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Preparation method and application of large size and shape ratio graphene microsheet

A graphene micro-flake and large-size technology, applied in the direction of graphene, nano-carbon, etc., can solve the problems of precise and controllable atomic layer number of reduced graphene oxide products, inability to obtain graphene micro-flakes, graphene easy to agglomerate, etc. , to achieve the effect of less layers, low cost and large finished product area

Active Publication Date: 2013-09-25
JIANGNAN GRAPHENE RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The use of laser heating to reduce graphene oxide solution (or spin-coating solution) and the patterning preparation on this basis have been reported many times, but the method used before requires the laser to directly irradiate the graphene oxide dispersed in the solvent, not only the reduced Graphene is easy to agglomerate, and its own impurities or weak acid substances in the solution may prevent partial reduction of carboxyl groups on the edge of graphene oxide, so that larger-sized graphene microplates cannot be obtained
In fact, it is quite difficult to precisely control the number of atomic layers or the size of the product by using the traditional solution irradiation method to reduce graphene oxide.

Method used

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  • Preparation method and application of large size and shape ratio graphene microsheet

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Glue the glass substrate or independent graphene oxide paper vertically on the support and put it into the quartz tube. The distance between the sample and the window at the end of the quartz tube is about 150mm. Use a mechanical pump and a molecular pump to draw a vacuum until the pressure in the tube drops to 10 -2 Pa; close the exhaust valve, feed some high-purity nitrogen for 2-5 minutes until it fills the furnace tube, then close the nitrogen valve, reopen the exhaust valve, and wait until the pressure in the tube drops to 10 -2 Pa, nitrogen gas is introduced again, and after repeated 2-3 times, the vacuum is continuously pumped for 2-3 hours until the pressure drops to the limit of about 1x10 -4 Pa. Introduce high-purity hydrogen (99.999%) until the relative negative pressure inside the tube rises to -0.05Pa.

[0025] 2. Install the fiber laser, adjust its vertical height and horizontal position, so that the emitted laser beam is just focused on the sample s...

Embodiment 2

[0029] 1. Will be mixed with impurities (such as SiO 2 Graphene oxide paper (powder, metal particles, carbon nanotubes, etc.) is stuck vertically on the support and put into the quartz tube. The distance between the sample and the window at the end of the quartz tube is about 150mm. Use a mechanical pump and a molecular pump to draw a vacuum until the pressure in the tube drops to 10 -2 Pa; close the exhaust valve, feed some high-purity nitrogen for 2-5 minutes until it fills the furnace tube, then close the nitrogen valve, reopen the exhaust valve, and wait until the pressure in the tube drops to 10 -2 Pa, nitrogen gas is introduced again, and after repeated 2-3 times, the vacuum is continuously pumped for 2-3 hours until the pressure drops to the limit of about 1x10 -4 Pa. Introduce high-purity hydrogen (99.999%) until the relative negative pressure inside the tube rises to -0.05Pa.

[0030] 2. Install the fiber laser, adjust its vertical height and horizontal position, ...

Embodiment 3

[0034] 1. A graphene oxide paper containing patterned and complex structures (such as polymer coatings) is glued vertically on a support and placed in a quartz tube. The distance between the sample and the window at the end of the quartz tube is about 150mm. Use a mechanical pump and a molecular pump to draw a vacuum until the pressure in the tube drops to 10 -2 Pa; close the exhaust valve, feed some high-purity nitrogen for 2-5 minutes until it fills the furnace tube, then close the nitrogen valve, reopen the exhaust valve, and wait until the pressure in the tube drops to 10 -2 Pa, nitrogen gas is introduced again, and after repeated 2-3 times, the vacuum is continuously pumped for 2-3 hours until the pressure drops to the limit of about 1x10 -4 Pa. Introduce high-purity hydrogen (99.999%) until the relative negative pressure inside the tube rises to -0.05Pa.

[0035] 2. Install the fiber laser, adjust its vertical height and horizontal position, so that the emitted laser ...

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Abstract

The invention relates to a preparation method and application of a large size and shape ratio graphene microsheet. The method comprises the following steps: arranging oxidized graphene paper or a mixed material containing partial impurities in a quartz tube, introducing H2 at a certain air pressure, and focusing a sample for performing scanning heating by using high-speed laser, wherein a complete graphene microsheet with less than ten atomic layers and high electric conductivity and high uniformity can be prepared in a room temperature environment under certain conditions, and the impurities in the material can be finely processed. The average atomic layer number of the prepared graphene is 6-8, the particle size is between 2.0 and 3.0nm, and the shape ratio of the microsheet can be close to 10,000. The optical and conductive performances are obviously superior to those of the graphene microsheet prepared by the traditional chemical reducing method; according to fine regulation of the laser scanning parameters, the method has the advantages of repeatedly performing sample treatment and pattern processing, along with high target processability, controllable layer number and size of the microsheet, simple equipment, cleanliness, high efficiency and flexible operation, and has excellent industrial application value.

Description

technical field [0001] The invention relates to a preparation method of graphene microchips, in particular to a preparation method of graphene microchips with large size and shape ratio and its application. Background technique [0002] Graphene microflakes generally refer to ultra-thin graphene layered stacks with more than 10 carbon layers and a thickness in the range of 5-100 nanometers. In some literatures, it is also called GrapheneNanosheets. Graphene microsheets maintain the original planar carbon six-membered ring conjugated crystal structure of graphite, and have excellent mechanical strength, electrical conductivity, and thermal conductivity, as well as good lubrication and high temperature resistance. and anti-corrosion properties. Compared with ordinary graphite, the thickness of graphene microsheets is in the nanoscale range, but its radial width can reach several to tens of microns, and it has a large shape ratio (diameter / thickness ratio). Graphene microshee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 王皓陈海力郭冰
Owner JIANGNAN GRAPHENE RES INST
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