Iron-nitrogen-doped graphene porous material with dual-site catalytic oxygen reduction activity, and preparation method and application therefor

A porous material and graphene technology, applied in the field of nanomaterials, can solve the problems of low specific surface area and limitation, achieve large specific surface area, enrich active sites, and improve electrochemical activity

CN105609793AInactive Publication Date: 2016-05-25FUDAN UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2016-05-25
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention belongs to the technical field of a nanomaterial, and specifically relates to an iron-nitrogen-doped graphene porous material with dual-site catalytic oxygen reduction activity, and a preparation method and an application therefor. The porous material is formed by embedding graphite-carbon-coated iron carbide into a nitrogen-doped porous graphene band network structure; the preparation method for the iron-nitrogen-doped graphene porous material comprises the steps of preparing a graphene oxide solution; adding a proper amount of conductive macromolecular pyrrole to the graphene oxide solution; obtaining uniform hydrogel through a hydrothermal process; performing oxidative polymerization on the hydrogel by ferric iron; then dispersing the hydrogel into a fresh ferric iron solution to complete adsorption; then performing drying and high-temperature carbonization thermal processing; and finally removing non-active and free iron phase from the reaction system by dilute acid so as to obtain the iron-nitrogen-doped graphene porous material. The porous material can be used as the negative electrode catalyst for a fuel cell, and shows quite high catalytic oxygen reduction activity, so that the porous material has quite important research meaning and bright application prospects.
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Description

technical field

[0001] The invention belongs to the technical field of nanomaterials, and in particular relates to an iron-nitrogen-doped graphene porous material with double-site catalyzed oxygen reduction and its preparation method and application. Background technique

[0002] With the rapid development of modern industry, people's demand for energy is also increasing. Due to its high energy density and power density, fuel cells have gradually become a new type of clean and alternative energy storage. Among the components of a fuel cell, the cathode catalyst of its electrode is an extremely important central component and often determines the final performance of the fuel cell. Although noble metal platinum and its complexes have long been regarded as excellent catalyst materials due to their high catalytic activity, their high production cost and low chemical stability greatly limit their popularization. Therefore, there is an urgent need to find a cathode replacement ...

Examples

Embodiment 1

[0060] (1) Take 10mL of 1mg / mL graphene oxide nanoribbon aqueous solution, add 4vol% of pyrrole, and ultrasonically disperse until a uniform suspension is formed 1.

[0061] (2) The suspension 1 was sealed in a 20mL autoclave, and placed in an oven at 80°C for 12 hours to obtain a graphene oxide nanoribbon / pyrrole composite hydrogel with good mechanical properties.

[0062] (3) Disperse the obtained hydrogel in 25mL of 0.24M ferric chloride solution, stir for 1-12h to complete the polymerization reaction, and then wash the obtained sample with distilled water and absolute ethanol (to remove the by-products of the polymerization reaction and unreacted pyrrole monomer). Then the washed sample was redispersed in 50mL of 0.24M ferric chloride solution, stirred and reacted for 1-12h, and the adsorption of ferric iron was completed. Finally, the wet hydrogel is obtained by filtration.

[0063] (4) Add tert-butanol to the wet hydrogel, pour out the tert-butanol after soaking for 5 ...

Embodiment 2

[0067] (1) Take 10mL of 5mg / mL graphene oxide nanobelt aqueous solution, add 8vol% pyrrole, and disperse ultrasonically until a uniform suspension is formed 2.

[0068] (2) The suspension 2 was sealed in a 20mL autoclave, and reacted in an oven at 100°C for 6h to obtain a graphene oxide nanoribbon / pyrrole composite hydrogel with better mechanical properties.

[0069] (3) Disperse the obtained hydrogel in 50mL of 0.24M ferric nitrate solution, stir the reaction for 1-12h to complete the polymerization reaction, and then wash the obtained sample with distilled water and absolute ethanol (to remove the by-products of the polymerization reaction and unused reacted pyrrole monomer). Subsequently, the washed sample was redispersed in 100mL of 0.24M ferric nitrate solution, stirred and reacted for 1-12h, and the adsorption of ferric iron was completed. Finally, the wet hydrogel is obtained by filtration.

[0070] (4) Add ethanol to the wet hydrogel, pour out the ethanol after soaking...

Embodiment 3

[0074] (1) Take 10mL of 10mg / mL graphene oxide nanobelt aqueous solution, add 12vol% pyrrole, and disperse ultrasonically until a uniform suspension is formed 3.

[0075] (2) The suspension 3 was sealed in a 20mL autoclave, and reacted in an oven at 120°C for 6h to obtain a graphene oxide nanoribbon / pyrrole composite hydrogel with better mechanical properties.

[0076] (3) Disperse the obtained hydrogel in 100mL of 0.24M ferric sulfate solution, stir for 2-10h to complete the polymerization reaction, and then wash the obtained sample with distilled water and absolute ethanol (to remove the by-products of the polymerization reaction and unused reacted pyrrole monomer). Then redisperse the washed sample in 200mL 0.24M ferric sulfate solution, stir and react for 2-10h to complete the adsorption of ferric iron. Finally, the wet hydrogel is obtained by filtration.

[0077] (4) Add tert-butanol to the wet hydrogel, pour out the tert-butanol after soaking for 10 hours, repeat 3 tim...