A method for preparing nitrogen-doped carbon material containing pure pyridine nitrogen based on chemical vapor deposition

A chemical vapor deposition, nitrogen-doped carbon technology, applied in nanotechnology, electrical components, structural parts, etc. for materials and surface science, which can solve the problems that are not completely convincing, cannot be prepared on a large scale, and have relatively high equipment requirements. Advanced problems, to achieve the effect of suitable for large-scale production, low cost, controllable amount of nitrogen doping

Active Publication Date: 2019-05-03
CENT SOUTH UNIV
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  • Claims
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Problems solved by technology

The research on the active sites of nitrogen-doped nanocarbon materials is also becoming the focus of attention. Many researchers believe that pyridinic nitrogen contributes to the formation of catalytic active sites for oxygen reduction reaction (ORR), but their views cannot completely make convincing because in their synthesized catalysts, the type of nitrogen is always a mixture of graphitic nitrogen, pyridinic nitrogen, pyrrolic nitrogen and nitrogen oxide
[0004] In recent years, researchers have attempted to study the relationship between it and ORR catalytic activity by preparing pure pyridinic nitrogen. Donghui Guo designed an "edge-patterned" highly oriented pyrolytic graphite (HOPG) as a substrate for pure pyridinic nitrogen. , Zhiqiang Luo successfully prepared pure pyridine nitrogen-doped graphene by CVD. However, because their process requires high equipment and the preparation process is too complicated, it is not yet possible to prepare a new catalyst of pure pyridine nitrogen-doped carbon material on a large scale.
[0005] So far, pure pyridine nitrogen doped carbon materials are still a novel and challenging work, not only low doping rate but also high energy consumption, so this patent discloses a simple, easy, effective, and large-scale preparation Method for doping carbon materials with pure pyridinic nitrogen

Method used

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  • A method for preparing nitrogen-doped carbon material containing pure pyridine nitrogen based on chemical vapor deposition
  • A method for preparing nitrogen-doped carbon material containing pure pyridine nitrogen based on chemical vapor deposition

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Experimental program
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Embodiment 1

[0034] Based on carbon paper, with 1M HNO 3 After the surface of the carbon paper was roughened for 2 hours, it was washed to neutral and dried at 80°C for 6 hours, and then the dried carbon paper was placed in 6wt.%Ni(NO 3 ) 3 solution for 6 hours, then dried at 80°C for 6 hours after taking it out, and then the surface was loaded with Ni(NO 3 ) 3 The carbon paper is placed in the CVD deposition furnace, under N 2 (6L min -1 ,99.9%) under a protective atmosphere, the temperature was raised to 500°C and kept for a period of 4 hours, and N 2 (3L min -1 ,99.9%), after 2h, the reducing gas H 2 (3L min -1 ,99.9%), then in N 2 (6L min -1 ,99.9%) under a protective atmosphere, the temperature was raised to 700°C, and at C 3 h 6 with N 2 Mixed atmosphere (C 3 h 6 :3L min -1 ; N 2 :4L min -1 ) for 40min; finally in N 2 (6L min -1 ,99.9%) the protective atmosphere dropped to room temperature. Choose 20mol L -1 The HF was used to "cut" the CNFs for 30 min, washed wi...

Embodiment 2

[0036] Based on carbon paper, with 1M HNO 3 After the surface of the carbon paper was roughened for 2 hours, it was washed to neutral and dried at 80°C for 6 hours, and then the dried carbon paper was placed in 6wt.%Ni(NO 3 ) 3 solution for 6 hours, then dried at 80°C for 6 hours after taking it out, and then the surface was loaded with Ni(NO 3 ) 3 The carbon paper is placed in the CVD deposition furnace, under N 2 (6L min -1 ,99.9%) under a protective atmosphere, the temperature was raised to 350°C and kept for a period of 4 hours, and N was introduced for the first 2 hours of the holding period 2 (3L min -1 ,99.9%), after 2h, the reducing gas H 2 (3L min -1 ,99.9%), then in N 2 (6L min -1 ,99.9%) under a protective atmosphere, the temperature was raised to 600°C, and at C 3 h 6 with N 2 Mixed atmosphere (C 3 h 6 :3L min -1 ; N 2 :4L min -1 ) for 40min; finally in N 2 (6L min -1 ,99.9%) the protective atmosphere dropped to room temperature. Choose 20mol L ...

Embodiment 3

[0038] Based on carbon paper, with 1M HNO 3 After the surface of the carbon paper was roughened for 2 hours, it was washed to neutral and dried at 80°C for 6 hours, and then the dried carbon paper was placed in 6wt.%Ni(NO 3 ) 3 solution for 6 hours, then dried at 80°C for 6 hours after taking it out, and then the surface was loaded with Ni(NO 3 ) 3 The carbon paper is placed in the CVD deposition furnace, under N 2 (6L min -1 ,99.9%) under a protective atmosphere, the temperature was raised to 600°C and kept for a period of 4 hours, and N was introduced for the first 2 hours of the holding period. 2 (3L min -1 ,99.9%), after 2h, the reducing gas H 2 (3L min -1 ,99.9%), then in N 2 (6L min -1 ,99.9%) under a protective atmosphere, the temperature was raised to 800°C, and at C 3 h 6 with N 2 Mixed atmosphere (C 3 h 6 :3L min -1 ; N 2 :4L min -1 ) for 40min; finally in N 2 (6L min -1 ,99.9%) the protective atmosphere dropped to room temperature. Choose 15mol L...

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Abstract

The invention discloses a method for preparing a nitrogen-doped carbon material containing pure pyridine nitrogen on the basis of chemical vapor deposition. The method comprises the following steps: generating carbon nanofibers on the surface of a substrate by virtue of a chemical vapor deposition method, performing corrosion treatment on the carbon nanofibers by adopting a hydrofluoric acid, and performing nitrogen doping on the carbon nanofibers subjected to the corrosion treatment to obtain the nitrogen-doped carbon material. The preparation method is easy to operate, low in cost and suitable for large-scale production; the prepared nitrogen-doped carbon material has the characteristics of large nitrogen doping amount and doping amount controllability, and the application requirement of a fuel cell is met by a pure pyridine nitrogen-containing structure.

Description

technical field [0001] The invention relates to a method for preparing a nitrogen-doped carbon material, in particular to a method for preparing a nitrogen-doped carbon material containing pure pyridine nitrogen based on chemical vapor deposition, and belongs to the technical field of fuel cell catalytic materials. Background technique [0002] In recent years, the rapid reduction of traditional energy sources and the increasing demand for energy have brought great challenges to human beings and society. The development and research of new energy sources have also become the focus of many researchers. Fuel cell technology, as an effective means of hydrogen energy utilization, is one of the power generation devices of renewable energy. It is considered as the energy star of the 21st century and has broad application prospects. The United States has listed fuel cell technology as one of the technologies related to national security, and it was rated as one of the top ten techn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88H01M4/90B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00H01M4/8867H01M4/9083Y02E60/50
Inventor 谢志勇孙敏梁伊丽尹绍峰伍小波邓晓婷温俊园
Owner CENT SOUTH UNIV
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