Oxide-substrate-assisted method for quickly preparing large-size single-crystal graphene

A single crystal graphene, substrate-assisted technology, applied in chemical instruments and methods, single crystal growth, single crystal growth, etc., can solve the problems of long processing time, complicated procedures, increased nucleation difficulty, etc., and shorten the growth cycle , increase the growth rate, good application prospects

Active Publication Date: 2015-12-02
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the main method to obtain large-size single-crystal graphene is to reduce the nucleation points in the early stage of growth. active sites, this method has the problems of complex surface treatment process and long processing time, which greatly increases the preparation cost; second, the use of extremely low methane flow rate during the growth period increases the difficulty of nucleation, but the extremely low methane flow rate will Causes very long growing time, increases energy consumption and growing cost
Moreover, during the growth process, nucleation is a probabilistic event. As time increases during the growth process, new nuclei will inevitably form randomly, so the size of single-crystal graphene obtained by this method has a certain limit.
In the experiment, large-size graphene single crystals can be effectively obtained by combining these two methods reasonably, but the complex process, long growth cycle and high cost make it difficult to realize the industrialization of large-size single-crystal graphene

Method used

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  • Oxide-substrate-assisted method for quickly preparing large-size single-crystal graphene
  • Oxide-substrate-assisted method for quickly preparing large-size single-crystal graphene
  • Oxide-substrate-assisted method for quickly preparing large-size single-crystal graphene

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Experimental program
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Effect test

Embodiment approach 1

[0039] Embodiment 1: A method for rapid preparation of large-size single-crystal graphene assisted by an oxide substrate

[0040] This embodiment is in figure 1 In the setup shown, a metal foil is placed on top of an oxide substrate, and the metal foil is followed by the following steps:

[0041] 1. Place the metal foil without any surface treatment on the oxide substrate, put it into the chemical vapor deposition equipment, feed Ar, the flow rate is more than 300 sccm, and the working pressure is normal pressure (that is, one atmospheric pressure or about 1× 10 5 Pa), and then start to heat up, and the heating process lasts for 50 to 70 minutes;

[0042] 2. When the temperature rises to 900~1100℃, H 2 Gas, H 2 The flow rate is 2-50 sccm, the Ar flow rate remains unchanged, and the annealing process is carried out, and the annealing duration is 30-100 min;

[0043] 3. After the annealing is over, start to introduce CH 4 gas, CH 4 The flow rate is 0.5~5sccm, adjust the H...

Embodiment approach 2

[0108] Embodiment 2: Influence of methane flow rate and growth time in an oxide substrate-assisted rapid preparation method of large-size single-crystal graphene

[0109] Experiment 1: A low-cost and fast method for preparing large-scale single-crystal graphene in this experiment is carried out according to the following steps:

[0110] 1. Place the metal copper foil without any surface treatment on Al 2 o 3 On the substrate, put it into the chemical vapor deposition equipment, feed Ar, the flow rate is 500 sccm, and the working pressure is 1×10 5 Pa, then start to heat up, and the heating process lasts for 60 minutes;

[0111] 2. When the temperature rises to 1000°C, H 2 Gas, H 2 The flow rate is 2sccm, the Ar flow rate is kept constant, and the annealing process is carried out, and the annealing duration is 40min;

[0112] 3. After the annealing is over, start to introduce CH 4 gas, CH 4 The flow rate is 0.5sccm, H 2 and Ar flow remain unchanged, the working pressure...

Embodiment approach 3

[0122] Embodiment 3: Influence of hydrogen gas flow in an oxide substrate-assisted rapid preparation of large-size single-crystal graphene

[0123] A kind of oxide substrate assisted rapid preparation method of large-scale single-crystal graphene of this experiment is to carry out as follows:

[0124] 1. Place the metal copper foil without any surface treatment on Al 2 o 3 On the substrate, put it into the chemical vapor deposition equipment, feed Ar, the flow rate is 500 sccm, and the working pressure is 1×10 5 Pa, then start to heat up, and the heating process lasts for 60 minutes;

[0125] 2. When the temperature rises to 1000°C, H 2 Gas, H 2 The flow rate is 20sccm, the Ar flow rate remains constant, and the annealing process is carried out, and the annealing duration is 40min;

[0126] 3. After the annealing is over, start to introduce CH 4 gas, CH 4 The flow rate is 5sccm, H 2 and Ar flow remain unchanged, the working pressure is 1×10 5 Pa, the growth time is 2m...

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Abstract

The invention provides an oxide-substrate-assisted method for quickly preparing large-size single-crystal graphene, relating to a preparation method of single-crystal graphene. The method is mainly characterized in that metal foil is used as a catalyst and growth substrate, oxide is used as a substrate to closely contact the metal foil, and a normal-pressure chemical vapor deposition (CVD) process is utilized to quickly obtain the large-size high-quality single-crystal graphene. The method solves the technical problems of substrate surface treatment, long growth cycle and the like in the CVD process for preparing large-size single-crystal graphene by using the common single crystal as the substrate, and quickly prepares the high-quality large-size single-crystal graphene sample by using the very simple process.

Description

technical field [0001] The invention relates to a method for rapid preparation of large-scale single crystal graphene assisted by an oxide substrate. Background technique [0002] Graphene is a two-dimensional honeycomb structure formed by densely packed single-layer carbon atoms, and is the basic unit of carbonaceous materials in other dimensions. In 2004, Geim and Novoselov successfully exfoliated graphene from graphite by using micromechanical exfoliation method. This huge breakthrough triggered an upsurge in research on graphene, and a series of novel properties of graphene began to show up in front of people. The valence and conduction bands of graphene intersect at the six vertices of the Fermi level, which is a zero-gap material, and its energy band structure is linear near the Fermi level. Each carbon atom contributes an unbonded electron, endowing graphene with good electrical conductivity and ultra-high carrier mobility (theoretically, its carrier mobility can rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/02C30B25/18
Inventor 徐小志张智宏刘开辉
Owner PEKING UNIV
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