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Fluorine and nitrogen co-doped three-dimensional graphene material and one-step carbonization preparation method thereof

A graphene and co-doping technology, applied in the direction of graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of not having the characteristics of graphene, complex process, toxicity, etc., achieving easy industrialization and simple process. , the effect of broad application prospects

Active Publication Date: 2019-03-08
GUILIN UNIV OF ELECTRONIC TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The technical problems of this technology are: xenon difluoride has a foul smell, is toxic, and has strong oxidizing properties.
The technical problem of this technology is that hydrofluoric acid is a toxic and highly corrosive reagent.
[0016] 1. The experimental procedure requires 5 steps, the process is complicated, the product quality is not easy to control, and the production cost is greatly increased;
[0017] 2. The thickness of the obtained material reaches tens of nanometers. If the thickness of the material is too large, it will not have the characteristics of graphene directly, and also reduce the specific surface area of ​​the material.
[0020] 1. The fluorine source polytetrafluoroethylene suspension is expensive;
[0021] 2. The production process requires two steps of carbonization, and the preparation time is long;
[0027] At present, there is no public technology that uses industrial-grade polytetrafluoroethylene powder and melamine powder as precursors to prepare fluorine and nitrogen co-doped three-dimensional graphene materials by one-step carbonization and applies them to supercapacitors. In the present invention, we realize the following: Polytetrafluoroethylene powder and melamine powder are used as precursors to directly prepare fluorine and nitrogen co-doped functionalized three-dimensional graphene materials. Interestingly, when the mixed precursor is carbonized, its specific surface area can change sensitively with temperature

Method used

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  • Fluorine and nitrogen co-doped three-dimensional graphene material and one-step carbonization preparation method thereof
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  • Fluorine and nitrogen co-doped three-dimensional graphene material and one-step carbonization preparation method thereof

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Embodiment 1

[0059] A fluorine, nitrogen co-doped three-dimensional graphene material and a one-step carbonization preparation method thereof, the specific preparation method is as follows:

[0060] Step 1, mixing of raw materials, weighing 3.0 g of melamine powder and 4.5 g of polytetrafluoroethylene powder in a mass ratio of 1:1.5, mixing and manual grinding in a mortar to obtain a uniform powder sample;

[0061] Step 2, one-step carbonization method, put the uniform powder sample obtained in step 1 into a quartz boat, put it into a tube furnace, and raise the temperature from room temperature to 700°C at a heating rate of 5°C / min under a nitrogen atmosphere Carry out carbonization, heat preservation carbonization time is 2.0h, obtain fluorine, nitrogen co-doped three-dimensional graphene material after cooling.

[0062] The fluorine, nitrogen co-doped three-dimensional graphene material prepared in embodiment 1 is tested by transmission scanning electron microscope, and the results are ...

Embodiment 2

[0069] In order to reflect the influence of carbonization temperature on the specific surface area of ​​the material of the present invention, examples of different carbonization temperatures are given.

[0070] A fluorine, nitrogen co-doped three-dimensional graphene material and a one-step carbonization preparation method thereof, the steps not particularly specified in the specific steps are the same as the preparation method described in Example 1, the difference is that the step 2 is heated to Carbonization is carried out at 800°C, that is, the carbonization temperature is 800°C.

[0071] The fluorine, nitrogen co-doped three-dimensional graphene material prepared in embodiment 2 is tested through isotherm adsorption curve and pore size distribution, the result is as follows Figure 7 and 8 As shown, the results show that the specific surface area of ​​fluorine and nitrogen co-doped three-dimensional graphene material is 284 m 2 g -1 , with a total pore volume of 0.79...

Embodiment 3

[0073] In order to reflect the influence of carbonization temperature on the specific surface area of ​​the material of the present invention, examples of different carbonization temperatures are given.

[0074] A fluorine, nitrogen co-doped three-dimensional graphene material and a one-step carbonization preparation method thereof, the steps not particularly specified in the specific steps are the same as the preparation method described in Example 1, the difference is that the step 2 is heated to Carbonization is carried out at 600°C, that is, the carbonization temperature is 600°C.

[0075] The fluorine and nitrogen co-doped three-dimensional graphene material prepared in embodiment 3 are tested through isotherm adsorption curve and pore size distribution, and the results are as follows: Figure 9 and 10 As shown, the results show that the specific surface area of ​​the 3D graphene material co-doped with fluorine and nitrogen is 60 m 2 g -1 , with a total pore volume of...

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Abstract

The invention discloses a fluorine and nitrogen co-doped three-dimensional graphene material. The fluorine and nitrogen co-doped three-dimensional graphene material is prepared by taking polytetrafluoroethylene and melamine as precursors through mixing and uniformly grinding and carrying out a one-step carbonization method; fluorine and nitrogen elements of three-dimensional graphene are uniformlydistributed; the specific surface area is 1200 to 1400m<2>g<-1> and the total pore volume is 2.5 to 2.9cm<3>g<-1>; the specific surface area of the material can be greatly regulated and controlled tobe 50 to 1600m<2>g<-1> through changing the carbonization temperature and the total pore volume is regulated and controlled to be 0.2 to 3.2cm<3>g<-1>. The one-step carbonization preparation method comprises the following steps: 1, mixing the raw materials; 2, carrying out a one-step carbonization method. Three-dimensional graphene grids in the material are uniform, and the fluorine and nitrogenelements are uniformly distributed; the repeatability is good and the carbonization temperature is moderate; the material is synthesized through one-step carbonization and a technology is simple and easy to operate. The material has a wide application prospect in the field of super-capacitors and a carbon functional material.

Description

technical field [0001] The invention relates to the field of modified carbon materials, in particular to a fluorine and nitrogen co-doped three-dimensional graphene material and a one-step carbonization preparation method thereof. Background technique [0002] Energy is the main driving force for the development of human society. Throughout the history of human development, every innovation in energy technology has caused major changes in social productivity and production relations, thus promoting the development of history. However, due to the rapid development of industrialization and the unrestrained exploitation of fossil fuels such as coal, oil, and natural gas, a series of problems such as resource shortage and environmental pollution have been caused, and the development and use of renewable energy have received increasing attention. As a green and environmentally friendly functional material, carbon nanomaterials are widely used in new energy storage and conversion...

Claims

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Application Information

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IPC IPC(8): C01B32/184
CPCC01B32/184C01B2204/32C01B2204/22
Inventor 彭洪亮段典成王扬扬徐芬孙立贤
Owner GUILIN UNIV OF ELECTRONIC TECH
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