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Method for liquid nitrogen assisted preparation of high quality graphene, and high quality graphene prepared through method

A liquid nitrogen-assisted, graphene technology, applied in high-quality graphene and its preparation, liquid nitrogen-assisted preparation of high-quality graphene, high-quality graphene field, can solve the problems of poor graphene quality, high cost, complicated operation and the like

Inactive Publication Date: 2018-10-09
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Among these methods, some methods prepare high-quality graphene, but are expensive and complicated to operate; some methods are simple to operate, but the prepared graphene is of poor quality

Method used

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  • Method for liquid nitrogen assisted preparation of high quality graphene, and high quality graphene prepared through method
  • Method for liquid nitrogen assisted preparation of high quality graphene, and high quality graphene prepared through method
  • Method for liquid nitrogen assisted preparation of high quality graphene, and high quality graphene prepared through method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] This example is used to illustrate the preparation of high-quality graphene assisted by liquid nitrogen.

[0082]1g of flake graphite (purchased from Sigma-Aldrich Company, 50 mesh, purity 99% by weight, the same below) was added to 50ml perchloric acid (purchased from Beijing Chemical Plant, mass concentration was 72%), stirred at room temperature for 3min ,filter.

[0083] The filtered graphite was placed in a corundum crucible, filled with argon and sealed. Put the crucible in a microwave oven (Galanz domestic microwave oven, 700W power), microwave for 3 minutes, take it out after cooling, and obtain 600ml fluffy worm-like graphite.

[0084] Put the worm-like graphite obtained by microwave into a 1000ml beaker, add 600ml of liquid nitrogen, and then use a high-speed mechanical stirrer to stir (the instrument was purchased from IKA, T 18 digital ULTRA-TURRAX, S 18N-19G dispersing cutter head). The rotation speed was set at 15000r / mi, the time was 20min, and liquid n...

Embodiment 2

[0091] This example is used to illustrate the preparation of high-quality graphene assisted by liquid nitrogen.

[0092] 1g flake graphite (purchased from Sigma-Aldrich Company, 50 mesh, purity 99% by weight, the same below) was added to 50ml of concentrated sulfuric acid (purchased from Beijing Chemical Plant, mass concentration was 98%), stirred at room temperature for 2 God, filter.

[0093] The filtered graphite was placed in a corundum crucible, filled with argon and sealed. Put the crucible in a microwave oven (Galanz domestic microwave oven, 700W power), microwave for 3 minutes, take it out after cooling, and obtain 320ml fluffy worm-like graphite.

[0094] Put the worm-like graphite obtained by microwave into a 1000ml beaker, add 600ml of liquid nitrogen, and then use a high-speed mechanical stirrer to stir (the instrument was purchased from IKA, T 18 digital ULTRA-TURRAX, S 18N-19G dispersing cutter head). The rotation speed was set at 15000r / min, the time was 20min...

Embodiment 3

[0097] This example is used to illustrate the preparation of high-quality graphene assisted by liquid nitrogen.

[0098] 1g of flake graphite (purchased from Sigma-Aldrich company, 50 mesh, purity 99% by weight, the same below) was added to 50ml of concentrated nitric acid and concentrated sulfuric acid mixed acid (the volume ratio of concentrated nitric acid and concentrated sulfuric acid was 3:2, and the concentrated nitric acid Purchased from Beijing Chemical Plant, the mass concentration is 98%, concentrated sulfuric acid was purchased from Beijing Chemical Plant, the mass concentration was 98%), stirred at room temperature for 2 days, and filtered.

[0099] The filtered graphite was placed in a corundum crucible, filled with nitrogen and sealed. Put the crucible in a microwave oven (Galanz domestic microwave oven, 700W power), microwave for 3 minutes, take it out after cooling, and obtain 480ml fluffy worm-like graphite.

[0100] Put the worm-like graphite obtained by mi...

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Abstract

The invention relates to a method for liquid nitrogen assisted preparation of high quality graphene, and high quality graphene prepared through the method. According to the present invention, the graphene has characteristics of low oxygen content, few defects, high content of few-layer graphene (less than 5 layers) and high two-dimensional lamella size; the method comprises: placing worm-like graphite in liquid nitrogen, stirring at a high speed, and volatilizing the liquid nitrogen after completing the stirring to obtain the graphene powder; the method is fast, efficient, safe, environmentally friendly and low-cost; the obtained graphene has good quality and has the oxygen content of below 8%, wherein the peak intensity ratio of the D peak to the G peak is below 0.8, and the peak intensity ratio of the 2D peak to the G peak is more than 0.2 in the Raman spectrum of the graphene; and the method can be used for the large-scale production of high-quality graphene.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and relates to a kind of graphene and its preparation method, especially a kind of high-quality graphene and its preparation method. More specifically, the invention relates to a liquid nitrogen-assisted method for preparing high-quality graphene Method and high-quality graphene obtained. Background technique [0002] Graphene is carbon atoms with sp 2 The hexagonal honeycomb two-dimensional structure material formed by hybrid orbitals has many excellent properties. Graphene has ultra-high light transmittance, high thermal conductivity, high electron mobility, high electrical conductivity, room temperature quantum Hall effect, adjustable energy band gap, excellent mechanical properties, efficient hydrogen storage performance, singular magnetic chemical properties and perfect charge-to-charge interactions. Because of its unparalleled properties, graphene is considered to be the materia...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B2204/04C01B2204/32C01P2002/72C01P2002/82C01P2004/03C01P2004/04
Inventor 智林杰张涛麟
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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