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Preparation method of cobaltosic-oxide nitrogen-doped graphene synthesized by laser and with adjustable oxygen vacancies

A technology of tricobalt nitrogen oxide and laser synthesis, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of ineffective regulation and control of content, and achieve improved catalytic performance, simple process, and easy operation convenient effect

Inactive Publication Date: 2019-04-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the existing synthesis process cannot synthesize metal oxide composite nitrogen-doped graphene rich in oxygen vacancies at low temperature and low pressure and cannot effectively control the content of oxygen vacancies in the composite system. The irradiation energy and time of the energy laser can adjust the concentration of oxygen vacancies in the composite system and keep the structure of the composite system unchanged, and improve the OER / ORR catalytic performance of the material through the oxygen vacancies created on the surface and the Co-N-C bonds at the interface

Method used

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  • Preparation method of cobaltosic-oxide nitrogen-doped graphene synthesized by laser and with adjustable oxygen vacancies
  • Preparation method of cobaltosic-oxide nitrogen-doped graphene synthesized by laser and with adjustable oxygen vacancies
  • Preparation method of cobaltosic-oxide nitrogen-doped graphene synthesized by laser and with adjustable oxygen vacancies

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Embodiment 1

[0023] A method for preparing laser-synthesized oxygen-vacancy tunable tricobalt tetroxide nitrogen-doped graphene, comprising the following steps:

[0024] (1) Use graphite oxide to ultrasonically disperse in absolute ethanol to make a suspension of 0.33mg / ml, take 24ml of the suspension and add 1.2ml of 0.2M cobalt acetate solution, 0.5ml of 30% NH 4 OH solution and 0.7ml deionized water, oil bath at 80°C for 10h;

[0025] (2) Pour the solution obtained in step (2) into a reaction kettle, and react at 150° C. for 3 hours;

[0026] (3) Perform high-speed centrifugation on the sample obtained in step (3) at 12,000 to 20,000 rpm, then repeatedly wash with deionized water for 3 to 4 times, obtain a precipitate and freeze-dry;

[0027] (4) Mix the sample obtained in step (3) with deionized water in a mass ratio of 1:3 and put it into a test tube. Under magnetic stirring, irradiate the solution with nanosecond parallel pulse laser 15mJ energy for 15min, and the magnetic stirring ...

Embodiment 2

[0030] A preparation method for laser synthesis of oxygen vacancy adjustable tricobalt tetroxide nitrogen-doped graphene, its basic steps are the same as in Example 1, the difference is that in step (4) irradiate the solution with nanosecond parallel pulse laser 75mJ energy for 15min, and then step Same as Example 1.

Embodiment 3

[0032] A preparation method for laser synthesis of oxygen vacancy adjustable tricobalt tetroxide nitrogen-doped graphene, its basic steps are the same as in Example 1, the difference is that in step (4), the solution is irradiated with nanosecond parallel pulse laser 97mJ energy for 5min, and the following steps Same as Example 1.

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Abstract

The invention discloses a preparation method of cobaltosic-oxide nitrogen-doped graphene synthesized by laser and with adjustable oxygen vacancies. The preparation method comprises the following stepsof: using oxidized graphene to ultrasonically disperse in absolute ethyl alcohol, preparing into 0.33mg / ml suspension, taking 24ml suspension, adding 1.2ml 0.2M cobaltous acetate solution, 0.5ml NH4OH solution with the concentration of 30% and 0.7ml deionized water, and carrying out oil bathing for 10 hours at a temperature of 80 DEG C; pouring the solution into a reaction kettle, and reacting for 3 hours at a temperature of 150 DEG C; then carrying out high-speed centrifugation at a speed of 12000-20000r / m, then repeatedly cleaning for 3-4 times by using the deionized water, obtaining precipitates and carrying out freezing and drying; mixing a sample and the deionized water into a test tube according to the mass ratio of 1:2-1:5, and under magnetic stirring, using 15-97mJ energy of nanosecond parallel pulse laser to irradiate the solution for 5-25 minutes; carrying out centrifuging, freezing and drying to obtain the cobaltosic-oxide nitrogen-doped graphene with the adjustable oxygenvacancy. The preparation method disclosed by the invention has the beneficial effects that by adjustment for the irradiation energy and time of low-energy laser, the concentration of the oxygen vacancies in the composite system is adjusted and the unchanged structure of the composite system is maintained.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, in particular to a preparation method for hydrothermally synthesizing oxygen vacancy-adjustable tricobalt tetroxide composite nitrogen-doped graphene by using low-energy laser irradiation. Background technique [0002] Due to the increasingly serious energy crisis and environmental pollution caused by fossil fuels, people pay more and more attention to the development and utilization of renewable energy, which has led to widespread attention to the key technologies of renewable energy conversion and storage, including Fuel cells, metal-air batteries, electrolyzed water, etc., the electrochemical reactions involved include HER, OER and ORR. Due to the slow kinetics of these reactions, it is necessary to look for efficient and cheap electrocatalysts to replace the most active, but expensive and scarce noble metals (Pt, Ru, etc. and their oxides (IrO 2 , RuO 2 ) becomes particularly i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24
CPCB01J27/24
Inventor 杨静刘紫薇杜希文
Owner TIANJIN UNIV
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