

[0047] Preferably, the pretreated graphene film tight coil material 1 after the coating pre-lamination process is subjected to a hole-forming process, and the pretreated graphene film tight coil material 1 is provided with 2000 micropores / m having a hole diameter of 10 μm. 2 Open with a distribution density of .

[0048] Preferably, the pretreated graphene film tight coil material 1 that has been subjected to the hole-forming treatment is cured in an environment of 50° C. for 3 hours.

[0049] Preferably, in step S6, a post-lamination roll press mechanism 4 is used for the multi-layer roll press, and the post-lamination roll press mechanism 4 includes two pulling rolls 41 and a winding round roll 42, the rotation speed of the pulling roll 41 is set to 1 m / min, the rotation speed of the winding round roll 42 is set to 1 m / min, and the winding tension is controlled to 5 N.

[0050] Preferably, the pretreated graphene film tight coil material 1 has a width of 10 cm and a length of 30 m.

[0051] Preferably, the gap D between adjacent film layers in the pretreated graphene film loose coil material 2 is twice the film layer thickness.

[0052] Preferably, in the homogenization treatment in step S2, the homogenization pressure is 30 MPa, and the temperature is controlled at 10° C., and in the degassing treatment, the degree of vacuum is maintained at 1 KPa.

[0053] Preferably, in step S6, the multi-layer roll press includes a payout section, a first precision press section, a second precision press section, a third precision press section, a fourth precision press section, and a winding section, and the payout section and the winding section are all equipped with a tension control unit and a tension amplifier, and the first precision press section, the second precision press section, the third precision press section, and the fourth precision press section are all equipped with a pressure control unit, a pressure sensor, a linear speed control unit, and a speedometer, and the tension control unit, pressure control unit, and linear speed control unit are all connected to a PLC central processing unit. EXAMPLES

[0054] The manufacturing process of the graphene heat dissipation film coil material includes the following steps S1 to S6.

[0055] S1: Disperse the graphene oxide cake in deionized water to prepare a 6 wt% graphene oxide dispersion.

[0056] S2: Ammonia water is slowly injected into the graphene oxide dispersion until the pH value of the graphene oxide dispersion reaches 10, and then homogenization and degassing treatment are performed to obtain a graphene oxide slurry with a viscosity of 60,000 Pa / s and a particle size controlled in the range of 0.5 μm to 3 μm.

[0057] S3: Prepare a substrate, coat the graphene oxide slurry on the substrate with a coater while controlling the coating thickness to 0.5 mm, then dry in an environment of 85°C, and then perform peeling and slitting to obtain a pretreated graphene film. Control the winding speed to 2.5 m / min and the winding tension to 200 N and wind it up with a winding mechanism to form a tight pretreated graphene film tight coil material 1.

[0058] S4: The pretreated graphene film tight coil material 1 is placed in a rewinding mechanism, and an rewinding process is performed by controlling the rotation speed of the rewinding mechanism to less than 30 m / min and the winding tension to 30 N or less, to obtain a pretreated graphene film loose coil material 2 having a predetermined tension.

[0059] S5: The pretreated graphene film loose coil material 2 is subjected to low-temperature treatment in an environment of 450°C for 200 hours, then to carbonization treatment in an environment of 1400°C or less for 50 hours, and finally to graphitization treatment in an environment of 3200°C or less for 50 hours to obtain a graphene foam film coil material.

[0060] S6: The graphene foam coil material is subjected to single-layer roll pressing or multi-layer roll pressing by the action of a pressing roll with a pressure of 5 T to obtain a graphene heat dissipation coil material with a thermal conductivity of 2000 w·m / K.

[0061] Preferably, in step S4, before performing a rewinding process on the pretreated graphene film tight coil material 1, a coating pre-lamination process is performed using a pre-lamination mechanism 3, the pre-lamination mechanism 3 including a pay-out roll group 31, an adhesive containing tube group 32, and a take-up roll 33, and the coating pre-lamination process step includes the following steps S4-1 and S4-1.

[0062] S4-1: A plurality of pretreated graphene film tight coil materials 1 are attached to the unwinding roll group 31, the rotation speed of the unwinding roll group 31 is set to 5 m / min, the rotation speed of the winding roll 33 is set to 5 m / min, and the winding tension is controlled to 500 N.

[0063] S4-2: Put adhesive into the adhesive containing tube group 32, and apply the adhesive evenly to the surface of the pretreated graphene film tight coil material 1 through the adhesive containing tube group 32 to form an adhesive layer, and then dry it in an environment of 60°C for 48 minutes to make the dry thickness of the adhesive layer 20 μm.

[0064] Preferably, the adhesive comprises one or more of the following: epoxy resin, phenolic resin, acrylic resin, polyvinyl alcohol resin, polyethylene glycol water-based resin, polyurethane resin.

[0065] Preferably, the pretreated graphene film tight coil material 1 after the coating pre-lamination process is subjected to a hole-forming process, and the pretreated graphene film tight coil material 1 is provided with microholes having a hole diameter of 500 μm at a rate of 100,000 pieces / m 2 Open with a distribution density of .

[0066] Preferably, the pretreated graphene film tight coil material 1 that has been subjected to the hole-forming treatment is cured in an environment of 150° C. for 10 hours.

[0067] Preferably, in step S6, a post-lamination roll press mechanism 4 is used for the multi-layer roll press, and the post-lamination roll press mechanism 4 includes five pulling rolls 41 and a winding round roll 42, the rotation speed of the pulling roll 41 is set to 5 m / min, the rotation speed of the winding round roll 42 is set to 5 m / min, and the winding tension is controlled to 200 N.

[0068] Preferably, the pretreated graphene film tight coil material 1 has a width of 70 cm and a length of 200 m.

[0069] Preferably, the gap D between adjacent film layers in the pretreated graphene film loose coil material 2 is 9 times the film layer thickness.

[0070] Preferably, in the homogenization treatment in step S2, the homogenization pressure is 150 MPa and the temperature is controlled at 50° C., and in the degassing treatment, the degree of vacuum is maintained at 10 KPa.

[0071] Preferably, in step S6, the multi-layer roll press includes a payout section, a first precision press section, a second precision press section, a third precision press section, a fourth precision press section, and a winding section, and the payout section and the winding section are all equipped with a tension control unit and a tension amplifier, and the first precision press section, the second precision press section, the third precision press section, and the fourth precision press section are all equipped with a pressure control unit, a pressure sensor, a linear speed control unit, and a speedometer, and the tension control unit, pressure control unit, and linear speed control unit are all connected to a PLC central processing unit. EXAMPLES

[0072] The manufacturing process of the graphene heat dissipation film coil material includes the following steps S1 to S6.

[0073] S1: Disperse the graphene oxide cake in deionized water to prepare a 4 wt% graphene oxide dispersion.

[0074] S2: Ammonia water is slowly injected into the graphene oxide dispersion until the pH value of the graphene oxide dispersion reaches 8, and then homogenization and degassing treatment are performed to obtain a graphene oxide slurry with a particle size controlled in the range of 0.5 μm to 3 μm and a viscosity of 35,000 Pa / s.

[0075] S3: Prepare a substrate, coat the graphene oxide slurry on the substrate with a coater while controlling the coating thickness to 0.3 mm, then dry in an environment of 65°C, and then perform peeling and slitting to obtain a pretreated graphene film. The pretreated graphene film is wound up by a winding mechanism while controlling the winding speed to 1.5 m / min and the winding tension to 100 N to form a tight pretreated graphene film tight coil material 1.

[0076] S4: The pretreated graphene film tight coil material 1 is placed in a rewinding mechanism, and an rewinding process is performed by controlling the rotation speed of the rewinding mechanism to less than 30 m / min and the winding tension to 30 N or less, to obtain a pretreated graphene film loose coil material 2 having a predetermined tension.

[0077] S5: The pretreated graphene film loose coil material 2 is subjected to low-temperature treatment in an environment of 350°C for 100 hours, then to carbonization treatment in an environment of 1400°C or less for 30 hours, and finally to graphitization treatment in an environment of 3200°C or less for 30 hours to obtain a graphene foam film coil material.

[0078] S6: The graphene foam coil material is subjected to single-layer roll pressing or multi-layer roll pressing by the action of a pressing roll with a pressure of 3 T to obtain a graphene heat dissipation coil material with a thermal conductivity of 1400 w·m / K.

[0079] Preferably, in step S4, before performing an unwinding process on the pretreated graphene film tight coil material 1, a coating pre-lamination process is performed using a pre-lamination mechanism 3, the pre-lamination mechanism 3 including a pay-out roll group 31, an adhesive containing tube group 32, and a take-up roll 33, and the coating pre-lamination process step includes the following steps S4-1 and S4-2.

[0080] S4-1: A plurality of pretreated graphene film tight coil materials 1 are attached to the unwinding roll group 31, the rotation speed of the unwinding roll group 31 is set to 3 m / min, the rotation speed of the winding roll 33 is set to 3 m / min, and the winding tension is controlled to 250 N.

[0081] S4-2: Put adhesive into the adhesive containing tube group 32, and apply the adhesive evenly to the surface of the pretreated graphene film tight coil material 1 through the adhesive containing tube group 32 to form an adhesive layer, and then dry it in an environment of 40°C for 30 minutes to make the dry thickness of the adhesive layer 10 μm.

[0082] Preferably, the adhesive comprises one or more of the following: epoxy resin, phenolic resin, acrylic resin, polyvinyl alcohol resin, polyethylene glycol water-based resin, polyurethane resin.

[0083] Preferably, the pretreated graphene film tight coil material 1 after the coating pre-lamination process is subjected to a hole-forming process, and the pretreated graphene film tight coil material 1 is provided with 50,000 micropores having a hole diameter of 300 μm per m. 2 Open with a distribution density of .

[0084] Preferably, the pretreated graphene film tight coil material 1 that has been subjected to the hole-forming treatment is cured in an environment of 100° C. for 6 hours.

[0085] Preferably, in step S6, a post-lamination roll press mechanism 4 is used for the multi-layer roll press, and the post-lamination roll press mechanism 4 includes three pulling rolls 41 and a winding round roll 42, the rotation speed of the pulling roll 41 is set to 3 m / min, the rotation speed of the winding round roll 42 is set to 3 m / min, and the winding tension is controlled to 100 N.

[0086] Preferably, the pretreated graphene film tight coil material 1 has a width of 40 cm and a length of 100 m.

[0087] Preferably, the gap D between adjacent film layers in the pretreated graphene film loose coil material 2 is 5 times the film layer thickness.

[0088] Preferably, in the homogenization treatment in step S2, the homogenization pressure is 90 MPa and the temperature is controlled at 30° C., and in the degassing treatment, the degree of vacuum is maintained at 5 KPa.

[0089] Preferably, in step S6, the multi-layer roll press includes a payout section, a first precision press section, a second precision press section, a third precision press section, a fourth precision press section, and a winding section, and the payout section and the winding section are all equipped with a tension control unit and a tension amplifier, and the first precision press section, the second precision press section, the third precision press section, and the fourth precision press section are all equipped with a pressure control unit, a pressure sensor, a linear speed control unit, and a speedometer, and the tension control unit, pressure control unit, and linear speed control unit are all connected to a PLC central processing unit.

[0090] In short, the above are merely preferred embodiments of the present invention, and equivalent changes and modifications made based on the scope of the patent application of the present invention should be included in the scope of the present invention.

Claims

1. A manufacturing process for a graphene heat dissipation film coil material, comprising: Step S1 of dispersing the graphene oxide cake in deionized water to prepare a 3 wt% to 6 wt% graphene oxide dispersion; Step S2 of slowly injecting ammonia water into the graphene oxide dispersion until the pH value of the graphene oxide dispersion reaches 6 to 10, and then performing homogenization and degassing treatment to obtain a graphene oxide slurry having a particle size controlled in the range of 0.5 μm to 3 μm and a viscosity of 15,000 to 60,000 Pa / s; A step S3 of preparing a substrate, applying the graphene oxide slurry onto the substrate with a coater while controlling the coating thickness to 0.1 to 0.5 mm, drying the substrate in an environment of 40 to 85° C., and then performing peeling and slitting to obtain a pretreated graphene film, and winding the pretreated graphene film with a winding mechanism while controlling the winding rotation speed to 0.5 to 2.5 m / min and the winding tension to 20 to 200 N to form a tight pretreated graphene film tight coil material (1); Step S4: placing the pretreated graphene film tight coil material (1) into a rewinding mechanism, and performing an rewinding process by controlling the rotation speed of the rewinding mechanism to less than 30 m / min and the winding tension to 30 N or less to obtain a pretreated graphene film loose coil material (2) having a predetermined tension; Step S5 of subjecting the pretreated graphene film loose coil material (2) to low-temperature treatment in an environment of 200 ° C. to 450 ° C. for 12 to 200 hours, then carbonizing treatment in an environment of 1400 ° C. or less for 10 to 50 hours, and finally graphitizing treatment in an environment of 3200 ° C. or less for 10 to 50 hours to obtain a graphene foam film coil material; and step S6 of subjecting the graphene foam film coil material to single-layer roll pressing or multi-layer roll pressing by the action of a pressing roll at a pressure of 1 T to 5 T to obtain a graphene heat-dissipating coil material having a thermal conductivity of 800 to 2000 W m / K.

2. In step S4, before performing a rewinding process on the pretreated graphene film tight coil material (1), a coating pre-lamination process is performed using a pre-lamination mechanism (3), the pre-lamination mechanism (3) including a pay-out roll group (31), an adhesive containing tube group (32), and a take-up roll (33), and the coating pre-lamination process step includes step S4-1 of attaching a plurality of pretreated graphene film tight coil materials (1) to the pay-out roll group (31), setting the rotation speed of the pay-out roll group (31) to 1 to 5 m / min, setting the rotation speed of the take-up roll (33) to 1 to 5 m / min, and controlling the winding tension to 5 to 500 N; and step S4-2 of putting adhesive into an adhesive containing tube group (32), uniformly applying the adhesive to the surface of the pretreated graphene film tight coil material (1) through the adhesive containing tube group (32) to form an adhesive layer, and then drying the adhesive layer in an environment of 20 to 60° C. for 3 to 48 minutes to make the dry thickness of the adhesive layer 2 to 20 μm.

3. 3. The manufacturing process for a graphene heat dissipation film coil material according to claim 2, wherein the adhesive comprises one or more of an epoxy resin, a phenolic resin, an acrylic resin, a polyvinyl alcohol resin, a polyethylene glycol aqueous resin, and a polyurethane resin.

4. The pretreated graphene film tight coil material (1) after the coating pre-lamination process is subjected to a hole-making process, and microholes having a hole diameter of 10 to 500 μm are formed in the pretreated graphene film tight coil material (1) at a rate of 2,000 to 100,000 pcs / m. 2 The manufacturing process of the graphene heat dissipation film coil material according to claim 2, characterized in that the opening is made with a distribution density of 0.01 mm or more.

5. The manufacturing process for graphene heat dissipation film coil material according to claim 4, characterized in that the pretreated graphene film tight coil material (1) that has been subjected to the hole drilling treatment is cured in an environment of 50 ° C to 150 ° C for 3 to 10 h.

6. 2. The manufacturing process of the graphene heat dissipation film coil material according to claim 1, characterized in that in step S6, a post-lamination roll press mechanism (4) is used for the multi-layer roll press, the post-lamination roll press mechanism (4) includes 2 to 5 pulling rolls (41) and a winding round roll (42), the rotation speed of the pulling roll (41) is set to 1 to 5 m / min, the rotation speed of the winding round roll (42) is set to 1 to 5 m / min, and the winding tension is controlled to 5 to 200 N.

7. The pretreated graphene film tight coil material (1) has a width of 10 cm to 70 cm and a length of 3 The manufacturing process for the graphene heat dissipation film coil material according to claim 1, characterized in that the length is 0 m to 200 m.

8. The manufacturing process of the graphene heat dissipation film coil material according to claim 1, characterized in that the gap D of adjacent film layers in the pretreated graphene film loose coil material (2) is 2 to 9 times the thickness of the film layer.

9. The manufacturing process of the graphene heat dissipation film coil material according to claim 1, characterized in that in the homogenization treatment of step S2, the homogenization pressure is 30 to 150 MPa, and the temperature is controlled to 10 ° C. to 50 ° C., and in the degassing treatment, the degree of vacuum is maintained at 1 KPa to 10 KPa.

10. 2. The manufacturing process of graphene heat dissipation film coil material according to claim 1, wherein in step S6, the multi-roll press includes a payout section, a first precision press section, a second precision press section, a third precision press section, a fourth precision press section and a winding section, the payout section and the winding section are all provided with a tension control unit and a tension amplifier, the first precision press section, the second precision press section, the third precision press section and the fourth precision press section are all provided with a pressure control unit, a pressure sensor, a linear speed control unit and a speedometer, and the tension control unit, the pressure control unit and the linear speed control unit are all connected to a PLC central processing unit.

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