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Method for preparing thin layer graphene on surface of metal catalyst

A technology of metal catalyst and thin-layer graphene, which is applied in the direction of metal material coating process, coating, gaseous chemical plating, etc., can solve the problems of controllability and uniformity of high-quality graphene film layers, etc. Achieve the effect of reducing carbon content, simple process and promoting segregation

Inactive Publication Date: 2014-02-12
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these current segregation methods have not solved the problem of the controllability and uniformity of the number of layers of large-area high-quality graphene films grown on the surface of metal catalysts.

Method used

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  • Method for preparing thin layer graphene on surface of metal catalyst
  • Method for preparing thin layer graphene on surface of metal catalyst
  • Method for preparing thin layer graphene on surface of metal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1 The method for preparing thin-layer graphene comprises the steps:

[0055] (1) Thin film deposition of any of the catalysts Ni, Fe, Co and CuNi alloys: using magnetron sputtering on SiO 2 / Si wafer is coated with a catalyst film with a thickness of 270 nm;

[0056] (2) Carburizing: During the carburizing process, the conventional CVD method is used to introduce CH 4 (20 sccm) + H 2 (100 sccm) + Ar(100 sccm) mixed gas;

[0057] (3) Hydrogen etching: the sample was slowly heated to 970 °C for hydrogen etching (flow rate of 550 sccm). During the single hydrogen etching process, the original disordered graphene film or the first Removal of graphene formed at metal catalyst grain boundaries during one-step CVD process;

[0058] (4) Graphene segregation growth: After hydrogen etching, argon gas (600 sccm) was passed through the quartz tube for 2 minutes to exhaust the hydrogen, and then the sample was rapidly cooled to room temperature, and segregated graphene...

Embodiment 2

[0059] Example 2 The method for preparing thin-layer graphene comprises the steps:

[0060] (1) Deposition of any one or several alloy films of catalysts Ni, Fe, Co, Cu, Pt, Ru: use electron beam evaporation to coat a catalyst film with a thickness of 300 nm on the MgO substrate;

[0061] (2) Gas carburization: C is introduced into PECVD during carburization 2 h 2 (20 sccm) + H 2 (30 sccm) + Ar(30 sccm) mixed gas;

[0062] (3) Plasma etching: the sample was slowly heated (up to 1080 °C) for hydrogen plasma etching (flow rate of 500 sccm). Removal of nascent disordered carbon layers on the surface of the metal catalyst or graphene formed at the grain boundaries of the metal catalyst during the first PECVD process in a separate plasma etching process;

[0063] (4) Graphene segregation growth: After hydrogen etching, argon gas (400 sccm) was passed through the quartz tube for 2 minutes to exhaust the hydrogen, and then the sample was rapidly cooled to room temperature, and...

Embodiment 3

[0064] Example 3 The method for preparing thin-layer graphene comprises the steps:

[0065] (1) Catalyst Pt, Ru, Co and CuNi alloy film deposition: using thermal evaporation on SiO 2 The substrate is coated with a catalyst film with a thickness of 650 nm;

[0066] (2) Solid carburizing: PMMA, PVP, PVA, PE, sugar, activated carbon, amorphous carbon, acetylene black, carbon black. Moreover, the solid carbon source can be evenly distributed on the surface of the catalyst in the form of solution and powder, with a thickness of 1 mm;

[0067] (3) Etching: The sample was slowly heated to 1080 °C for hydrogen etching (flow rate of 500 sccm). Removal of the original disordered graphene film on the surface of the metal catalyst or the graphene formed at the grain boundary of the metal catalyst during the first step of CVD in a separate hydrogen etching process;

[0068] (4) Graphene segregation growth: After hydrogen etching, argon gas (600 sccm) was passed through the quartz tube...

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Abstract

The invention discloses a method for preparing thin layer graphene on the surface of a metal catalyst. The method comprises the following steps: 1, putting a metal catalyst matrix in a chemical vapor deposition (CVD) system, and heating and annealing in an H2 and Ar gas mixed atmosphere; 2, carrying out a high temperature carburizing reaction by utilizing different carbon sources; 3, slowly heating samples while etching by introducing a large flow of hydrogen; and 4, completely discharging hydrogen in the CVD system through the Ar gas after the hydrogen etching, and rapidly cooling to room temperature for segregating uniform graphene layers. The number of the graphene layer can be accurately controlled by changing the thickness, the carburizing amount and the hydrogen etching amount of the metal catalyst matrix. The method has the advantages of simple process, easy operation, compatibility with the semiconductor industry, realization of the controllable preparation of graphene, and a graphene material produced through the method has important application prospects in the electronic field, the photoelectric field, the sensing field and the like.

Description

technical field [0001] The invention relates to a preparation method of a graphene material, in particular to a method for preparing wafer-sized graphene with a controllable layer number and uniform thickness by segregating and growing on the surface of a metal catalyst. Background technique [0002] Graphene is a carbon atom with SP 2 A two-dimensional monoatomic layer of a hexagonal crystal structure formed by bonds. Due to its unique structure and excellent physical properties, graphene has received extensive attention from the scientific community. In recent years, some researchers have developed a chemical vapor deposition (CVD) synthesis of graphene technology using Cu or Ni as a catalyst, which has shown great advantages in large-scale synthesis of nearly perfect graphene. Since graphene with different layers has different properties and corresponding applications, it is the goal pursued by researchers to realize the layer number controllable growth and process comp...

Claims

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Application Information

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IPC IPC(8): C23C16/26C23C16/52C23C16/02
Inventor 刘立伟龚佑品张学敏高嵩朱超龙明生耿秀梅
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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