Method for preparing graphene film on metal surface

A graphene film and metal surface technology, applied in the field of graphene film preparation, can solve the problems of high cost, high electrodeposition temperature, small area, etc., and achieve the effects of controllable shape, simple process and large area

Inactive Publication Date: 2020-02-11
ARMOR ACADEMY OF CHINESE PEOPLES LIBERATION ARMY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the quality of graphene prepared by mechanical exfoliation method is high, but the area of ​​graphene obtained is less than 1×1 mm, which cannot be applied to actual production.
Although large-area graphene can be obtained by chemical vapor deposition, its cost is high and its controllability is poor
The graphite oxide reduction method can produce a large number of graphene samples, which can meet the needs of industrial production. However, the use of oxidants destroys the internal conjugated structure of the prepared graphene and greatly reduces its performance.
[0004] CN102888636A reports a method for preparing metal surface graphene by electrodeposition in carbonate and halide salt molten solution. The electrodeposition temperature of this method is higher and must be higher than the melting point of the mixed solution, which is difficult to control in actual operation. Electrodeposition equipment is demanding and difficult to apply to actual production
CN103523770 provides ion implantation of Ge into the SiC substrate, and then heat treatment to precipitate graphene, but this process cannot prepare large-area graphene, and its preparation cost is relatively high

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  • Method for preparing graphene film on metal surface
  • Method for preparing graphene film on metal surface
  • Method for preparing graphene film on metal surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Graphene film preparation method of the present invention is as follows:

[0028] (1) Configure the basic plating solution.

[0029] Main salt: NiSO 4 ·6H 2 O, content 210g / L; anode activator: NiCl 2 , content 35g / L; buffer: boric acid, content 24g / L; conductive salt: sodium chloride, content 20g / L; carbon source: lysine, content 0.25mol / L. Using 10wt% H 2 SO 4 The solution was adjusted to pH 4.

[0030] (2) Pretreatment of the base material.

[0031] The base material is H62 brass sheet.

[0032]Electro-cleaning: Electro-cleaning fluid configuration is as follows: NaOH 40g / L, NaOH 3 PO 4 160g / L, Na 2 CO 3 40g / L, NaCl 5g / L; process parameters are as follows: voltage: 10V; time: 32s.

[0033] Activation: prepare No. 3 activation solution for activation: citric acid (C 6 h 8 o 7 ·H 2 O) 140g / L, sodium citrate (C 6 h 5 Na 3 o 7 2H 2 O) 90g / L, NiCl 2 3g / L; process parameters are as follows: voltage: -20V; time: 45s.

[0034] Washing: Rinse with dei...

Embodiment 2

[0040] Graphene film preparation method of the present invention is as follows:

[0041] (1) Configure the basic plating solution.

[0042] Main salt: CuSO 4 ·6H 2 O, content 190g / L; anode activator: NiCl 2 , content 38g / L; buffer: boric acid, content 25g / L; conductive salt: sodium chloride, content 12g / L; carbon source: ascorbic acid, content 0.45mol / L. Using 10wt% H 2 SO 4 The pH of the solution was adjusted to 4.5.

[0043] (2) Pretreatment of the base material.

[0044] The base material is 304 stainless steel sheet.

[0045] Electro-cleaning: Electro-cleaning fluid configuration is as follows: NaOH 30g / L, NaOH 3 PO 4 170g / L, Na 2 CO 3 30g / L, NaCl 6g / L; process parameters are as follows: voltage: 12V; time: 28s.

[0046] Activation: Firstly prepare No. 2 activation solution for activation: HCl (36-38wt%) 25g / L, NaCl 140g / L; process parameters are as follows: voltage: -8V; time: 60s. Then prepare No. 3 activation solution for activation: citric acid (C 6 h ...

Embodiment 3

[0053] Graphene film preparation method of the present invention is as follows:

[0054] (1) Configure the basic plating solution.

[0055] Main salt: CoSO 4 ·6H 2 O, content 230g / L; anode activator: NiCl 2 , content 31g / L; buffer: boric acid, content 26g / L; conductive salt: sodium chloride, content 28g / L; carbon source: arginine, content 0.1mol / L. Using 10wt% H 2 SO 4 The solution was adjusted to pH 3.

[0056] (2) Pretreatment of the base material.

[0057] The base material is T1 titanium alloy sheet.

[0058] Electro-cleaning: Electro-cleaning fluid configuration is as follows: NaOH 50g / L, NaOH 3 PO 4 150g / L, Na 2 CO 3 50g / L, NaCl4g / L; process parameters are as follows: voltage: 8V; time: 36s.

[0059] Activation: firstly prepare No. 1 activation solution for activation, H 2 SO 4 (95~98wt%) 60g / L, (NH 4 ) 2 SO 4 115 g / L; process parameters are as follows: voltage: -10V; time: 30s. Then prepare No. 3 activation solution for activation: citric acid (C 6 ...

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Abstract

The present invention relates to a method for preparing a graphene film on a metal surface, and the method includes the steps: (1) preparing basic plating solution; (2) pretreating a substrate material; (3) conducting electrochemical deposition on M-C coatings (M is Co, Ni and Cu); and (4) annealing treatment. The method of the present invention is based on an electro-deposition and heat treatmentprocess, and has the advantages of simple process and low cost, and therefore a large-area high-quality graphene film may be prepared, and the prepared graphene film has excellent conductivity and corrosion resisting property.

Description

technical field [0001] The invention relates to a method for preparing a graphene film on a metal surface. More specifically, the present invention relates to a method for preparing a graphene film based on electrodeposition and heat treatment processes. Background technique [0002] Graphene materials have excellent thermal, electrical and mechanical properties, and can be applied to the corrosion protection of metals. Graphene consists of carbon atoms with sp 2 Composed of hybridized monoatomic layers, closely arranged in regular hexagons. As an ideal two-dimensional atomic crystal, graphene has ultra-high electrical and thermal conductivity, huge theoretical specific surface area, and extremely high Young's modulus. It is expected to be applied in a wide range of fields such as micro-nano electronic devices, photoelectric detection and conversion materials, structural and functional enhanced composite materials, and energy storage. [0003] At present, the general grap...

Claims

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Application Information

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IPC IPC(8): C25D3/56C25D5/34C25F1/04C25D5/50
CPCC25D3/56C25D5/34C25D5/50C25F1/04
Inventor 谭俊张庆唐振陈茜刘晓亭谢凤宽臧艳孟令东徐瑶瑶蔡志海
Owner ARMOR ACADEMY OF CHINESE PEOPLES LIBERATION ARMY
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