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Graphene with high specific capacitance and preparation method thereof

A technology of high specific capacitance and graphene, applied in the direction of graphene, nano-carbon, etc., can solve the problems of easy aggregation, low quality of graphene, low yield, etc., to overcome the difficulty of separation, simplify the operation process, and overcome the problems of low purity Effect

Inactive Publication Date: 2013-03-27
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

With the development of various applications, the demand for graphene has increased greatly, and the structure and performance of graphene have higher requirements. However, the graphene produced by the "scotch-tape" stripping method has been unable to meet the needs of industrial applications.
The newly developed graphene preparation methods in recent years mainly include "top-down" method and "bottom-up" method: the former mainly uses graphite as raw material, through "mechanical exfoliation", "redox", "liquid phase Methods such as "exfoliation" and "electrochemical exfoliation" to overcome the strong π-π interaction between graphite layers to obtain graphene are time-consuming and laborious, and the yield is still low; the latter mainly uses some carbon-containing reagents, Such as ethanol and metal sodium, hexa-peri-hexabenzocorone (HBC), etc. prepare graphene through high temperature and high pressure reaction, but the quality of graphene produced by these methods is generally low, mainly for easy aggregation (low specific surface area), and the introduction of some Oxygen-containing groups (low conductivity), two-dimensional size and number of layers are not suitable for control, etc., and its application is limited
Although "chemical vapor deposition (CVD)" is also used as an effective "bottom-up" method to convert hydrocarbons or amorphous carbon into high-quality graphene, the equipment required for this method is expensive, and graphite The yield of ene is also low, and the preparation conditions must be precisely controlled (otherwise graphite crystals will be formed instead of graphene), which also limits the production and application of graphene

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  • Graphene with high specific capacitance and preparation method thereof
  • Graphene with high specific capacitance and preparation method thereof
  • Graphene with high specific capacitance and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0039] Add 1.45 g of sucrose to a solution of 3.5 ml of water, 100 μl of concentrated sulfuric acid and 20 mg of nickel nitrate to dissolve, then 2 g of MCM-22 molecular sieves, stir at room temperature, and dry at 100 °C and 160 °C for 12 hours, then Then add a mixed solution of 0.87 g sucrose, 3.5 ml water, 20 mg nickel nitrate and 60 μl concentrated sulfuric acid, mix well, and then dry at 100 °C and 160 °C for 12 h, put the obtained solid powder into a vacuum tube furnace, pass Nitrogen gas was roasted at 500 °C for 2 h, then taken out, put into 2.5 L of mixed solution of hydrofluoric acid and hydrochloric acid, wherein the concentration of hydrofluoric acid was 0.1 g / ml, and the concentration of hydrochloric acid was 0.3 g / ml, after stirring at 70 °C for 2 h, Centrifuge, wash the solid with water and sonicate, and finally freeze-dry the obtained solid sample to obtain graphene powder. The graphene powder contains 1-4 layers of graphene with a two-dimensional size in the r...

Embodiment 2

[0046] Add 1.0 g of sucrose to a solution of 3.5 ml of water, 100 μl of concentrated sulfuric acid and 20 mg of nickel sulfate to dissolve it, then add 2 g of MCM-22 molecular sieves, stir evenly at room temperature, and dry at 60 °C and 150 °C for 12 hours respectively. Then add a mixed solution of 1.0 g sucrose, 3.5 ml water, 20 mg nickel sulfate and 60 μl concentrated sulfuric acid, mix well, then dry at 100 °C and 160 °C for 12 hours, and put the obtained solid powder into a vacuum tube furnace , roasted at 1200 °C for 2 h under nitrogen gas, took it out, put it into a mixed solution of 2.5 L of hydrofluoric acid and hydrochloric acid, wherein the concentration of hydrofluoric acid was 0.3 g / ml, and the concentration of hydrochloric acid was 0.3 g / ml, and stirred at 20 °C for 3 h Afterwards, centrifugal separation, the solid was washed with water and ultrasonicated, and the finally obtained solid sample was freeze-dried to obtain graphene powder. The graphene powder contai...

Embodiment 3

[0048] Add 2.05 g of sucrose to a solution of 3.5 ml of water, 100 μl of concentrated sulfuric acid and 20 mg of nickel chloride to dissolve it, then add 2 g of MCM-22 molecular sieves, stir well at room temperature, and dry at 100 °C and 200 °C for 12 hours each , and then add a mixed solution of 1.27 g sucrose, 3.5 ml water, 20 mg nickel chloride and 60 μl concentrated sulfuric acid, mix well, then dry at 100 °C and 160 °C for 12 hours, and put the obtained solid powder into a vacuum tube In the furnace, blow nitrogen at 800 °C for 2 hours, take it out, put it into a mixed solution of 2.5 L of hydrofluoric acid and hydrochloric acid, wherein the concentration of hydrofluoric acid is 0.2 g / ml, and the concentration of hydrochloric acid is 0.3 g / ml, and stir at 80 °C After 2 h, it was centrifuged, the solid was washed with water and ultrasonicated, and finally the obtained solid sample was freeze-dried to obtain graphene powder. The graphene powder contains 1-10 layers of ...

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Abstract

The invention belongs to the technical field of nanometer material preparation, and in particular relates to a graphene with high specific capacitance and a preparation method thereof. The method specifically comprises the following steps: firstly soaking an MCM-22 molecular sieve into a mixture liquor of carbon source, nickel salt and concentrated sulphuric acid, so that carbon source molecules and Ni2<+> ions fully enter spaces between the layers of the MCM-22 molecular sieve; then pre-carbonizing the MCM-22 molecular sieve at low temperature; in the presence of high-temperature inert gases, calcinating the MCM-22 molecular sieve for a certain time to obtain a compound of the graphene and the MCM-22 molecular sieve; and finally, the MCM-22 molecular sieve and nickel in the compound are dissolved, are centrifugally separated out and are dried to obtain the graphene. The graphene which is prepared through the method has the advantages of large specific area, high electric conductivity and controllable two-dimensional size and layers. The graphene can be used as a capacitance material of supercapacitors and has excellent capacitance performance. The method is simple to operate, is low in cost, has reproducibility and can be used for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, in particular, relates to a graphene with high specific capacitance and a new method for preparing graphene by template and catalysis. Background technique [0002] Graphene is a two-dimensional planar structure ultra-thin nanomaterial composed of 1-10 layers of carbon atoms. It has excellent electrical, optical and thermal properties, and plays a very important role in microelectronics, biomedicine, energy storage and conversion, sensors, etc., and is a material with important application prospects. With the needs of various application developments, the demand for graphene has greatly increased, and the requirements for the structure and performance of graphene are higher. However, the graphene produced by the "scotch-tape" exfoliation method can no longer meet the needs of industrial applications. The newly developed graphene preparation methods in recent years mainly include...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184
Inventor 王义孔继烈
Owner FUDAN UNIV
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