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Metal single atom doped graphene preparation method

A graphene and atom technology, applied in non-metallic elements, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of poor stability, high cost, low activity, etc., and achieve enhanced adsorption, simple operation, and easy amplification of the process. Effect

Active Publication Date: 2019-05-31
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of efficient, stable, easy industrialized controllable method for preparing metal single atom doped graphene, to solve the low activity of catalysts used in selective organic synthesis, metal-air batteries, pollutant degradation, etc. Problems such as poor stability and high cost, and the first realization of the preparation of high-content metal single atom doped graphene structure

Method used

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  • Metal single atom doped graphene preparation method

Examples

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Effect test

Embodiment 1

[0035] Take 5 g of urea and 50 mg of ferric nitrate, add 50 ml of water to dissolve it, stir it magnetically for 2 hours and mix well, dry at 80°C for 4 hours, grind uniformly to obtain a red powder, put it in the furnace with argon as protective gas ( The gas flow rate is 200 sccm), the temperature is raised to 300° C. at a heating rate of 10° C. / min, and the heat treatment is performed in an argon atmosphere for 3 hours, and then it is lowered to room temperature to obtain a yellow sample.

[0036] Take 2g of the above yellow sample and 150 mg of functionalized redox graphene (redox graphene has a carbon to oxygen atomic ratio of 4:1, polyvinylpyrrolidone / redox graphene is 2wt%), and mix them thoroughly in an ethanol solution 2 Dry in an oven at 80°C to obtain a gray sample. Put the gray sample into the furnace, use argon as the protective gas (gas flow rate is 300sccm), heat up to 800℃ at a heating rate of 5℃ / min, heat treatment under argon atmosphere for 1 hour, and then lowe...

Embodiment 2

[0040] Take 3 g of melamine and 100 mg of cobalt chloride, add 60 ml of water to dissolve it, stir it magnetically for 2 hours and mix well, dry it at 80°C for 4 hours, grind it evenly to obtain light red powder, put it in the furnace and protect it with argon The temperature was increased to 330°C at a temperature increase rate of 10°C / min, and the temperature was heated to 330°C under argon atmosphere, and then lowered to room temperature to obtain a yellow sample.

[0041] Take 2g of the above yellow sample and 300 mg of functionalized redox graphene (redox graphene has a carbon-to-oxygen ratio of 10:1, polyaniline / redox graphene is 3wt%) and mixed thoroughly in ethanol solution for 2 hours, Dry in an oven at 80°C to obtain a gray sample. Put the gray sample in the furnace, use argon as the protective gas (gas flow rate is 200sccm), heat up to 900°C at a heating rate of 4°C / min, heat treatment at 900°C in an argon atmosphere for 1 hour, and then lower to room temperature. A b...

Embodiment 3

[0045] Take 2 g of dicyandiamide and 20 mg of nickel nitrate, add 60 ml of water to dissolve it, stir it magnetically for 3 hours and mix well, dry it at 80°C for 4 hours, grind it evenly to obtain a light red powder, put it in the furnace with argon With shielding gas (gas flow rate of 300 sccm), the temperature was increased to 360° C. at a temperature increase rate of 10° C. / min, and the heat treatment was performed for 2 hours in an argon atmosphere, and then lowered to room temperature to obtain a yellow sample.

[0046] Take 2g of the above yellow sample and 300mg of polyaziridine (PEI) functionalized nitrogen-doped graphene (nitrogen-doped graphene contains 7wt% nitrogen and PEI / nitrogen-doped graphene is 3wt%) in ethanol The solution was mixed thoroughly for 1 hour and dried in an oven at 80°C to obtain a gray sample. Put the gray sample into the furnace, use argon as the protective gas (gas flow rate is 300sccm), heat up to 850°C at a heating rate of 5°C / min, heat treatm...

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Abstract

The invention relates to the field of metal single atom doped carbon materials, in particular to a controllable-supporting-amount metal single atom doped graphene preparation method. Surface functionalized graphene serves as a matrix, organic atomic dispersion metal salts including carbon nitride, melamine, amino acid, thiourea, urea, dicyandiamide, polyvinylpyrrolidone and the like serve as intermediates, and pyrolysis is performed in a protective atmosphere to obtain a series of metal single atom doped graphene structures. The method has advantages that graphene serves as the matrix, atomicmonodispersion of metal salts is realized by organics, and metal single atom doped graphene controllable in content and type is finally obtained through secondary pyrolysis. By the method, problems oflow doping amount, proneness to aggregation, uncontrollability and the like of metal single atoms are effectively solved.

Description

Technical field [0001] The invention relates to the field of metal monoatom doped carbon materials, in particular to a method for preparing metal monoatom doped graphene with a controllable loading amount. Background technique [0002] Catalysts are widely used in all walks of life around the world, and the catalytic process is closely related to people's daily production and life. How to prepare high-quality, high-activity catalysts is a key factor restricting the development of many industrial processes and related fields. Because different reaction processes are very different, the types and components of catalysts required are also different. A key factor that determines the performance of the catalyst is the number and concentration of reactive sites. Generally speaking, as the size of the catalyst particles decreases, the number and ratio of catalytic active sites will increase. Therefore, how to reduce the size of catalysts, from macroscopic particles to microscopic part...

Claims

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Application Information

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IPC IPC(8): C01B32/194
CPCY02E60/50
Inventor 刘畅赵石永薛梦瑶成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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