Metal@graphitized carbon/graphene composite electrocatalyst material and its preparation method

A metal compound and composite electricity technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve environmental pollution, reduce the ratio of M/C heterojunctions, and increase the thickness of carbon shells, etc. problems, to achieve the effect of rich raw material resources, high catalytic activity, and high interface ratio

Active Publication Date: 2021-03-30
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, those synthesized by this method are usually discrete metal (or metal compound) nanoparticles or pomegranate-like M@C aggregates wrapped in carbon tubes, and the thickness of the carbon shell is usually very large.
This will not only greatly reduce the ratio to the M / C heterojunction that can participate in the electrocatalytic reaction, but also reduce the intrinsic activity of the M / C heterojunction
In addition, this method requires a long high-temperature reaction time and a large amount of inert gas consumption, which undoubtedly greatly increases its preparation cost and makes its industrialization process extremely slow.
In addition, when adjusting the components on both sides of M / C, it is likely to introduce and produce a lot of toxic and corrosive substances and gases such as ammonia and phosphine, which will not only cause great damage to the heating equipment , will also cause serious environmental pollution

Method used

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  • Metal@graphitized carbon/graphene composite electrocatalyst material and its preparation method
  • Metal@graphitized carbon/graphene composite electrocatalyst material and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A 4 mg / mL GO aqueous solution was obtained by the modified hummers method. Add 0.02 mL of 0.5 M potassium ferrocyanide solution to 1 mL of GO aqueous solution under stirring, shake well and add 0.2 mL of 0.5 M nickel chloride solution to it to obtain nickel ferrocyanide / graphene composite, and Wash 3 times with water. The resulting nickel ferrocyanide / graphene composite was dispersed in 1 mL of water, frozen with liquid nitrogen, and then lyophilized in a cold desiccator for 16-24 hours to obtain a nickel ferrocyanide / graphene sponge ( figure 1 ).

[0028] Transfer the above nickel ferrocyanide / graphene sponge into a glove box containing argon and seal it in a 50 mL quartz vial containing a small amount of carbon cloth. Then put the above-mentioned quartz bottle in a household microwave oven, and use 1000 W of power radiation for 10 s to obtain FeNi@nitrogen-doped grapheneized carbon / graphene composite catalyst ( figure 1 a). As an OER catalyst, it obtains 10mA cm ...

Embodiment 2

[0030] A 4 mg / mL GO aqueous solution was obtained by the modified hummers method. Add 0.02 mL of 0.5 M potassium ferrocyanide solution to 1 mL of GO aqueous solution under stirring, shake well and then add 0.2 mL of 0.5 M nickel chloride solution to obtain nickel ferrocyanide / graphene composite, and Wash 3 times with water. The obtained nickel ferrocyanide / graphene composite was dispersed in 1 mL of 0.6 M urea aqueous solution, frozen with liquid nitrogen, and then lyophilized in a cold desiccator for 16-24 hours to obtain nickel ferrocyanide / graphene containing urea. Graphene Sponge ( figure 1 ).

[0031] Transfer the above-mentioned nickel ferrocyanide / graphene sponge containing urea into a glove box containing argon and seal it in a 50 mL quartz vial containing a small amount of carbon cloth. Then put the above-mentioned quartz bottle in a household microwave oven, and use 1000 W of power to irradiate for 10 s to obtain FeNi nitride@nitrogen-doped graphene-based carbon / g...

Embodiment 3

[0033]A 4 mg / mL GO aqueous solution was obtained by the modified hummers method. Add 0.02 mL of 0.5 M potassium ferrocyanide solution to 1 mL of GO aqueous solution under stirring, shake well and then add 0.2 mL of 0.5 M nickel chloride solution to obtain nickel ferrocyanide / graphene composite, and Wash 3 times with water. The obtained nickel ferrocyanide / graphene composite was dispersed in 1 mL of 0.6 M sodium hypophosphite aqueous solution, frozen with liquid nitrogen, and then lyophilized in a cold desiccator for 16-24 hours to obtain ferrous iron containing sodium hypophosphite Nickel cyanide / graphene sponge ( figure 1 ).

[0034] Transfer the above nickel ferrocyanide / graphene sponge containing sodium hypophosphite into a glove box containing argon and seal it in a 50 mL quartz vial containing a small amount of carbon cloth. Then put the above-mentioned quartz bottle in a household microwave oven, and use 1000 W power to irradiate for 10 s to obtain FeNi phosphide@nitr...

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Abstract

The invention belongs to the technical field of electro-catalytic materials and particularly relates to a metal@ graphitized carbon / graphene compound electro-catalyst material and a preparation methodthereof. The preparation method provided by the invention comprises the following steps: firstly, synthesizing a metal-organic framework (MOF) / graphene compound by adopting an excess metal-induced compound strategy, and then, converting MOF to metal and carbon-containing gas by utilizing the high temperature instantaneously generated by the microwave adsorption heating effect of graphene so as torealize second-level synthesis similar to chemical vapor deposition of metal@ graphitized carbon with a core-shell structure, thereby obtaining the metal@ graphitized carbon / graphene compound. A series of metals and metal compound@ heterogeneous atom doped graphitized carbon shell / graphene compounds with the core-shell structure are obtained by changing the components of the MOF or introducing precursors of elements such as N, P, S and B in a microwave process. The preparation method provided by the invention is simple in process and low in cost, and raw material resources are rich; and the prepared electro-catalyst material has high catalytic activity and long cycle life and can serve as a next-generation catalyst material for water decomposition equipment, metal-air cells and fuel cells.

Description

technical field [0001] The invention belongs to the technical field of electrocatalyst materials, and in particular relates to HER, OER and ORR electrocatalyst materials and preparation methods thereof. Background technique [0002] With the increasing energy crisis and environmental pollution, the development of efficient energy storage and conversion technologies including water splitting devices, metal-air batteries and fuel cells is inevitable. The development of these devices strongly relies on the development of catalysts for the hydrogen evolution reaction (HER), oxygen evolution reaction (OER), and oxygen reduction reaction (ORR). However, currently commercially available catalysts are mainly high-cost catalysts based on noble metals and noble metal oxides, which greatly limits the further development of these devices. Therefore, the development of low-cost catalysts with similar catalytic activity to noble metals and noble metal oxides is a current research hotspot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/08C25B1/04C25B11/091H01M4/90
CPCB01J27/24B01J35/0033B01J35/08C25B1/04C25B11/04H01M4/9041H01M4/9083Y02E60/36Y02E60/50
Inventor 徐宇曦卜凡兴
Owner FUDAN UNIV
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