A kind of nitrogen-doped graphdiyne riveted transition metal single-atom catalyst and its preparation method and application

A transition metal and transition metal salt technology, applied in structural parts, electrical components, battery electrodes, etc., can solve the problems of reduced catalyst activity, limited non-precious metal catalyst activity, low atom utilization, etc., and achieve high catalytic activity.

Active Publication Date: 2021-05-11
NANJING NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The study found that the nitrogen in the catalyst can coordinate with the transition metal atoms to form a TM-N structure, and these TM-N structures are the catalytic active sites of the TM-N-C catalyst. When the size of the metal particle is reduced to the atomic size, its specific surface area and surface The energy will be multiplied, and it is very easy to agglomerate to form large clusters in the process of preparation and reaction, resulting in low atom utilization, which leads to a decrease in catalyst activity and limits the activity of non-noble metal catalysts.

Method used

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  • A kind of nitrogen-doped graphdiyne riveted transition metal single-atom catalyst and its preparation method and application
  • A kind of nitrogen-doped graphdiyne riveted transition metal single-atom catalyst and its preparation method and application
  • A kind of nitrogen-doped graphdiyne riveted transition metal single-atom catalyst and its preparation method and application

Examples

Experimental program
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Embodiment 1

[0040]Dissolve 50 mg of hexa[trimethylsilyl]ethynyl]benzene in 15 mL of tetrahydrofuran, stir for 1 h under Ar gas purging, add 1 mL of tetrabutylammonium fluoride at 0°C for 15 min; add 20 mL of ethyl acetate to dilute, Then add 20 mL of saturated saline to wash three times, extract and separate the liquid to take the upper layer solution, add 20 mg of anhydrous magnesium sulfate to remove water and filter, and the mixture is rotary evaporated at 45 ° C to remove the solvent to obtain a yellow solid hexaethynylbenzene; 100 mL of acetone and 5 mL Pyridine, 1mL tetramethylethylenediamine, and 2*2cm*10 acid-washed copper foil were stirred at 50°C for 2h under the protection of Ar gas to obtain a mixture, and the hexaethynylbenzene obtained in the previous step was dissolved in 50mL of acetone, and the Slowly add the above mixture to react for 36h; centrifuge the reacted mixture at 10000r / min to get the black solid, and wash it with N,N,N,N-tetramethylethylenediamine, acetone, eth...

Embodiment 2

[0042] Mix 10 mg of graphyne synthesized in Example 1 with 50 mg of melamine in 30 mL of ethanol (AR), and stir thoroughly at room temperature 20° C. for 12 h; place the mixture in a vacuum oven at 70° C. and dry for 6 h to obtain mixture A; The dried mixture A was placed in a tube furnace, heated to 900°C for 2 hours under an Ar gas atmosphere, and pyrolyzed at a rate of 5°C / min, and cooled to room temperature to obtain a black solid B; all the black solid B was mixed with 0.1 Disperse mol of ferric chloride hexahydrate into 30mL water, stir magnetically under Ar atmosphere at 25°C for 12h to obtain mixture C, use a 200W power ultrasonic machine to sonicate for 10min, and centrifuge at 10000r / min for 10min to obtain solid precipitate D; all solid precipitate D Disperse in 30mL of water, dissolve 5mg of sodium borohydride in 10mL of water, add to the above dispersion under Ar atmosphere, stir with a magnetic stirrer at 20°C for 12h; wash the stirred mixed solution twice with wa...

Embodiment 3

[0045] The preparation method of embodiment 3 is the same as that of embodiment 2, except that ferric chloride hexahydrate is replaced by ferric nitrate nonahydrate.

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Abstract

The invention discloses a nitrogen-doped graphyne riveted transition metal single-atom catalyst and its preparation method and application. The catalyst is doped with nitrogen atoms in a new type of carbon material graphyne carrier, and the transition metal single atom is combined with N , The covalent interaction between C atoms is riveted on the surface of nitrogen-doped graphyne, so that the transition metal is uniformly dispersed on the surface of nitrogen-doped graphyne in the form of single atoms. In the catalyst of the present invention, the transition metal atoms are evenly dispersed on the surface of the nitrogen-graphyne-based catalyst in the state of a single atom, providing a large number of active sites for redox reactions, and using graphyne as the carbon substrate has excellent morphology characteristics. It is beneficial to the formation of catalytic active sites and to exert the catalytic advantages of single atoms. The catalyst of the invention has high electrocatalytic activity for oxygen reduction under alkaline conditions, simple and effective preparation process, low cost, easy promotion and production, and has great significance in the field of fuel cell development and application.

Description

technical field [0001] The invention belongs to the technical field of material chemistry and electrocatalyst, and in particular relates to a preparation method of a fuel cell cathode catalyst, in particular to a nitrogen-doped graphyne riveted transition metal single-atom catalyst and its preparation method and application. Background technique [0002] Because of its superior performance and environmental friendliness, cleanliness and non-pollution, fuel cells have shown outstanding advantages in various types of batteries. It can directly convert chemical energy into electrical energy and has a very high fuel utilization rate. It has always been a hot spot in the field of energy research. hotspot. Oxygen reduction reaction (ORR) is the first reduction reaction of fuel cells and one of the important basic reactions in living organisms. However, due to its slow reaction kinetics and complicated reaction steps, it is necessary to select a suitable catalyst to improve its rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/8825H01M4/9041H01M4/9083H01M2004/8689Y02E60/50
Inventor 蔡称心周家兴胡耀娟蔡哲炜潘永慧吴萍
Owner NANJING NORMAL UNIVERSITY
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