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Graphene preparation method

A graphene and inorganic salt technology, applied in the field of carbon-containing organic matter conversion non-gas phase growth graphene, to achieve the effects of high product purity, good dispersibility and short reaction period

Inactive Publication Date: 2015-09-02
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, as far as the applicant knows, there is no report so far that uses inorganic salts as a reaction medium to utilize carbon-containing organic matter to convert non-vapor-phase grown graphene.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Weigh 7.325g of sodium citrate and 21.002g of sodium bicarbonate in a molar ratio of 1:10, put them into an agate mortar and grind them thoroughly and mix them evenly.

[0023] (2) Put the mixture obtained in the previous step into a high-temperature tube furnace, pass high-purity argon for 30 minutes to exhaust the residual air in the furnace tube, then heat it from room temperature to 900 °C at a heating rate of 3 °C / min, and keep it warm 1h, then naturally cool to room temperature, turn off the argon, and take out the black solid mixture of graphene and inorganic salt reaction medium.

[0024] (3) Put the solid mixture obtained in the previous step into the hydrochloric acid lotion and soak for 5 hours, separate by suction filtration, wash several times with deionized water and absolute ethanol, put it in a vacuum drying oven at 100°C and dry for 12 hours to obtain Graphene material.

[0025] figure 1 It is a scanning electron microscope picture of the prepared...

Embodiment example 2

[0027] (1) Weigh 2.188g of sodium gluconate and 20.000g of calcium carbonate at a molar ratio of 1:20, put them into an agate mortar and grind them thoroughly and mix them evenly.

[0028] (2) Put the mixture obtained in the previous step into a high-temperature tube furnace, pass high-purity argon for 30 minutes to exhaust the residual air in the furnace tube, then heat it from room temperature to 700 °C at a heating rate of 5 °C / min, and keep it warm 5h, then naturally cooled to room temperature, closed the argon, and took out the black solid mixture of graphene and inorganic salt reaction medium.

[0029] (3) Put the solid mixture obtained in the previous step into the sulfuric acid lotion and soak for 5 hours, separate by suction filtration, wash several times with deionized water and absolute ethanol, put it in a vacuum drying oven at 100°C and dry for 12 hours to obtain Graphene material.

[0030] figure 2 It is a transmission electron microscope picture of the prepar...

Embodiment example 3

[0032] (1) Weigh 9.70g of starch and 27.26g of zinc chloride at a molar ratio of 1:4, put them into an agate mortar, grind them and mix them well.

[0033](2) Put the mixture obtained in the previous step into a high-temperature tube furnace, pass high-purity nitrogen gas for 30 minutes to exhaust the residual air in the furnace tube, then heat it from room temperature to 850°C at a heating rate of 10°C / min, and keep it warm for 3h , then cool naturally to room temperature, turn off the nitrogen, and take out the black solid mixture that obtains graphene and inorganic salt reaction medium.

[0034] (3) Put the solid mixture obtained in the previous step into the sulfuric acid lotion and soak for 5 hours, separate by suction filtration, wash several times with deionized water and absolute ethanol, put it in a vacuum drying oven at 100°C and dry for 12 hours to obtain Graphene material.

[0035] image 3 It is a high-resolution transmission electron microscope image of the pre...

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Abstract

The invention discloses a graphene preparation method. Under a high-temperature inert atmosphere, inorganic salt serving as a reaction medium is directly converted for non-vapor phase growth controllable synthesis by a carbonaceous organic material to obtain a large-area high-quality graphene material through regulation of heating rate, heat insulation time, raw material ratio and the like. The thickness of prepared graphene is 0.7-2nm, the area of the graphene is several micrometers, and the number of layers of the graphene is 1-8. The prepared graphene has various characteristics of the graphene material and can serve as electrode materials of lithium ion batteries, super-capacitors, solar cells and the like, catalyst carriers and the like. The cheap inorganic salt is taken as the reaction medium to be converted by the carbonaceous organic material, the graphene is synthesized through non-vapor phase growth at a low temperature, operation technology is quite simple, operation cost is low, reaction cycle is short, product sizes and shapes are uniform, and dispersity, yield and product purity are high. Compared with widely-applied stripping and conventional high-temperature growth methods, the graphene preparation method has the advantages of controllable preparation, mass synthesis and the like. The graphene preparation method is suitable for industrial production and large-scale application.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and in particular relates to a method for converting carbon-containing organic matter into non-gas-phase grown graphene. Background technique [0002] Graphene is a single-layer two-dimensional crystal structure with carbon atoms arranged in a hexagonal honeycomb shape. It is the basic unit of carbonaceous materials such as zero-dimensional fullerenes, one-dimensional carbon nanotubes and three-dimensional graphite. Since Andre K. Geim and Konstantin S. Novoselov, two scientists from the University of Manchester in the United Kingdom, successfully prepared single-layer graphene by a simple tape stripping method in 2004, this two-dimensional crystal has become a popular topic in the field of material science research. The hot spot has attracted great attention of researchers all over the world. Due to their outstanding contributions in the field of graphene preparation, the above two...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 曹传宝朱有启
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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