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Preparation method of mono-atomic metal-carbon composite catalyst for electro-catalytic reactions

An electrocatalysis, carbon composite technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the problem of increased specific surface area and poor conductivity of metal oxides. Good and unsuitable electrocatalysts, etc.

Inactive Publication Date: 2017-07-14
INST OF NEW ENERGY SHENZHEN
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Problems solved by technology

On the other hand, the specific surface area of ​​single-atom catalysts increases sharply when the metal particles are reduced to the single-atom level, resulting in a sharp increase in the free energy of the metal surface, and it is easy to agglomerate and couple to form large clusters during preparation and reaction, resulting in catalyst deactivation
[0005] In addition, although carbon materials have the advantages of good electrical conductivity and large specific surface area, they have fewer surface adsorption sites. Therefore, the current single-atom-supported catalysts mainly use metal oxides as supports. However, metal oxides have poor conductivity and are also Not suitable as a support for electrocatalysts

Method used

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  • Preparation method of mono-atomic metal-carbon composite catalyst for electro-catalytic reactions
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  • Preparation method of mono-atomic metal-carbon composite catalyst for electro-catalytic reactions

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[0025] An embodiment of the present invention provides a method for preparing a single-atom metal-carbon composite catalyst for electrocatalytic reactions, which includes the following steps:

[0026] S01. Mix the carbon material with the nitrogen source, under the protection of nitrogen, burn at 500°C-900°C for 1-5 hours, then raise the temperature to 1050°C-1150°C and burn for 1-5 hours, and finally cool down to room temperature to obtain the purpose carbon materials;

[0027] S02. Dissolving transition metal nitrate and / or acetate in the first volatile solvent to form a metal single atom source solution; uniformly dispersing the target carbon material in the second volatile solvent to form a dispersed Carbon material solution; while stirring, add the metal single atom source solution dropwise to the dispersed carbon material solution, and stir until the first volatile solvent and the second volatile solvent are completely volatilized Finally, stop stirring to obtain a meta...

Embodiment 1

[0037] Mix 100mg of graphene and 100mg of melamine evenly, place in a tube furnace, heat to 750 degrees Celsius under a nitrogen atmosphere, burn for 2 hours, then heat up to 1050 degrees Celsius, burn for 2 hours, and finally drop to room temperature, A sample was removed and labeled DG. Ultrasonically disperse 3 mg of DG powder in 10 mL of ethanol solution, and add dropwise 0.034 mL of ethanol solution of nickel nitrate with a concentration of 0.1 M (ie mol / L, the same below). The mixed solution was stirred, and after 24 hours, the solvent evaporated completely to obtain a precipitate, which was transferred to a tube furnace, and burned for 2 hours at 750 degrees Celsius under nitrogen protection to obtain a graphene-supported nickel nanoparticle material (Ni @DG). Finally, the sample was placed in a hydrochloric acid solution with a concentration of 1M and stirred for 48 hours, washed several times with deionized water, and dried to obtain a graphene-supported single-atom ...

Embodiment 2

[0041] Mix 100mg of commercial graphene and 100mg of melamine evenly, place in a tube furnace, heat to 750 degrees Celsius under nitrogen atmosphere, burn for 2 hours, then raise the temperature to 1050 degrees Celsius, burn for 2 hours, and finally cool down to room temperature , a sample was taken and labeled DG. 3 mg of DG powder was ultrasonically dispersed in 10 mL of ethanol solution, and 0.034 mL of 0.1 M ferric nitrate solution in ethanol was added dropwise. The mixed solution was stirred, and the solvent evaporated completely after 24 hours to obtain a precipitate, which was transferred to a tube furnace and burned for 2 hours at 750 degrees Celsius under the condition of nitrogen protection to obtain iron nanoparticles supported graphene ( Fe@DG). Finally, the sample was placed in a hydrochloric acid solution with a concentration of 1M and stirred for 48 hours, washed several times with water, and dried to obtain a single-atom nickel-supported graphene material (HCl...

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Abstract

The invention discloses a preparation method of a mono-atomic metal-carbon composite catalyst for electro-catalytic reactions. The preparation method comprises the following steps: dropwise adding a mono-atomic metal source solution into a dispersed carbon material solution, stirring the solution until a first volatile solvent and a second volatile solvent are completely evaporated to obtain a carbon material loaded on metal salts, burning the carbon material loaded on metal salts at a temperature of 500 to 1000 DEG C under the protection of inert gas to obtain a carbon material loaded on metals (simple substance), and dipping the carbon material loaded on metals in an acid solution so as to remove the metals to obtain the mono-atomic metal-carbon composite catalyst. The catalyst has a high catalytic activity and does not need the assistance of precious metals, the cost is low, and the operation is simple.

Description

technical field [0001] The invention relates to a catalyst for an electrocatalytic reaction, in particular to a method for preparing a single-atom metal-carbon composite catalyst used for an electrocatalytic reaction. Background technique [0002] Hydrogen energy is considered to be one of the most promising energy sources in the 21st century. Hydrogen energy is an extremely superior new energy source. Its main advantages are: high combustion calorific value, clean and pollution-free, abundant resources, and wide application range. Hydrogen is stored in the vast ocean. If the hydrogen is extracted, there will be about 1.4×10 17 tons, generating 9,000 times as much heat as fossil fuels on Earth. The key technology to develop hydrogen energy includes two aspects: on the one hand, it needs to solve the problem of hydrogen production; on the other hand, it needs to improve the application efficiency of hydrogen energy in fuel cells. Whether hydrogen can be widely used, the ch...

Claims

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Application Information

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IPC IPC(8): B01J23/745B01J23/755B01J23/889B01J27/22
CPCB01J23/745B01J23/755B01J23/889B01J27/22B01J37/009B01J37/06B01J37/082B01J35/399B01J35/393B01J35/33
Inventor 姚向东贾毅张龙舟严学成茆胜
Owner INST OF NEW ENERGY SHENZHEN
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