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A kind of preparation method of nitrogen-doped porous carbon electrocatalyst with core-shell structure

A technology of nitrogen-doped porous carbon and core-shell structure, which is applied in structural parts, circuits, electrical components, etc., can solve the problems of unfavorable active centers using substrate transport, high raw material costs, and high active layer thickness to achieve excellent reactivity , low price, and improved electrocatalytic performance

Active Publication Date: 2021-11-16
JIAXING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cost of raw materials used in the above method is high, and at the same time, it only has a one-dimensional and two-dimensional structure, and lacks a three-dimensional interconnected material transmission channel.
In addition, the high thickness of the active layer of NPC is not conducive to the utilization of active centers inside NPC and the transport of substrates.

Method used

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  • A kind of preparation method of nitrogen-doped porous carbon electrocatalyst with core-shell structure
  • A kind of preparation method of nitrogen-doped porous carbon electrocatalyst with core-shell structure
  • A kind of preparation method of nitrogen-doped porous carbon electrocatalyst with core-shell structure

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Experimental program
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Effect test

Embodiment 1

[0034] The BC film was cut into pieces (4.0 cm × 8.0 cm), washed with deionized water and put into 30 mL of 0.2 mol / L Zn(NO 3 ) 2methanol solution, then placed in a 50mL stainless steel autoclave, closed reaction at 100°C for 12 hours, then took it out, rinsed it with distilled water, and freeze-dried. The dried product sheet was immersed in 30mL of 0.1mol / L methanol solution of 2-methylimidazole, and reacted at 80°C for 12h, rinsed with distilled water after taking it out, and freeze-dried to obtain ZIF- 8 is the ZIF-8@BC membrane of the shell. The ZIF-8@BC film was placed in a nitrogen atmosphere at a temperature of 3°C / min to 950°C, graphitized at 950°C for 3 hours in a nitrogen atmosphere, and an NPC@CNF carbon film with high conductivity and high electrocatalytic activity was obtained after annealing and cooling , tagged NPC@CNF-950.

[0035] After testing, the coating thickness of the nitrogen-doped porous carbon of the NPC@CNF-950 product is 30-50nm, and the thicknes...

Embodiment 2

[0037] The BC film was cut into pieces, washed with deionized water and put into 30mL 0.1mol / L Zn(NO 3 ) 2 methanol solution, then placed in a 50mL stainless steel autoclave, closed reaction at 100°C for 12 hours, then took it out, rinsed it with distilled water, and freeze-dried. The dried product sheet was immersed in 30mL of 0.1mol / L methanol solution of 2-methylimidazole, and reacted at 80°C for 6h, rinsed with distilled water after taking it out, and freeze-dried to obtain ZIF- 8 is the ZIF-8@BC membrane of the shell. The ZIF-8@BC film was placed in a nitrogen atmosphere at a temperature of 3°C / min to 950°C, graphitized at 950°C for 3 hours in a nitrogen atmosphere, and an NPC@CNF carbon film with high conductivity and high electrocatalytic activity was obtained after annealing and cooling .

[0038] By adjusting the concentration of zinc salt and the reaction time with 2-methylimidazole, the NPC@CNF carbon film product with nitrogen-doped porous carbon coating thickne...

Embodiment 3

[0040] The BC film was cut into pieces, washed with deionized water and put into 30 mL of 0.5 mol / L Zn(NO 3 ) 2 methanol solution, then placed in a 50mL stainless steel autoclave, closed reaction at 100°C for 12 hours, then took it out, rinsed it with distilled water, and freeze-dried. The dried product sheet was immersed in 30 mL of 0.1 mol / L methanol solution of 2-methylimidazole, and reacted at 80°C for 8 hours, rinsed with distilled water after taking it out, and freeze-dried to obtain ZIF- 8 is the ZIF-8@BC membrane of the shell. The ZIF-8@BC film was placed in a nitrogen atmosphere at a rate of 6°C / min to 1100°C, graphitized at 1100°C for 6 hours in a nitrogen atmosphere, and an NPC@CNF carbon film with high conductivity and high electrocatalytic activity was obtained after annealing and cooling , labeled NPC@CNF-1100.

[0041] By adjusting the concentration of zinc salt and the reaction time with 2-methylimidazole, the NPC@CNF-1100 carbon film product with a coating ...

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Abstract

The invention relates to the technical field of inorganic materials and aims to provide a method for preparing a nitrogen-doped porous carbon electrocatalyst with a core-shell structure. Including: placing bacterial cellulose film on Zn(NO 3 ) 2 The closed reaction in the methanol solution, the product is immersed in the methanol solution of 2-methylimidazole to react after cleaning and freeze-drying; then after cleaning and freeze-drying, the bacterial cellulose / ZIF-8 macroscopic three-dimensional composite film is obtained; Burning in a nitrogen atmosphere, annealing and cooling to obtain a nitrogen-doped porous carbon electrocatalyst with a core-shell structure. The invention uses bacterial cellulose as a starting material, has wide sources and low price, and has a three-dimensional interconnected pore structure, which is beneficial to the efficient transmission of reaction substrates. Composite materials with different ZIF‑8 shell thicknesses can be tuned to tune the catalytic activity of porous carbon electrocatalysts. After combining CNF and NPC, the electrocatalytic performance is significantly improved, showing excellent catalytic activity in the oxygen reduction reaction, and also showing excellent activity in the oxygen evolution reaction.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and in particular relates to a preparation method of a nitrogen-doped porous carbon electrocatalyst with a core-shell structure. Background technique [0002] The oxygen reduction reaction (Oxygen Reduction Reaction, ORR) on the "three-phase interface" of the fuel cell cathode catalyst is an important constraint factor for the performance improvement of the entire battery. one of the reasons. The nitrogen-doped porous carbon (Nitrogen-doped Porous Carbon, NPC) material obtained after high-temperature carbonization using metal-organic frameworks (Metal-Organic Frameworks, MOFs) rich in nitrogen atoms as a precursor has a large specific surface area and active sites. It is a potential electrocatalytic material to replace noble metals. However, in the process of preparing NPC with MOFs, the degree of graphitization of NPC is often increased by increasing the annealing temperature, ther...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88H01M4/96H01M4/90
CPCH01M4/8825H01M4/8842H01M4/8882H01M4/9083H01M4/96Y02E60/50
Inventor 李以名曹雪波汪建平牛瑛山
Owner JIAXING UNIV
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