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Method for synthesizing graphene by catalyzing solid carbon source with two-stage process at normal pressure

A solid carbon source and synthetic graphite technology, which is applied in the field of graphene synthesis by CVD, can solve the problems of high energy consumption, unsuitability for industrial production, and high equipment requirements, and achieve the effects of low energy consumption, low cost, and high quality

Inactive Publication Date: 2015-05-13
CHONGQING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in most technologies that use amorphous carbon as a carbon source to synthesize graphene, the high vacuum conditions required in the reaction process require high equipment and high energy consumption, and are not suitable for large-scale industrial production.

Method used

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  • Method for synthesizing graphene by catalyzing solid carbon source with two-stage process at normal pressure
  • Method for synthesizing graphene by catalyzing solid carbon source with two-stage process at normal pressure
  • Method for synthesizing graphene by catalyzing solid carbon source with two-stage process at normal pressure

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Experimental program
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Effect test

preparation example Construction

[0017] The present invention provides a kind of preparation method, the present invention is described in detail in conjunction with accompanying drawing, comprises the following steps:

[0018] (1) cleaning SiO2 2 / Si substrate and metal substrate:

[0019] ① SiO with a certain size 2 Put the / Si substrate in clean acetone and isopropanol in sequence for ultrasonic cleaning for 5 minutes, rinse with deionized water, and dry.

[0020] ②Metal substrates refer to copper foil. Put a certain size of copper foil into clean dilute acetic acid, acetone, and isopropanol in order to ultrasonically clean it for 5 minutes, rinse it with deionized water, and dry it.

[0021] (2) SiO processed in step 1) 2 The / Si substrate is placed in a magnetron sputtering apparatus, using magnetron sputtering technology, optimizing the sputtering conditions, and depositing a layer of cobalt film. A certain thickness of amorphous carbon is then sputtered on the cobalt film.

[0022] (3) SiO deposit...

example 1

[0026] Example 1: As the CVD time changes, compare the evolution of graphene films under different reaction times.

[0027] Follow steps 1) in ① and step 2) in 1cm*1cm of SiO 2 Deposit metal Co on the / Si substrate, and then deposit amorphous carbon separately for 1min; then deposit cobalt film and SiO of amorphous carbon 2 / Si sheet (amorphous carbon / cobalt film / SiO 2 / Si) and the 1cm*1cm copper foil cleaned according to the method ② in step 1) are put into the quartz tube. Exhaust the air in the reaction chamber according to step 3). incoming Ar and H 2 The numerical intervals of the flow rates are 300-600sccm and 30-80sccm respectively. The temperature in the front temperature zone is raised to 700°C, and the temperature in the back temperature zone is 1050°C. At this temperature, keep the carrier gas unchanged, and the value range of the constant temperature annealing time is 30-90min. After the amorphous carbon / cobalt film / SiO 2 / Si sheet is pushed into the central a...

example 2

[0029] Example 2: Comparison of the influence of the amount of sputtering deposition of amorphous carbon on the synthesis of graphene. Figure 5 Shown are optical micrographs and corresponding Raman spectra of graphene synthesized under the condition of sputtering amorphous carbon for different times.

[0030] Follow steps 1) in ① and step 2) in 1cm*1cm of SiO 2 Deposit metal Co on the / Si substrate, and then deposit amorphous carbon for 0.5min, 1min and 2min respectively (as shown in Figure (5a-c)); after that, deposit cobalt film and SiO of amorphous carbon 2 / Si(amorphous carbon / cobalt film / SiO 2 / Si) sheet and the 1cm*1cm copper foil cleaned according to the method ② in step 1) are put into the quartz tube. Exhaust the air in the reaction chamber according to step 3). incoming Ar and H 2 The numerical intervals of the flow rates are 300-600sccm and 30-80sccm respectively. The temperature in the front temperature zone is raised to 700°C, and the temperature in the back...

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Abstract

The invention belongs to the technical field of carbon material preparation, and relates to the field of graphene production, in particular to a novel method for synthesizing single-layer graphene with a CVD (chemical vapor deposition) method under the normal-pressure condition through a two-stage reaction process by taking a solid carbon source as a precursor and for graphene layer number control through accurate control of supply quantity of the solid carbon source. According to the method, at normal pressure and lower temperature, in a first-stage reaction process, a catalyst is used, a gas capable of reacting with the solid carbon source is introduced, and the solid carbon source is transformed into a carbon-containing gas reaction species under the action of the catalyst; in a second reaction process, the generated carbon-containing gas reaction species is absorbed on the surface of a metal catalyst through conveying of a carrier gas and under the action of the metal catalyst, and graphene is grown on the surface of the metal catalyst through chemical steps including absorption, dissolution, diffusion, precipitation and the like. Single-layer graphene is synthesized successfully with the method, and the graphene layer number can be controlled by changing the supply quantity of amorphous carbon source with the method.

Description

Technical field [0001] The invention relates to the technical field of carbon nanomaterial preparation, in particular to a new technology for synthesizing graphene by CVD under normal pressure through a two-stage reaction process using solid carbon sources as precursors. Background technique [0002] Graphene is a new type of material with a two-dimensional honeycomb structure formed by stacking a single layer of carbon atoms. Since 2004, Dr. Novoselov and Professor Geim, two scientists from the University of Manchester in the United Kingdom, successfully separated high-quality graphene that exists alone in the laboratory by mechanical exfoliation (Novoselov K S, et al.science, 2004, 306, 666.), Set off the research upsurge of graphene, along with the continuous deepening of research, new preparation method emerges in an endless stream, mainly contains micromechanical exfoliation method (Novoselov K S, et al.Science, 2004,306,666.), redox method (Stankovich S, et al. al.Car...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 胡宝山杨倩金燕方千瑞董立春
Owner CHONGQING UNIV