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Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition

A chemical vapor deposition, graphene technology, applied in graphene, gaseous chemical plating, nanotechnology for materials and surface science, etc., can solve problems such as cumbersome transfer process, restrict graphene application, defects, etc. The effect of preparation efficiency

Active Publication Date: 2012-07-18
SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both copper and nickel are metals with a melting point of over 1,000 degrees Celsius. After the growth of graphene, it is necessary to transfer graphene from the metal substrate to other substrates for device research, but this transfer process is very cumbersome, and it is easy to introduce Contamination and Defects
The complex transfer process severely restricts the application of graphene and consumes metal substrate materials
In addition, during the graphene growth process, these catalysts are in the solid state, and there is no report on the preparation of graphene by liquid catalysts by CVD technology.

Method used

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  • Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition
  • Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition
  • Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Using liquid gallium as a catalyst and solid carbon source to prepare graphene at low temperature

[0050] (1) Weigh 0.5 g of simple gallium with a purity of 99.999%, and place it on a gallium nitride substrate. Weigh 15 mg of solid carbon source naphthalene, put it in a quartz test tube with one end closed, and place it in the low-temperature heating zone of a tube furnace.

[0051] (2) Increase the temperature of the substrate, and the argon gas flow rate is 200 sccm as a protection. Simultaneously heat the carbon source to 150-200°C. When the substrate temperature reaches 500-700° C., the flow rate of hydrogen gas is 2 sccm, the flow rate of argon gas is 200 sccm, and the reaction time is 60 min.

[0052] Stop heating the liquid source and the tube furnace, and take out the sample after the chamber cools down to room temperature. The purity of the carrier gas used in the chemical gas phase reaction is higher than 99.999%.

[0053] (3) Freeze the sample...

Embodiment 2

[0055] Example 2: Using liquid gallium as a catalyst and gaseous carbon source to prepare graphene at high temperature

[0056] (1) Weigh 0.5 g of simple gallium with a purity of 99.999% and place it on an alumina substrate.

[0057] (2) The temperature of the substrate is raised with the argon flow rate of 200 sccm as a protection. When the furnace temperature rises to 1000° C., the methane flow rate is 2 sccm, the argon flow rate is 200 sccm, and the reaction time is 3 minutes. Stop heating the tube furnace, and take out the sample after cooling down to room temperature at a cooling rate greater than 30°C per second.

[0058] (3) The process of exfoliating graphene is similar to Example 1.

[0059] Example result: as Figure 4 It is shown that high-quality graphene is obtained in a short time at a higher temperature, and the 2D peak is located at 2700cm -1 Nearby, and twice the intensity of the G peak, indicating that the graphene is a single layer, and no defect peaks a...

Embodiment 3

[0060] Example 3: Using liquid gallium as a catalyst and gaseous carbon source to prepare graphene at high temperature

[0061] (1) Weigh 0.5 g of gallium elemental substance with a purity of 99.999%, and place it on a quartz substrate.

[0062] (2) The temperature of the substrate is raised with the argon flow rate of 200 sccm as a protection. When the furnace temperature rises to 1000° C., the methane flow rate is 5 sccm, the argon flow rate is 200 sccm, and the reaction time is 30 minutes. Stop heating the tube furnace and remove the sample after the chamber has cooled to room temperature.

[0063] (3) The process of exfoliating graphene is similar to Example 1.

[0064] Example result: as Figure 5 It is shown that thicker graphene is obtained at higher temperature for a longer time, and the 2D peak is located at 2700cm -1 Nearby, it is about 0.8 times the intensity of the G peak, indicating that graphene is multi-layered, and a smaller defect peak appears. Through hi...

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Abstract

The invention discloses a method for preparing a graphene film by using a liquid metal or alloy as a catalyst and adopting chemical vapor deposition. The metal with low melting point comprises typical gallium, tin, indium and the like; and the alloy with low melting point comprises gallium-copper, gallium-nickel, indium-copper, indium-nickel, tin-copper, tin-nickel, copper-silver-tin and the like. The chemical vapor deposition is performed above the melting point of the metal or alloy catalyst, so that the continuous graphene film is formed on the surface of the catalyst and the interface of the catalyst and a substrate. Compared with the graphene grown on the surface of a solid catalyst such as copper and nickel, the invention has the advantages that the prepared graphene is controllable in layer number, low in requirement for the micro morphology of the surface of the substrate and suitable for multiple substrate materials, and the catalyst is very easy to remove. The obtained graphene positioned on the surface of the liquid has unique application value.

Description

technical field [0001] The invention relates to a method for preparing graphene, in particular to a method for preparing high-quality graphene by chemical vapor deposition using liquid metal or alloy as a catalyst. Background technique [0002] Graphene is a two-dimensional honeycomb grid structure composed of carbon atoms with a thickness of a single layer or several atomic layers. The in-plane π orbitals of graphene give graphene excellent electron transport properties. Graphene has an unparalleled high electron mobility, and the transfer rate of charges in graphene can reach an unprecedented 200,000 cm 2 / vs, more than 100 times more than silicon. This advantage makes graphene very likely to replace silicon as the basic material for the next generation of ultra-high frequency transistors and is widely used in high-performance integrated circuits and new nanoelectronic devices. The application of graphene in transparent conductive films, electronic devices, and optical ...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC23C16/003C01B31/04C23C16/26B82Y30/00B82Y40/00C01B32/186
Inventor 丁古巧王庶民龚谦朱云孙雷狄增峰谢晓明江绵恒
Owner SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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