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One-step in situ preparation of doped graphene with tunable nitrogen content and species

A technology of in-situ preparation and nitrogen content, applied in the field of doped graphene, can solve the problems of complex nitrogen-doped graphene preparation process, high preparation cost, controllable content and types of difficult nitrogen elements, etc., and achieve good catalytic stability. , large specific surface area, uniform effect of nitrogen doping

Active Publication Date: 2016-10-05
HARBIN INST OF TECH
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Problems solved by technology

[0004] The purpose of the present invention is to solve the problems that the current nitrogen-doped graphene preparation process is complicated, the preparation cost is high, it is difficult to industrialize and the content and type of nitrogen element in the prepared nitrogen-doped graphene can be controlled, and to provide a one-step in-situ preparation Method for doping graphene with tunable nitrogen content and species

Method used

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  • One-step in situ preparation of doped graphene with tunable nitrogen content and species
  • One-step in situ preparation of doped graphene with tunable nitrogen content and species
  • One-step in situ preparation of doped graphene with tunable nitrogen content and species

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specific Embodiment approach 1

[0023] Embodiment 1: In this embodiment, a method for one-step in-situ preparation of doped graphene with adjustable nitrogen content and type is carried out according to the following steps:

[0024] 1. Put 1-500g of carbon nitride in a quartz tube sealed at one end, wherein the inner diameter of the quartz tube is φ=5-100mm, length=20cm, a cylindrical quartz plug is placed at the open end, and the outer surface of the quartz plug is Diameter φ = 4 ~ 99mm, length = 5cm, the difference between the inner diameter of the quartz tube and the outer diameter of the quartz plug is 1mm;

[0025] 2. Put the quartz tube with carbon nitride in the tube furnace, and then vacuum the tube furnace to 8×10 -4 ~9×10 -4 Pa, and then feed a flow rate of 50 to 90 sccm shielding gas into the tube furnace;

[0026] 3. Heat the tube furnace treated in step 2 to 740-750°C at a rate of 1-5°C / min, and then keep it warm for 5-120min to obtain nitrogen-doped graphene;

[0027] 4. Heat the tube furnac...

specific Embodiment approach 2

[0033] Embodiment 2: This embodiment differs from Embodiment 1 in that the protective gas described in step 2 is high-purity argon or high-purity nitrogen. Other steps and parameters are the same as in the first embodiment.

specific Embodiment approach 3

[0034] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that in Step 3, the tube furnace treated in Step 2 is heated to 740° C. at a rate of 2° C. / min. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention relates to a method for preparing doped graphene with adjustable nitrogen content and adjustable varieties, in particular to a single-step method for preparing doped graphene with adjustable nitrogen content and adjustable varieties in situ, and aims to solve the problems that the conventional nitrogen-doped graphene is complex in preparation technology, relatively high in preparation cost, and difficult to industrialize, and the nitrogen content and varieties in the prepared nitrogen-doped graphene cannot be controlled. The method provided by the invention comprises the following steps: placing carbon nitride in a quartz tube with one sealed end; placing a cylindrical quartz plug at the open end of the quartz tube; transferring the quartz tube into a tube furnace; under the protection of an inert atmosphere, carrying out temperature raising and temperature keeping, and continuously carrying out temperature raising and temperature keeping, so as to finally adjust the nitrogen content and varieties in the nitrogen-doped graphene. The method is simple and environment-friendly; the prepared nitrogen-doped graphene is controllable in the nitrogen content and varieties, can replace commercial Pt / C to be used as an oxygen reduction catalyst, and is applied to the fields of batteries, photocatalysis, catalytic oxidation, gas sensors and medicine transportation.

Description

technical field [0001] The invention relates to a method for one-step in-situ preparation of doped graphene with adjustable nitrogen content and type. Background technique [0002] Graphene material is a single atomic layer material with a two-dimensional honeycomb structure, which is the basic structural unit of fullerene, carbon nanotube and graphite. Since the preparation of single-layer graphene by Andre K. Geim of the University of Manchester in 2004 (Science 2004, 306, 666-669), it has attracted extensive attention from the scientific and industrial circles. Graphene has excellent electrical, thermal and mechanical properties. (Science., 2009, 324, 1530-1534; Nature., 2005, 438, 201-204.) [0003] The structure and properties of graphene can be changed by element doping, enabling it to achieve richer chemical functions and applications. For example, when nitrogen atoms are introduced into graphene, the lone pair electrons of nitrogen atoms can undergo delocalized co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
Inventor 韩杰才宋波李加杰张宇民
Owner HARBIN INST OF TECH
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