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Preparation method of high-thermal-conductivity self-supporting vertically oriented graphene film

A graphene thin film, vertical orientation technology, applied in the direction of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of low production efficiency, insufficient thermal conductivity, and difficulty in self-supporting of thermal conductive films, and achieve controllable deposition thickness, Effect of lower surface energy and excellent thermal conductivity

Inactive Publication Date: 2021-07-23
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the existing problems of complex preparation process of vertically oriented graphene, high equipment requirements, and low production efficiency, the present invention provides a method for preparing a self-supporting vertically oriented graphene film with high thermal conductivity, which solves the problem of the existing graphene heat-conducting film production. Low efficiency, insufficient thermal conductivity, high cost, and difficulty in self-support, which limit its application and commercialization in the field of high thermal conductivity to a certain extent

Method used

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  • Preparation method of high-thermal-conductivity self-supporting vertically oriented graphene film

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Embodiment 1

[0033] Graphene oxide (Graphene Oxide, GO) dispersion with a concentration of 10 mg / mL was prepared by the improved Hummers method: under ice bath conditions (0-4 °C), 1 g of graphite powder and 1 g of NaNO 3 into the beaker, followed by the addition of 46 mL of concentrated sulfuric acid H 2 SO 4 (≥98wt%) Stirring was continued for 10 minutes. Slowly add 6g KMnO 4 After stirring for 10 minutes, the ice bath was removed, and the above mixed solution was transferred to an oil bath at 35° C. and stirred for 10 hours. Then slowly add 80 mL of deionized water, and then heat to 80 ° C for 30 minutes, then add 200 mL of deionized water and keep stirring, and finally add 6 mL of H 2 o 2 (30wt%). The above mixed solution was washed with HCl (5wt%) and deionized water respectively, and centrifuged (6000r / min) until the pH was 3–4 to obtain the GO dispersion.

[0034] Preparation of modified single-walled carbon nanotubes: first prepare 50 mL of CTAB aqueous solution with a mass f...

Embodiment 2

[0037] Adopt the Hummers method improved Hummers method preparation concentration of embodiment 1 to be the GO dispersion liquid of 15mg / mL, get 4mL GO solution, add dodecylsulfonic acid 12mg, the modified single-walled carbon nanotube 3mg that embodiment 1 makes wherein, 0.6 mg of hexapolyethylene glycol monododecyl ether was stirred with magnetic force at 1000 rpm for 24 hours, then ultrasonically (power of 200 W, ultrasonic frequency of 50 Hz) for 5 hours and then thoroughly mixed and used as an electrodeposition solution. A 0.2T magnetic field was applied at both ends of the vertical electrodes, a copper foil (15 μm thick) was used as the working electrode, and a platinum sheet was used as the counter electrode, and a constant voltage of 3.0V was applied for 2 hours through the electrochemical workstation. Subsequently, the copper foil loaded with vertical graphene oxide was frozen in a low-temperature refrigerator at -20°C for 12 hours, then freeze-dried at -55°C for 24 ho...

Embodiment 3

[0039] Adopt the Hummers method improved Hummers method of embodiment 1 to prepare the GO dispersion liquid that concentration is 20mg / mL, get 2.5mL GO solution, add the modified single-walled carbon nanotube 12.5 that dodecylsulfonic acid 50mg, embodiment 1 make wherein mg, lauryl polyoxyethylene ether 1.25mg, with a rotating speed of 2000rpm, magnetically stirred for 12 hours; then ultrasonic (power 200W, ultrasonic frequency 50Hz) for 5 hours and fully mixed to serve as electrodeposition solution. Apply a 0.4T magnetic field at both ends of the vertical electrodes, use copper foil (thickness 15 μm) as the working electrode, and a platinum sheet as the counter electrode, and apply a constant voltage of 4.0V for 2 hours through the electrochemical workstation. Subsequently, the copper foil loaded with vertical graphene oxide was frozen in a low-temperature refrigerator at -25°C for 12 hours, then freeze-dried at -55°C for 24 hours, and then placed in 1mol / L K 2 S 2 o 8 Etch...

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Abstract

A preparation method of a high-thermal-conductivity self-supporting vertically oriented graphene film comprises the following steps: 1) preparing a graphene oxide dispersion liquid; 2) adding long-chain alkyl sulfonic acid, modified single-walled carbon nanotubes and a nonionic surfactant into the graphene oxide dispersion liquid, stirring, and carrying out ultrasonic treatment; 3) under the action of an external magnetic field, taking the mixed solution as an electro-deposition solution, and depositing graphene oxide by adopting an electrochemical deposition method; 4) freezing, freeze-drying, corroding off the substrate, and graphitizing to obtain a vertically oriented graphene film; and 5) pressing the film. The vertically oriented graphene film layer obtained by the invention can effectively accelerate longitudinal heat conduction and has excellent heat conductivity; and by adding long-chain alkyl sulfonic acid into the electrochemical deposition liquid, the surface energy of graphene oxide is effectively reduced, graphene can be vertically arranged, meanwhile, the film deposition thickness is controllable, the thermal conductivity is remarkably improved, and large-scale production is easy to achieve.

Description

technical field [0001] The invention relates to a surface vertically oriented graphene film with high thermal conductivity, in particular to a preparation method for a self-supporting vertically oriented graphene film with high thermal conductivity. Background technique [0002] As a new type of two-dimensional material, graphene's unique single graphite atomic layer structure endows it with ultra-high mechanical strength, excellent electrical conductivity, and good chemical and thermodynamic stability. A lot of research and application. High thermal conductivity graphene is a new type of heat-conducting and heat-dissipating material, which can conduct heat in the horizontal and vertical directions, and has the characteristics of good thermal conductivity, low thermal resistance, and light weight. With the development of electronic equipment in the direction of high power and high power consumption, heat dissipation has become an urgent problem to be solved in electronic pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01B32/194
CPCC01B32/184C01B32/194C01B2204/24
Inventor 杨凯胡磊朱宇灿万中全贾春阳
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA