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Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film

A technology of graphene film and composite substrate, which is applied in the direction of graphene, coating, metal material coating process, etc., can solve the problems of graphene film size limitation, complicated process, high hardware investment and high preparation cost, and achieve shape and The effect of less size limitation, strong layer number control ability and wide process window

Active Publication Date: 2015-05-27
SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, thermal evaporation, magnetron sputtering and pulsed laser deposition technology hardware investment and preparation costs are high, and the size of graphene film is limited by large-scale equipment
In addition, patent 201110096201.2 only obtains a single-layer graphene film, while patent 201110266477.0 stated that "by adjusting different reaction temperatures, the spatial distribution range and concentration of carbon also change accordingly, such as the spatial distribution range and concentration of carbon at low temperatures will increase, so as the reaction temperature decreases, the number of graphene layers increases; by controlling the reaction temperature, a graphene film with a continuously adjustable number of layers can be prepared. In the process of controlling the number of layers by the reaction temperature, The interdiffusion between the two metals, the dissolution of carbon on the metal substrate, and the formation of graphene by carbon precipitation are carried out simultaneously, and these dynamic processes are closely related to the temperature of the CVD process. It is necessary to control the number and quality of graphene layers based on experimental experience. quite complicated

Method used

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  • Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film
  • Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film
  • Layer-number-controllable graphite film based on nickel-copper composite substrate and preparation method of film

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]The preparation of embodiment 1 monolayer graphene

[0040] 1. Experimental method

[0041] 1) Ni-Cu composite substrate: cut copper foil with a thickness of 25 μm, a purity of 99.8%, a width of 10 cm, and a length of 50 cm. Copper foils were cleaned with acetone and isopropanol and dried with nitrogen. A 150nm metal Ni layer was formed on the surface of Cu using industrial nickel plating process (for nickel plating method refer to electrodeposition nanocrystalline material technology, edited by Tu Zhenmi et al., National Defense Industry Press, publication date: April 1, 2008, ISBN: 9787118055528).

[0042] 2) Carburizing process: use liquid benzene as carbon source, heat to 150-200°C, base temperature is 300°C, keep for 30 minutes, Ar flow rate is 300sccm, H 2 The flow rate is 2 sccm.

[0043] 3) Carbon precipitation process: Cut off the carbon source, raise the substrate temperature to 500°C, keep it warm for 60 minutes, Ar flow rate is 300 sccm, H 2 The flow rate...

Embodiment 2

[0046] The preparation of embodiment 2 monolayer graphene

[0047] The carbon source is replaced by solid carbon sources such as phenanthrene, pyrene, polystyrene, polymethyl methacrylate to prepare the graphene film of the nickel-copper composite substrate, and other parameters are the same as embodiment 1, and the method is as follows:

[0048] method one:

[0049] 1) Ni-Cu composite substrate: cut copper foil with a thickness of 25 μm, a purity of 99.8%, a width of 10 cm, and a length of 50 cm. Copper foils were cleaned with acetone and isopropanol and dried with nitrogen. A 150nm nickel layer is formed on the surface of the copper foil using an industrial nickel plating process.

[0050] 2) Carburizing process: use phenanthrene as carbon source, weigh 0.015g phenanthrene, heat to 100-150°C, base temperature is 300°C, hold for 60 minutes, Ar flow rate is 300sccm.

[0051] 3) Carbon precipitation process: cut off the carbon source, raise the substrate temperature to 600°C...

Embodiment 3

[0068] The preparation of embodiment 3 multilayer graphene

[0069] 1. Experimental method

[0070] 1) Ni-Cu composite substrate: cut copper foil with a thickness of 25 μm, a purity of 99.9%, a width of 20 cm, and a length of 20 cm. The cut copper foils were cleaned with acetone and isopropanol and then dried with nitrogen. A 600nm nickel layer is formed on the copper foil surface using an industrial nickel plating process.

[0071] 2) Carburizing process: take Nai as carbon source, heat to 80-120°C, base temperature is 300°C, keep for 60 minutes, Ar flow rate is 300sccm, H 2 The flow rate is 2 sccm.

[0072] 3) Carbon precipitation process: the substrate temperature is raised to 650°C, kept for 20-180 minutes, the Ar flow rate is 300 sccm, the H 2 The flow rate is 1 sccm.

[0073] 2. Experimental results: Raman results show that there is carbon signal after 20 minutes of heat preservation, but there is no graphene, and double-layer graphene is formed after 40 minutes of ...

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Abstract

The invention relates to the field of graphite film preparation, and in particular relates to a layer-number-controllable graphite film based on a nickel-copper composite substrate and a preparation method of the film. The preparation method comprises the following steps of: 1) preparing the nickel-copper composite substrate; 2) carburizing, namely heating the nickel-copper composite substrate to 200-300 DEG C, then introducing a carbon source gas and a carrier gas, and carrying out heat preservation for 30-240 minutes for carburization of a nickel layer; and 3) depositing carbon, namely cutting off the supply of the carbon source gas, raising the temperature of the nickel-copper composite substrate to 300-1000 DEG C, introducing the carrier gas, and carrying out heat preservation for 10-180 minutes so as to obtain the graphite film based on the nickel-copper composite substrate. The preparation method has the beneficial effects that a novel preparation process is provided, the layer number of graphite is controlled more easily, the problem that the existing composite substrate is high in preparation cost, and a graphite film material which is low in cost, simple in preparation method, easy to control, good in product quality and large in area is obtained.

Description

technical field [0001] The invention relates to the field of graphene thin film preparation, and specifically discloses a graphene thin film material with controllable layer number based on a nickel-copper composite substrate and a preparation method thereof. Background technique [0002] Graphene film has important application value because it has good flexibility, mechanical strength and electrical conductivity. Chemical vapor deposition (Chemical Vapor Deposition, CVD) is the most cost-effective technical way to prepare graphene film. Large-area graphene films can be prepared on metal surfaces such as Cu and Ni, and can be transferred to various substrate surfaces, but it is difficult to control the number of layers of graphene on metal surfaces such as Cu and Ni. The solubility in Ni is very large (6.4 to 2.7at% at 700 to 1000°C), and multilayer graphene is easy to prepare by CVD, but the uniformity of the number of layers is poor. Due to the low solubility of carbon on...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/06C23C8/20C23C16/26C01B31/02C01B32/184
Inventor 丁古巧朱云谢晓明江绵恒
Owner SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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