Hydrothermal synthesis method of a nitrogen-doped graphene-supported cobalt oxygen reduction reaction electrocatalyst

A technology of nitrogen-doped graphene and electrocatalyst, which is applied in the direction of circuits, electrical components, battery electrodes, etc., can solve the problems of conductivity and catalytic stability defects, and achieve simple and easy-to-control preparation methods, high selectivity, and excellent reaction conditions mild effect

Active Publication Date: 2019-07-19
HEFEI UNIV OF TECH
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  • Abstract
  • Description
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Problems solved by technology

Transition metal compounds mainly include transition metal sulfides, transition metal oxides (including spinel type and perovskite type) and transition metal complexes (Feng Y J et al, Fuel Cells, 2000, 10(1), 77- 83; Wu Z S et al, Journal of the American Chemical Society, 2012, 134, 9082-9085; Liang Y et al, Nature Materials, 2011, 10, 780-786), this type of transition metal compound as an electrocatalyst in the conductivity and catalytic stability Sexuality and other aspects also have certain defects

Method used

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  • Hydrothermal synthesis method of a nitrogen-doped graphene-supported cobalt oxygen reduction reaction electrocatalyst
  • Hydrothermal synthesis method of a nitrogen-doped graphene-supported cobalt oxygen reduction reaction electrocatalyst
  • Hydrothermal synthesis method of a nitrogen-doped graphene-supported cobalt oxygen reduction reaction electrocatalyst

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Embodiment 1

[0034] 1. Using graphite powder with a particle size of less than 20 μm as raw material, graphene oxide (GO) was prepared by the conventional Hummer method;

[0035] 2. Mix and grind GO and urea according to the mass ratio of 1:10, put them into a 160°C oven for nitrogen-doped heat treatment for 6 hours, and after cooling, crush the nitrogen-doped GO and wash it with deionized water, and then add it into deionized water for ultrasonic dispersion The concentration in 0.5h is 1.5g·L -1 uniform dispersion liquid; add 0.5 times GO quality cobalt nitrate crystals to the dispersion liquid, stir and disperse evenly, then transfer the mixed liquid into a hydrothermal reaction kettle, and conduct a hydrothermal reaction at 160°C for 12 hours; after cooling, open the reaction kettle and add Hydrazine hydrate with 15 times the quality of GO, adjust the pH value of the solution to 10 with ammonia water, seal the reaction vessel, and perform hydrothermal reduction reaction at 180°C for 10 ...

Embodiment 2

[0039] 1. Using graphite powder with a particle size of less than 20 μm as raw material, graphene oxide (GO) was prepared by the conventional Hummer method;

[0040] 2. Mix and grind GO and urea according to the mass ratio of 1:3, put them into an oven at 180°C for nitrogen-doped heat treatment for 4 hours, and after cooling, crush the nitrogen-doped GO and wash it with deionized water, then add it into deionized water for ultrasonic dispersion The concentration in 0.5h is 1.5g·L -1 The uniform dispersion liquid; transfer the dispersion liquid into a hydrothermal reaction kettle, and conduct a hydrothermal reaction at 140°C for 4 hours; open the reaction kettle after cooling, adjust the pH value of the solution to 10 with ammonia water, add hydrazine hydrate 10 times the quality of GO and seal it Reaction kettle, hydrothermal reduction reaction at 110°C for 4h, the reaction solution was cooled and filtered under reduced pressure, washed twice with deionized water and absolute ...

Embodiment 3

[0045] 1. Using graphite powder with a particle size of less than 20 μm as raw material, graphene oxide (GO) was prepared by the conventional Hummer method;

[0046] 2. Mix and grind GO and urea according to the mass ratio of 1:5, put them into an oven at 120°C for nitrogen-doped heat treatment for 24 hours, and after cooling, crush the nitrogen-doped GO and wash it with deionized water, then add it into deionized water for ultrasonic dispersion The concentration in 0.5h is 1.5g·L -1 A homogeneous dispersion liquid; add cobalt acetate crystals twice the quality of GO to the dispersion liquid, stir and disperse evenly, transfer the mixed liquid into a hydrothermal reaction kettle, and conduct a hydrothermal reaction at 200°C for 4 hours; open the reaction kettle after cooling, and add Hydrazine hydrate with 40 times the quality of GO, adjust the pH value of the solution to 10 with ammonia water, seal the reaction vessel, and perform hydrothermal reduction reaction at 140°C for ...

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Abstract

The invention discloses a hydrothermal synthesis method for a nitrogen-doping graphene-loaded cobalt oxygen reduction reaction electrocatalyst. The hydrothermal synthesis method comprises the steps of fully mixing and placing GO (graphene oxide) and urea in a baking oven for nitrogen-doping thermal treatment; smashing and adding the nitrogen-doping GO into deionized water for ultrasound dispersion for 0.5 hour, transferring the obtained product to a hydrothermal reaction kettle, performing magnetic stirring for 20 minutes, adding a cobalt salt, continuing to stir for 10 minutes, and sealing the reaction kettle for hydrothermal reaction; and adding hydrazine hydrate after the hydrothermal reaction is completed, adjusting pH of a solution to be 10 with concentrated ammonia water, sealing the reaction kettle, and continuing hydrothermal reduction reaction to obtain a nitrogen-doping graphene-loaded cobalt composite material. The nitrogen-doping graphene-loaded cobalt composite material prepared according to the method is used as the oxygen reduction reaction electrocatalyst, a cyclic voltammetry reduction peak potential in 0.1M of KOH solution is -0.18V (vs.Ag / AgCl), and an initial potential is -0.1V (vs.Ag / AgCl).

Description

[0001] 1. Technical field [0002] The invention relates to a synthesis method of an electrocatalyst for an oxygen reduction reaction, in particular to a hydrothermal synthesis method of an electrocatalyst for a nitrogen-doped graphene-supported cobalt oxygen reduction reaction. [0003] 2. Background technology [0004] Among the electrocatalysts for oxygen reduction reaction, Pt and Pt-based metal-supported carbon composites are currently the most commonly used and have the best catalytic activity. Researchers have carried out a lot of research work in reducing the cost of oxygen reduction reaction electrocatalysts, finding new preparation methods and new support materials, which can be roughly divided into Pt-based and non-Pt-based catalysts. [0005] The work of Pt-based catalysts is mainly to dope Fe, Co, Ni, Cu and other non-noble metals on the basis of Pt / C (Niu Get al, Nano Letters, 2016, 16(6), 3850-3857; Salgadoa J et al, Applied Catalysis B: Environmental, 2005, 57(...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/90
CPCH01M4/90H01M4/9083Y02E60/50
Inventor 翟林峰王冉孙敏
Owner HEFEI UNIV OF TECH
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