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Fullerene-based Fe and N-doped porous carbon material as well as preparation method and application thereof

A technology based on fullerene and fullerene derivatives, which is applied in the direction of fuel cell half-cells and primary battery half-cells, structural parts, electrical components, etc. The electrocatalytic oxygen reduction performance is backward, the half-wave potential is low, and there is no innovation, etc., to achieve the effect of good regularity, excellent uniformity, and moderate size

Active Publication Date: 2020-12-01
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

A recent work prepared mesoporous fullerene / Cu-Cu 2 O hybrid materials to promote the chemical adsorption of oxygen molecules in the initial stage of oxygen reduction, and tested the half-wave potential of 0.76V, but the above-mentioned technologies all have the problem of low half-wave potential, so the current carbon materials based on fullerene Morphology and structure design, heteroatom doping and electrocatalytic oxygen reduction performance are still lagging behind, and there is a lack of innovation in micro-nano structure

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  • Fullerene-based Fe and N-doped porous carbon material as well as preparation method and application thereof
  • Fullerene-based Fe and N-doped porous carbon material as well as preparation method and application thereof
  • Fullerene-based Fe and N-doped porous carbon material as well as preparation method and application thereof

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preparation example Construction

[0033] Such as figure 1 As shown, the embodiment of the present invention provides a method for preparing a fullerene-based Fe, N-doped porous carbon material, the method comprising the following steps:

[0034] S1 Use benzene solvent as a good solvent to dissolve the fullerene derivative, then mix it with an alcohol solvent as a poor solvent, let it stand at room temperature for 12 to 24 hours, then filter to obtain the precipitate, and dry the precipitate under vacuum for 8 Hours to 12 hours to prepare the precursor; among them, the solubility of fullerene molecules can be reduced by mixing a good solvent and a poor solvent in which fullerene molecules are dissolved. Under the action of van der Waals force, fullerene molecules self-assemble to form Micro-nano structure with three-dimensional hierarchical growth;

[0035]S2 In an ammonia atmosphere, the precursor is calcined at 600 ° C to 800 ° C for a preset time, so that the phase transition of the fullerene crystal occurs...

Embodiment 1

[0043] S1 Measure cumene 15mL and chlorobenzene 10mL respectively and mix them as a good solvent, weigh 20mg of ferrocenylpyrrolidine C 60 Dissolve in a good solvent and filter twice with a 0.22 micron organic filter to form a dark brown transparent solution; inhale the solution with a syringe and slowly inject 50mL of ethanol along the container wall; seal the above mixed solution at room temperature for 24 hours , a dark brown precipitate was obtained at the bottom of the container; the precipitate was collected at a centrifuge speed of 6000r / min and vacuum-dried at 40°C for 10 hours to obtain a three-dimensional hierarchically grown micro-nano structure, that is, a precursor;

[0044] S2 Place the obtained precursor product in a quartz crucible, raise the temperature to 600°C at a rate of 4°C / min in an ammonia flow rate of 50mL / min and keep it warm for 2 hours to obtain a black powder product, and obtain a fullerene-based Fe , N-doped porous carbon material.

Embodiment 2

[0046] S1 Measure cumene 10mL and chlorobenzene 10mL respectively and mix them as a good solvent, weigh 15mg of ferrocenylpyrrolidine C 60 Dissolve in a good solvent and filter twice with a 0.22 micron organic filter to form a dark brown transparent solution; inhale the solution with a syringe and slowly inject 60mL of ethanol along the container wall; seal the above mixed solution at room temperature for 12 hours , a dark brown precipitate was obtained at the bottom of the container; the precipitate was collected at a centrifuge speed of 6000r / min and vacuum-dried at 40°C for 12 hours to obtain a three-dimensional hierarchically grown micro-nano structure, that is, a precursor;

[0047] S2 Place the obtained precursor product in a corundum crucible, raise the temperature to 700°C at a rate of 5°C / min in an ammonia flow rate of 50mL / min and keep it warm for 3 hours to obtain a black powder product, and obtain a fullerene-based Fe , N-doped porous carbon material.

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Abstract

The invention belongs to the field of carbon composite materials, and discloses a fullerene-based Fe and N-doped porous carbon material as well as a preparation method and application thereof. The method comprises the following steps of: dissolving a fullerene derivative by taking a benzene solvent as a good solvent, then mixing the dissolved fullerene derivative with an alcohol solvent as a poorsolvent, making the mixture standing still at room temperature for a preset time, filtering to obtain a precipitate, and drying the precipitate under a vacuum condition for a preset time to obtain a precursor; and calcining the precursor in an ammonia atmosphere for a preset time to finally prepare the fullerene-based Fe and N-doped porous carbon material. According to the method provided by the invention, a micro-nano structure with three-dimensional graded growth can be formed through intermolecular self-assembly of the fullerene; and fullerene molecules contain N and Fe, and the micro-nanostructure subjected to high-temperature annealing treatment in an ammonia atmosphere has a pore structure in graded distribution, short-range ordered nano graphene sheets and high-content nitrogen doping, so that the N and Fe co-doped three-dimensional graded carbon composite material is prepared.

Description

technical field [0001] The invention belongs to the field of carbon composite materials, and more specifically relates to a fullerene-based Fe and N-doped pore-rich carbon material and a preparation method and application thereof. Background technique [0002] Driven by the growing fossil energy crisis, existing technologies have made significant investments in renewable energy sources such as metal-air batteries and fuel cells. However, the cathodic oxygen reduction reaction (ORR) limits its overall efficiency for kinetically hysteretic reactions and overpotentials. The noble metal platinum exhibits the highest kinetic activity in the ORR catalytic reaction, but its large-scale commercial application is hindered by high cost, poor long-term stability, and poor resistance to methanol. In addition, considering oxophilic transition metal compounds (such as Fe 3 o 4 Nanoparticles) and N-doped carbon substrates, metal / nitrogen-carbon series carbon materials have become promis...

Claims

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Application Information

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IPC IPC(8): H01M4/96H01M4/88H01M12/06
CPCH01M4/96H01M4/8825H01M4/8882H01M12/06Y02E60/50
Inventor 彭平彭志遥李芳芳
Owner HUAZHONG UNIV OF SCI & TECH
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