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Method for growing three-dimensional nitrogen-doped graphene by taking nanoporous graphene as substrate

A nitrogen-doped graphene and graphene technology, applied in nanotechnology and other directions, to achieve the effects of excellent electrochemical performance, uniform distribution, and uniform pore size

Active Publication Date: 2015-09-23
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Based on current studies, the controllable preparation of high-performance 3D nanoporous nitrogen-doped graphene composites remains a challenging topic

Method used

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  • Method for growing three-dimensional nitrogen-doped graphene by taking nanoporous graphene as substrate
  • Method for growing three-dimensional nitrogen-doped graphene by taking nanoporous graphene as substrate

Examples

Experimental program
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Embodiment 1

[0034] (1) 100 mg of graphene oxide and 5 mg of phosphoric acid prepared by the improved hummers method are added to 100 ml of 95% dehydrated alcohol and fully dispersed into a dispersion;

[0035] (2) Place the dispersion prepared in step (1) in an atmosphere of nitrogen and argon, and control the flow rate of nitrogen and argon to be 100L / h; heat up the dispersion at a rate of 10°C / min, at 2000°C After lower carbonization treatment for 50 hours, a multi-nanoporous graphene oxide precursor is obtained;

[0036] (3) the carbonized multi-nanoporous graphene oxide precursor in step (2) is activated in the plasma flow of argon and hydrogen, and feeds benzene and ammonia, and the flow rate of argon and hydrogen is 120L / h ; The concentrations of benzene and ammonia gas were added to be 0.5mol / L and 0.1mol / L respectively; Nitrogen-doped graphene was grown by vapor phase deposition at a temperature of 700°C, and the plasma was withdrawn after 10 minutes of reaction;

[0037] (4) The...

Embodiment 2

[0039] (1) Graphene oxide 100mg and 10mg ethyl silicate prepared by the improved hummers method are added to 95% dehydrated alcohol 100ml and fully dispersed into a dispersion;

[0040] (2) Place the dispersion prepared in step (1) in an atmosphere of nitrogen and argon, and control the flow rate to 100L / h; heat up the dispersion at a rate of 10°C / min, and carbonize it at 2500°C 50h, obtain the graphene oxide precursor of many nanopores;

[0041] (3) the carbonized multi-nanoporous graphene oxide precursor in step (2) is placed in the plasma flow of argon and hydrogen for activation, and feeds benzene and ammonia, and the flow rate of argon and hydrogen is 120L / h: Add benzene and ammonia at concentrations of 0.5 mol / L and 0.2 mol / L respectively, grow nitrogen-doped graphene by vapor deposition at 700°C, react for 10 minutes, and withdraw from the plasma;

[0042] (4) The product obtained in step (3) is subjected to heating and cooling treatment: start to cool down to 100° C....

Embodiment 3

[0044] (1) Add 100 mg of graphene oxide and 10 mg of boric acid prepared by the improved hummers method to 100 ml of deionized water and fully disperse into a dispersion;

[0045] (2) Place the dispersion prepared in step (1) in an atmosphere of nitrogen and argon, control the flow rate to 100L / h; heat up at a rate of 10°C / min, and carbonize at 2000°C for 50h to obtain multi-nano Porous graphene oxide precursors;

[0046] (3) The carbonized multi-nanoporous graphene oxide precursor in step (2) is placed in a hydrogen plasma flow for activation, and in argon, benzene and ammonia are passed into the hydrogen flow, and the argon flow rate is 120L / h , the hydrogen flow rate is 120L / h; the concentrations of benzene and ammonia are 0.5mol / L and 0.3mol / L respectively; nitrogen-doped graphene is grown by vapor deposition at 600°C, and the plasma is withdrawn after 10 minutes of reaction;

[0047](4) The product obtained in step (3) is subjected to heating and cooling treatment: start...

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Abstract

The invention provides a method for growing three-dimensional nitrogen-doped graphene by taking nanoporous graphene as a substrate. According to the method, oxidized graphene is taken as a precursor, a pore forming agent is added, nanometer micropores are formed in the surface of the oxidized graphene precursor through treatment, and the diameters of the pores are uniform and controllable; the precursor is combined with a silicon source and a nitrogen source through a plasma activation technology to realize the growth of porous nitrogen-doped graphene with different nitrogen contents, and a three-dimensional structure is obtained at a high temperature. According to the method, carbonized nanoporous oxidized graphene is taken as the substrate for the first time, the pore diameters of the nanometer pores of the prepared three-dimensional porous nitrogen-doped graphene are effectively controlled within 5-50 nm and are uniform, and the nanometer pores are distributed uniformly; the three-dimensional nitrogen-doped graphene with such pore diameters has more excellent electrochemical properties; since oxidized graphene is taken as the substrate, the use of a strong oxidant, which is used during an etching process when a metal substrate is used, is avoided, and the introduction of non-carbon impurity elements is also avoided, so that the nitrogen-doped graphene has higher purity.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for growing three-dimensional nitrogen-doped graphene using nanoporous graphene as a substrate. Background technique [0002] Due to its unparalleled specific surface area and electrical conductivity, graphene has led a new wave of research on carbon nanomaterials. However, graphene sheets are easy to agglomerate under the action of van der Waals force, which reduces its active surface area and application stability. Due to its special spatial structure, the porous three-dimensional graphene greatly reduces the agglomeration effect of graphene, thereby maintaining a high catalytically active surface area. Theoretical studies have shown that the energy band structure of graphene will change after nitrogen doping, which can greatly expand the application of graphene in the fields of optics, electricity and magnetism. [0003] Authorized paten...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y40/00
Inventor 王宗花赵启燕张菲菲杨敏夏建飞
Owner QINGDAO UNIV
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