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Preparation method and application of a zinc-based metal-organic framework material and its iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst

A technology of organic framework and electrocatalyst, applied in the direction of circuits, electrical components, battery electrodes, etc., can solve the problems of less attention in use

Active Publication Date: 2022-06-28
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of interpenetrating nonporous MOF complexes as pyrolytic precursors has so far received less attention compared to local studies on the use of porous MOFs in the preparation of carbon catalysts.

Method used

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  • Preparation method and application of a zinc-based metal-organic framework material and its iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst
  • Preparation method and application of a zinc-based metal-organic framework material and its iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst
  • Preparation method and application of a zinc-based metal-organic framework material and its iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of zinc-based metal-organic frameworks (Zn-TTPA):

[0041] The ligand TTPA-4 (13.4 mg, 0.03 mmol), terephthalic acid (10.0 mg, 0.06 mmol), zinc nitrate hexahydrate (17.8 mg, 0.06 mmol) were dissolved in 10 mL of DMF and deionized water (V:V =1:1) mixed solvent, placed in a hydrothermal still of tetrafluoroethylene and stirred evenly, heated to 100°C for reaction for 50 hours, slowly lowered to 15°C, collected the resulting crystals, and the crystals were prepared with a solvent (N,N-di Methylformamide, water, ethanol) were washed successively, and dried at room temperature to obtain a zinc-based metal organic framework material. The yield is about 65%.

[0042] figure 1 It is a structural diagram of the zinc-based metal organic framework material Zn-TTPA obtained in Example 1 of the present invention observed along the c-axis direction. In Zn-TTPA, observed along the c-axis direction, a quasi-hexagonal structure is formed in the Zn-TTPA framework. shaped ...

Embodiment 2

[0046] Step 1. Preparation of precursor Fe-Zn-TTPA:

[0047] The ligand TTPA-4 (13.4 mg, 0.03 mmol), terephthalic acid (10.0 mg, 0.06 mmol), zinc nitrate hexahydrate (17.8 mg, 0.06 mmol), ferric nitrate nonahydrate (1.01 mg, 0.0025 mmol) were added 10mL of DMF and deionized water (V:V=1:1) mixed solvent, heated to 100°C with stirring, stirred for 72 hours, slowly lowered to 15°C, filtered to obtain a powdery solid with a yield of about 67% .

[0048] Step 2. Preparation of iron-nitrogen co-doped carbon material

[0049] The powdered solid precursor Fe-Zn-TTPA material was put into a tube furnace, heated to 950°C at 5°C / min in a nitrogen atmosphere, maintained at this temperature for 2h, cooled to room temperature at 5°C per minute, An iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst was obtained.

[0050] image 3 are the XRD patterns of the zinc-based metal-organic framework material Zn-TTPA and the carbonized precursor Fe-Zn-TTPA obtained in Examples ...

Embodiment 3

[0059] Step 1. Preparation of precursor Fe-Zn-TTPA:

[0060] The ligand TTPA-4 (17.9 mg, 0.04 mmol), terephthalic acid (11.7 mg, 0.07 mmol), zinc nitrate hexahydrate (20.8 mg, 0.07 mmol), ferric nitrate nonahydrate (1.21 mg, 0.003 mmol) were added 20mL of DMF and deionized water (V:V=1:1) mixed solvent, heated to 95°C with stirring, stirred for 45 hours, slowly lowered to 30°C, filtered to obtain a powdery solid with a yield of about 64% .

[0061] Step 2. Preparation of iron-nitrogen co-doped carbon material

[0062] The powdered solid precursor Fe-Zn-TTPA material was put into a tube furnace, heated to 1100°C at 10°C / min in an argon atmosphere, kept at this temperature for 2h, and cooled to room temperature at 10°C per minute , to obtain iron-nitrogen co-doped carbon-based oxygen reduction electrocatalysts.

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Abstract

The invention discloses a preparation method and application of a zinc-based metal-organic framework material and its iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst. The catalyst of the invention is based on a newly designed zinc-based metal-organic framework material. The precursor Fe-Zn-TTPA was prepared by one-pot method based on metal-organic framework materials, and the precursor Fe-Zn-TTPA was carbonized at high temperature to obtain an iron-nitrogen-carbon-oxygen reduction electrocatalyst. The material of the invention is simple and easy to obtain, and the cost is low. The prepared iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst has high oxygen reduction catalytic activity, good stability and methanol tolerance, and can replace the noble metal Pt / C catalyst as The application of catalytic materials in fuel cells or metal-air batteries has broad application prospects and practical value.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a zinc-based metal organic framework material and an iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst based on the zinc-based metal organic framework material, and a preparation method and application thereof. Background technique [0002] Fuel cells and metal-air batteries are considered promising clean energy conversion devices. However, the slow kinetic nature of the oxygen reduction reaction (ORR) at the cathode limits the energy conversion efficiency of these devices. Currently, precious platinum (e.g., Pt / C) and its alloys still represent state-of-the-art catalysts, but high cost, scarce reserves, and poor stability severely hinder their large-scale applications. Consequently, there has been a growing interest in developing cost-effective, earth-abundant and efficient non-noble metal-based catalysts in this field in recent years. In this case, transi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88H01M4/86H01M4/90
CPCH01M4/9008H01M4/8882H01M4/8652Y02E60/50
Inventor 诸海滨黄佳维
Owner SOUTHEAST UNIV
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