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Preparation method of nitrogen-doped graphene oxide-supported carbon nanotubes and fe/zif8 composites

A technology of carbon nanotubes and composite materials, which is applied in the field of material chemistry, can solve the problems of high-temperature transition metals being easy to agglomerate, and achieve the effects of reducing agglomeration, high use value, and harmless to the environment

Active Publication Date: 2022-07-29
UNIV OF SHANGHAI FOR SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is: in existing carbon-based transition metal catalysts, the problem that high-temperature transition metals are easy to agglomerate

Method used

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  • Preparation method of nitrogen-doped graphene oxide-supported carbon nanotubes and fe/zif8 composites
  • Preparation method of nitrogen-doped graphene oxide-supported carbon nanotubes and fe/zif8 composites
  • Preparation method of nitrogen-doped graphene oxide-supported carbon nanotubes and fe/zif8 composites

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation method of sample ZIF8-900:

[0038] 1) Dissolve 4g of dimethylimidazole in 25mL of methanol, stir for 10min to obtain a dimethylimidazole solution, then take 1g of Zn(NO) 3 ) 6H 2 O was dissolved in 10 mL of methanol and stirred for 10 min to obtain Zn(NO 3 ) 6H 2 O solution, slowly add dimethylimidazole solution dropwise to Zn(NO 3 ) 6H 2 O solution (dropwise added for 5min) to obtain a uniform milky white mixed solution, the milky white mixed solution was continuously stirred at room temperature for 12h, centrifuged at 12000rpm for 20min, washed with methanol and dried at 60°C to obtain ZIF8.

[0039] 2) Step 2) Put the ZIF8 powder in the crucible, cover the crucible, calcine under Ar conditions, heat the tube furnace to 550°C at 3°C / min and keep it for 2h; then heat up to 3°C / min. The temperature was kept at 900 °C for 2 h, and finally the furnace was naturally cooled to room temperature under the protection of Ar to obtain the sample ZIF8-900.

Embodiment 2

[0041] Preparation method of sample Fe / ZIF8-900:

[0042] 1) Step 1) Dissolve 4 g of dimethyl imidazole in 25 mL of methanol, stir for 10 min to obtain a dimethyl imidazole solution, and then take 1 g of Zn(NO) 3 ) 6H 2 O was dissolved in 10 mL methanol and stirred for 10 min to obtain Zn(NO 3 ) 6H 2 O solution, slowly add dimethylimidazole solution dropwise to Zn(NO 3 ) 6H 2 O solution (dropwise added for 5 min) to obtain a uniform milky white mixed solution, the milky white mixed solution was continuously stirred at room temperature for 12 h, centrifuged at 12000 rpm for 20 min, washed with methanol and dried at 60 °C to obtain ZIF8. Then take 120mg ZIF8 sample, add it into 5mL methanol, stir for 15min to obtain solution A, then mix 5mL methanol with 60mg anhydrous FeCl 3 Mix and stir for 15 min to obtain solution B, mix and stir solution A and solution B for 12 h, centrifuge at 12000 rpm for 20 min, wash with methanol and dry at 60 °C for 5 h to obtain Fe / ZIF8 powder. ...

Embodiment 3

[0045] Preparation method of nitrogen-doped graphene oxide negative carbon nanotube Fe / ZIF8 (N-GO@Fe / ZIF8-900) composite material:

[0046]1) Add 3g urea to 50mL (1mg / mL) graphene oxide, ultrasonicate for 2h to obtain a uniform brown solution, put the brown solution in a refrigerator at -80°C for 12h to obtain a brown solid, and place the brown solid in freeze-drying Dry in the machine for 48h to obtain brown powder.

[0047] 2) Dissolve 4g of dimethylimidazole in 25mL of methanol, stir for 10min to obtain a dimethylimidazole solution, then take 1g of Zn(NO) 3 ) 6H 2 O was dissolved in 10 mL methanol and stirred for 10 min to obtain Zn(NO 3 ) 6H 2 O solution, slowly add dimethylimidazole solution dropwise to Zn(NO 3 ) 6H 2 O solution (dropwise added for 5 min) to obtain a uniform milky white mixed solution, the milky white mixed solution was continuously stirred at room temperature for 12 h, centrifuged at 12000 rpm for 20 min, washed with methanol, and then dried at 60 °...

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Abstract

The invention discloses a method for preparing nitrogen-doped graphene oxide-supported carbon nanotubes and Fe / ZIF8 composite materials, which is characterized in that: adding urea into a graphene oxide solution, freeze-drying to obtain brown powder; dissolving in methanol dimethylimidazole solution and Zn(NO) dissolved in methanol 3 ) 6H 2 O solution was mixed to obtain ZIF8; ZIF8, anhydrous FeCl 3 They were respectively added to methanol, and then mixed to obtain Fe / ZIF8; the brown powder was ground and mixed with Fe / ZIF8, and calcined to obtain a composite material of nitrogen-doped graphene oxide supported carbon nanotubes and Fe / ZIF8. The present invention forms a three-dimensional porous structure by combining "dot-line-surface", which is beneficial to the transmission of reaction substances and the exposure of more active sites, thereby improving the oxygen reduction performance, the preparation process is simple, the cost is low, and the material It has the advantages of good structural uniformity and excellent electrochemical performance.

Description

technical field [0001] The invention relates to a preparation method of nitrogen-doped graphene oxide-loaded carbon nanotubes and Fe / ZIF8 composite materials, and belongs to the technical field of material chemistry. Background technique [0002] In recent years, rechargeable zinc-air batteries (ZABs) have been regarded as a promising energy storage device due to their high safety, high energy density, abundant resources, and environmental friendliness [Fu J, Cano Z P, et al. Zinc–Air Batteries:Progress,Challenges,and Perspectives[J].Advanced Materials,2017,29(7):160468 5.1-1604685.34.], however, in the reaction process, slow kinetics and large overpotential reduce zinc The efficiency of ORR and OER on air electrodes in air batteries limits their large-scale applications. The noble metals in the commonly used noble metal cathode electrocatalysts are mainly Pt, Pb, Ru[Xiao Y, ZhangW.Mechanism of Electrocatalytically Active Precious Metal(Ni,Pd,Pt and Ru)Complexes in the Grap...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/90H01M4/88H01M12/08
CPCH01M4/9083H01M4/8878H01M12/08H01M2004/8684
Inventor 李田成张婷李生娟杨俊和吉莹夏营港
Owner UNIV OF SHANGHAI FOR SCI & TECH
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