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Cu-N-C oxygen reduction catalyst and preparation method thereof

A catalyst, cu-n-c technology, which is applied in electrical components, battery electrodes, circuits, etc., can solve the problems that the product is difficult to form exposed Cu-N active sites, difficult to control the electronic structure of active centers, and large copper ion diffusion coefficient. , to achieve the effect of promoting electron transfer, promoting exposure, and promoting mass transfer

Active Publication Date: 2021-12-17
WUYI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the diffusion coefficient of copper ions is large, and the copper agglomeration is serious at high temperature, which makes it difficult for the product to form exposed Cu-N active sites, and it is even more difficult to control the electronic structure of the active center, resulting in low Cu-N-C.

Method used

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  • Cu-N-C oxygen reduction catalyst and preparation method thereof
  • Cu-N-C oxygen reduction catalyst and preparation method thereof
  • Cu-N-C oxygen reduction catalyst and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0044] This embodiment provides a method for preparing a Cu-N-C oxygen reduction catalyst, comprising the following steps:

[0045] S1), dissolving 1.0g of 1,10-phenanthroline in 100mL of absolute ethanol, stirring to form a transparent and uniform solution, then adding 0.50g of copper chloride dihydrate, and continuing to stir to form a complex precursor;

[0046] S2), slowly add 5g of nano-MgO with a size of 20nm to the solution obtained in step (1), ultrasonic for 15min, after the ultrasonic is completed, stir the solution at 60°C until the absolute ethanol is completely volatilized, then put it into a vacuum drying oven at 60°C Under drying for 12h, then the product was ground into powder;

[0047] S3), the powder porcelain boat in the step S2 is sent into and placed in the tube furnace, under N 2 Or in an Ar atmosphere, the temperature was raised to 900°C at a heating rate of 2°C / min for the first high-temperature heat treatment, and after holding for 2 hours, the temper...

Embodiment 2

[0051] This embodiment provides a method for preparing a Cu-N-C oxygen reduction catalyst, comprising the following steps:

[0052] S1), dissolving 0.66g of 1,10-phenanthroline in 100mL of absolute ethanol, stirring to form a transparent and uniform solution, then adding 0.20g of copper chloride dihydrate, and continuing to stir to form a complex precursor;

[0053] S2), slowly add 2.5g of nano-MgO with a size of 20nm to the solution obtained in step S1), ultrasonic for 15min, after the ultrasonic is completed, stir the solution at 60°C until the absolute ethanol is completely volatilized, then put it into a vacuum drying oven at 60°C Under drying for 12h, then the product was ground into powder;

[0054] S3), the powder porcelain boat in the step (2) is sent into and placed in the tube furnace, under N 2 Or in an Ar atmosphere, the temperature was raised to 800°C at a heating rate of 5°C / min for the first high-temperature heat treatment, and after holding for 2 hours, the te...

Embodiment 3

[0058] Performance Testing

[0059] This embodiment takes the Cu-N-C catalyst prepared in Example 1 as the research object, and the structural characterization of the Cu-N-C catalyst is as follows Figure 1-5 As shown, the test results of its oxygen reduction performance as a catalyst are as follows Figure 6~7 Shown:

[0060] from figure 1 It can be observed that the two diffraction peaks at 2θ at 26.5 and 43.5° belong to the (002) and (101) crystal planes of graphitized carbon, respectively, which proves that the transition metal in the precursor can effectively catalyze the precursor to form graphitized carbon Material. And there is no diffraction peak related to Cu compounds (such as Cu 0 、Cu 2 O or CuO, etc.), indicating that the MgO template method used in the present invention can spatially isolate Cu ions in the complex precursor, thereby forming a highly dispersed Cu-N-C catalyst without metal agglomeration during heat treatment.

[0061] from figure 2 It can ...

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Abstract

The invention relates to a Cu-N-C oxygen reduction catalyst and a preparation method thereof. The preparation method comprises the following steps: (1) forming a complex precursor from a carbon / nitrogen organic matter and Cu ions; (2) doping a nano MgO template to enable a complex to be tightly adsorbed around magnesium oxide particles, and then carrying out solvent evaporation, drying and grinding; (3) carrying out primary heat treatment, acid pickling and drying on the MgO-containing composite precursor; and (4) carrying out secondary heat treatment. By doping MgO, Cu ions in a complex precursor can be separated in space, metal Cu agglomeration is avoided, and Cu-Nx catalytic active sites are highly dispersed; after MgO is removed through normal-temperature acid pickling, a porous structure is left in a product, the specific surface area of the catalyst is increased, active site exposure is promoted, and mass transfer in the catalytic process is promoted; and a small amount of Cu0 is separated out from the product after secondary heat treatment, electron transfer in the oxygen reduction reaction can be promoted, the coordination structure of the active center of the catalyst is regulated and controlled, and the oxygen reduction activity of the catalyst is further improved.

Description

technical field [0001] The invention relates to the technical field of catalytic materials, in particular to a Cu-N-C oxygen reduction catalyst and a preparation method thereof. Background technique [0002] In recent years, fuel cells, metal-air batteries, etc. have been placed high hopes as a new generation of clean energy devices. However, the noble metal catalyst Pt used in the cathode oxygen reduction reaction (ORR) is expensive, resource-scarce, and resistant to methanol / carbon monoxide poisoning. Problems such as poor capabilities have seriously hindered its large-scale commercialization. In recent years, people have vigorously developed transition metal-nitrogen-carbon (M-N-C) catalysts, but the current research on this type of catalyst is mainly based on Fe-N-C or Co-N-C, which is usually a mixture of direct pyrolysis nitrogen source, carbon source and metal source. Obtained, it is easy to agglomerate at high temperature, resulting in low density of active centers;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/9041H01M4/9083H01M4/8878H01M4/8882Y02E60/50
Inventor 詹云凤朱清滢吴金晓张泽鸿杨林贵张鑫唐秀凤温锦秀关雄聪
Owner WUYI UNIV
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