Preparation and application of Fe-N-CNFs catalyst based on Fe-MIL

A fe-n-cnfs and catalyst technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of poor conductivity, low specific surface area, and small porosity of Fe-N-C catalysts, and achieve high conductivity and specific surface area Large, the effect of improving the catalytic performance of oxygen reduction

Pending Publication Date: 2022-01-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems of small porosity, poor electrical conductivity and low specific surface area of ​​the Fe-N-C catalyst prepared by the existing method, the present invention uses Fe-MIL as the Fe source (Fe-MIL is a kind of metal-organic framework material), and adopts electrostatic Spinning technology prepared Fe-N-CNFs catalyst, which was applied to proton exchange membrane fuel cells, which improved the activity, mass transfer capacity and conductivity of the catalytic layer

Method used

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  • Preparation and application of Fe-N-CNFs catalyst based on Fe-MIL
  • Preparation and application of Fe-N-CNFs catalyst based on Fe-MIL
  • Preparation and application of Fe-N-CNFs catalyst based on Fe-MIL

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Embodiment 1

[0063] The method for preparing the Fe-N-CNFs (Carbon nanofibers) catalyst based on Fe-MIL comprises the following steps:

[0064] (1) 1.084g of ferric chloride hexahydrate and 0.664g of terephthalic acid were dissolved in 197ml of N,N-dimethylformamide, and ultrasonically dispersed for 5min to obtain a mixed solution;

[0065] (2) The mixed solution was reacted at a constant temperature of 150° C. for 12 hours. After the reaction was completed, it was centrifuged, washed, and dried at 80° C. for 6 hours to obtain a brown Fe-MIL precursor.

[0066] (3) 0.5g of precursor Fe-MIL was first added to 5ml of N,N-dimethylformamide, ultrasonicated for 30min, then 0.5g of polyacrylonitrile (PAN) was added and stirred at 20°C for 24h to obtain a mixed solution;

[0067] (4) Electrospinning the mixed solution for 5 hours at a voltage of 25kV and a flow rate of 0.5ml / h to obtain nanofibers;

[0068] (5) Pre-fire the nanofibers in an air atmosphere at a heating rate of 5 °C / min to 250 °C ...

Embodiment 2

[0074] The method for preparing the Fe-N-CNFs (Carbon nanofibers) catalyst based on Fe-MIL in this example refers to Example 1, the difference is that the Fe-MIL precursor added in step (3) is 0.75g, and the Fe-MIL precursor The mass ratio to polyacrylonitrile (PAN) is 1.5:1.

[0075] Figure 5 It can be seen that the catalyst contains Fe and Fe 3 C crystals, Fe and Fe coated with nitrogen-doped carbon nanofibers 3 C particles can serve as the active sites of the catalyst.

[0076] Image 6 It can be seen that the degree of graphitization of the catalyst is relatively high, I G / I D =1.06, a high degree of graphitization can improve the electron-conducting ability of the catalyst, thereby improving the catalytic activity of the catalyst.

[0077] Figure 7 It can be seen that the active components of the catalyst, graphitic nitrogen and pyridinic nitrogen, account for a total of 48.7%, graphitic nitrogen can increase the limiting current density, and pyridinic nitrogen ...

Embodiment 3

[0086]The method for preparing the Fe-N-CNFs (Carbon nanofibers) catalyst based on Fe-MIL in this embodiment refers to Example 1, the difference is that the Fe-MIL precursor added in step (3) is 1.0 g, and the Fe-MIL precursor The mass ratio to polyacrylonitrile (PAN) is 2:1.

[0087] Figure 16 It can be seen that the catalyst contains Fe and Fe 3 C crystals, Fe and Fe coated with nitrogen-doped carbon nanofibers 3 The C particle can be used as the active site of the catalyst, which is the same as in Example 2.

[0088] Figure 17 It can be seen that the degree of graphitization of the catalyst is relatively high, I G / I D =0.98, a high degree of graphitization can improve the electron-conducting ability of the catalyst, and then improve the catalytic activity of the catalyst, which is slightly higher than that of Example 2.

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Abstract

The invention provides preparation and application of a Fe-N-CNFs (Carbon Nanofibers) catalyst based on Fe-MIL, and the method is as follows: firstly, ferric chloride hexahydrate and terephthalic acid react in N, N-dimethylformamide to generate a Fe-MIL precursor, then the Fe-MIL precursor and a nitrogen-containing binder are mixed in N, N-dimethylformamide for electrostatic spinning to prepare nanofibers, and then the nanofibers are prepared into the Fe-N-CNFs catalyst based on Fe-MIL, and the Fe-N-CNFs (Carbon Nanofibers) catalyst is prepared after the Fe-N-CNFs catalyst is subjected to pre-sintering and pyrolysis. The catalyst is large in active area, high in electron transfer capability and high in mass transmission capability, so that the capability of catalyzing the oxygen reduction reaction is relatively high. In addition, the synthetic material is low in price, and the cost of the catalyst can be reduced, so that the catalyst has a relatively great application prospect in the aspect of proton exchange membrane fuel cells.

Description

technical field [0001] The invention belongs to the field of fuel cells, in particular to a preparation method of Fe-N-CNFs (Carbonnanofibers) catalyst based on Fe-MIL and its application in fuel cell oxygen reduction reaction. Background technique [0002] With the deteriorating energy and environmental problems and the increasing demand for clean energy, proton exchange membrane fuels have attracted widespread attention due to their high energy conversion efficiency, high power density and zero pollution emissions. However, the use of high-priced Pt / C catalysts in its cathode hinders the large-scale application of proton exchange membrane fuel cells. Therefore, it is urgent to develop non-precious metal catalysts with low price and high activity. Fe-N-C catalysts have made great progress as the most likely non-precious metal catalysts to replace Pt / C catalysts. Among them, iron nitrogen carbon nanofibers The catalyst has relatively excellent performance (J.L.Shui, C.Chen,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/86H01M4/90
CPCH01M4/9083H01M4/9041H01M4/8636H01M4/861H01M2004/8689Y02E60/50
Inventor 侯明罗文哲邵志刚
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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