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Large monocrystal graphene and preparation method thereof

A single crystal graphene, polymethyl methacrylate technology, applied in the field of large single crystal graphene and its preparation, can solve the problems of expensive single crystal substrate, long time and the like

Active Publication Date: 2015-05-27
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both can make the single crystal size of graphene reach the millimeter level, but there are also problems. The former takes a very long time, while the latter requires an expensive single crystal substrate

Method used

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  • Large monocrystal graphene and preparation method thereof
  • Large monocrystal graphene and preparation method thereof
  • Large monocrystal graphene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1. Two separate stacked copper foils quickly prepare isolated large single crystal graphene:

[0049] 1) Use a polishing solution composed of phosphoric acid and ethylene glycol according to a ratio of 3:1 (v / v) and deionized water to clean the copper foil (produced by Alfa Aesar, purity 99.8%, thickness 25μm), and cut the copper foil To stack the two pieces neatly, the distance between the two copper foils measured with a vernier caliper does not exceed 30μm;

[0050] 2) Place the stacked copper foil in a sleeve with a magnetic control device, and then place the sleeve in a tube furnace, pump it to the lowest air pressure, and purge it for 2-3 times at a low pressure of 1Pa Raise the temperature of the furnace body to 1035℃ under vacuum and gas-free conditions and keep it for 30 minutes;

[0051] 3) Keep the temperature of the furnace body constant, and pass in hydrogen gas with a flow rate of 100 sccm for 5 minutes;

[0052] 4) Keep the furnace temperature and hydrog...

Embodiment 2

[0060] Example 2. Two discretely stacked copper foils quickly prepare continuous large single crystal graphene films:

[0061] 1) Use a polishing solution composed of phosphoric acid and ethylene glycol according to a ratio of 3:1 (v / v) and deionized water to clean the copper foil (produced by Alfa Aesar, purity 99.8%, thickness 25μm), and cut the copper foil To stack the two pieces neatly, the distance between the two copper foils measured with a vernier caliper does not exceed 30μm;

[0062] 2) Put the stacked copper foil in a sleeve with a magnetic control device, and then put the sleeve in a tube furnace, pump it to the lowest air pressure, and purge it for 2-3 times at a low pressure of 1Pa Raise the temperature of the furnace body to 1035℃ under vacuum and gas-free conditions and keep it for 30 minutes;

[0063] 3) Keep the temperature of the furnace body constant, and pass in hydrogen gas with a flow rate of 100 sccm for 5 minutes;

[0064] 4) Keep the temperature of the furna...

Embodiment 3

[0069] Example 3. Single crystal graphene prepared in large quantities by convolving copper foil.

[0070] 1) Use a polishing solution composed of phosphoric acid and ethylene glycol in a ratio of 3:1 (v / v) and deionized water to clean large-area copper foil (manufactured by Alfa Aesar, purity 99.8%, thickness 25μm), Figure 8 (A) is a physical photo of a large area of ​​copper foil;

[0071] 2) Convolve the cleaned large-area copper foil into a roll, use a vernier caliper to measure that the distance between the two copper foils does not exceed 30μm, then put it into a sleeve with a magnetic control device, and then place the sleeve in a tube furnace , Under the state of pumping to the lowest pressure, purge 2-3 times, raise the temperature of the furnace body to 1035 ℃ under the highest vacuum without gas, and keep it for 30 minutes. Figure 8 (B) is a physical photo of a large area of ​​copper foil convolution;

[0072] 3) Keep the temperature of the furnace body constant, and p...

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Abstract

The invention relates to a large monocrystal graphene and a preparation method thereof. The preparation method comprises the following steps: 1) in a non-reducing gas atmosphere, carrying out annealing treatment on a copper base; 2) while introducing reducing gas into a reactor, carrying out annealing reduction on the copper base subjected to annealing treatment in the step 1); and 3) depositing graphene on the surface opposite the substrate on the gap formed by the two copper bases subjected to annealing reduction by a chemical vapor deposition process, thereby obtaining the isolated large monocrystal graphene. The preparation method can also further comprise the following steps: by using polymethyl methacrylate (PMMA) or polyethylene terephthalate (PET) as a medium, transferring the large monocrystal graphene onto the target base, and adjusting the growth time and gas flow rate in the graphene growth process to quickly prepare the isolated large monocrystal graphene sample. The method does not need longer preparation time or any expensive monocrystal base.

Description

Technical field [0001] The invention belongs to the field of graphene preparation, and specifically relates to a large single crystal graphene and a preparation method thereof. Background technique [0002] Graphene is a honeycomb-shaped two-dimensional atomic crystal composed of a single layer of carbon atoms closely arranged. Because of its excellent optical, electrical and mechanical properties, it has received extensive attention since its discovery. However, how to apply it to practical applications, the key lies in the need for efficient preparation methods. At present, a variety of graphene preparation methods have emerged, such as mechanical exfoliation, liquid exfoliation, graphene oxide reduction, silicon carbide epitaxy, chemical vapor deposition, and segregation growth. Among them, the chemical vapor deposition method has become one of the mainstream methods for preparing graphene due to its advantages of large area, high quality, regular shape, easy transfer, contr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 彭海琳王欢刘忠范
Owner PEKING UNIV
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