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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  • Description
  • Claims
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Based on current studies, the controllable preparation of high-performance

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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

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Example Embodiment

[0033] Example 1

[0034] (1) 100mg of graphene oxide and 5mg of phosphoric acid prepared by the modified hummers method are added to 100ml of 95% absolute ethanol 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 100L / h; increase the temperature of the dispersion at a rate of 10°C / min, at 2000°C After 50 hours of carbonization treatment, a nanoporous graphene oxide precursor is obtained;

[0036] (3) The carbonized nanoporous graphene oxide precursor in step (2) is activated in a plasma flow of argon and hydrogen, and benzene and ammonia are introduced, and the flow rate of argon and hydrogen is 120L / h Benzene and ammonia are added at concentrations of 0.5 mol / L and 0.1 mol / L, respectively; nitrogen-doped graphene is grown by vapor deposition at a temperature of 700 ℃, and the plasma is removed after 10 minutes of reaction;

[0037] (4) The product o...

Example Embodiment

[0038] Example 2

[0039] (1) 100mg of graphene oxide and 10mg of ethyl silicate prepared by the modified hummers method are added to 100ml of 95% absolute ethanol 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; increase the temperature of the dispersion at a rate of 10°C / min, and carbonize at 2500°C 50h to obtain a nanoporous graphene oxide precursor;

[0041] (3) The carbonized nanoporous graphene oxide precursor in step (2) is activated in a plasma flow of argon and hydrogen, and benzene and ammonia are introduced. The flow rates of argon and hydrogen are both 120L / h; Add benzene and ammonia at concentrations of 0.5 mol / L and 0.2 mol / L, and grow nitrogen-doped graphene by vapor deposition at a temperature of 700 ℃. After reacting for 10 minutes, the plasma is withdrawn;

[0042] (4) The product obtained in step (3) is heated and cooled: the temperature is low...

Example Embodiment

[0043] Example 3

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

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

[0046] (3) The carbonized nanoporous graphene oxide precursor in step (2) is activated in a hydrogen plasma stream, and benzene and ammonia are introduced into argon and hydrogen streams, and the argon flow rate is 120L / h , The flow rate of hydrogen 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 a temperature of 600℃, and the plasma is withdrawn after 10 minutes of reaction;

[0047] (4) The product obtained in step (3) is heated and coo...

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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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