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MOFs (Metal Organic Frameworks)-based NiCo@N-C dual-function oxygen electrode catalyst and preparation method thereof

A technology of oxygen electrode and catalyst, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve the effects of large specific surface area, increased N doping amount and conductivity, and increased stability

Inactive Publication Date: 2018-11-02
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the mononuclear characteristics of most MOFs, there are few reports on the application of heterogeneous binuclear MOFs-derived alloy catalysts in ORR or OER research fields, and there is no application of heterogeneous binuclear MOFs as templates to generate N-C-based NiCo alloy nanocatalysts for oxygen electrodes. Reports on functional electrocatalysis

Method used

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  • MOFs (Metal Organic Frameworks)-based NiCo@N-C dual-function oxygen electrode catalyst and preparation method thereof
  • MOFs (Metal Organic Frameworks)-based NiCo@N-C dual-function oxygen electrode catalyst and preparation method thereof
  • MOFs (Metal Organic Frameworks)-based NiCo@N-C dual-function oxygen electrode catalyst and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0038] Preparation of NiCo(1:1)@N-C bifunctional oxygen electrode catalyst:

[0039] Weigh 436.1mg Ni(NO 3 ) 2 .6H 2 O and 436.6mg Co(NO 3 ) 2 .6H 2 O was dissolved in methanol with a volume of 30mL and mixed evenly by ultrasonic to make metal precursor solution A; in addition, 985.2mg MeIM was weighed and dissolved in 10mL methanol and mixed evenly to make organic ligand solution B; the metal ion Ni 2+ with Co 2+ The total molar concentration in the organic reagent is 0.075mol / L; under the condition of magnetic stirring, the organic ligand solution B is gradually added to the metal precursor solution A to form a mixed solution, and the stirring is continued for 1h; In a hydrothermal kettle with a tetrafluoroethylene liner (50mL, filling degree 80%), conduct a solvothermal reaction at 100°C for 12 hours; vacuum filter the mixture obtained from the solvothermal reaction, wash it with methanol several times, and dry it in vacuum at 80°C Take it out after 12h to obtain a p...

Embodiment 2

[0044] With reference to the preparation method and test method of embodiment 1 catalyst, difference is that n(Ni 2+ ):n(Co 2+ ) adjusted to 1:2, namely weigh 581.6mg Ni (NO 3 ) 2 .6H 2 O and 1164.1mg Co(NO 3 ) 2 .6H 2 O was dissolved in methanol with a volume of 40mL, and ultrasonically mixed uniformly to make metal precursor solution A; in addition, 1.97g MeIM was weighed and dissolved in 40mL methanol and mixed uniformly to make organic ligand solution B; the metal ion Ni 2+ with Co 2+ The total molar concentration in the organic reagent is 0.075mol / L; NiCo(1:2)@N-C bifunctional oxygen electrode catalyst is prepared.

[0045] The NiCo(1:2)@N-C bifunctional oxygen electrode catalyst prepared in FE-SEM test embodiment 2, such as Figure 5 As shown, the obtained material is a rhombic dodecahedron with a slightly collapsed surface, and there are a small amount of carbon nanotube structures on each surface except spherical protrusions. The surface area of ​​the catalyst...

Embodiment 3

[0047] With reference to the preparation method and test method of embodiment 1 catalyst, difference is during liquid preparation, n(Ni 2+ ):n(Co 2+ ) adjusted to 1:4, that is, weigh 174.47mg Ni (NO 3 ) 2 .6H 2 O and 698.47mg Co(NO 3 ) 2 .6H 2 O was dissolved in methanol with a volume of 20mL, and ultrasonically mixed evenly to make metal precursor solution A; in addition, 985.2mg MeIM was weighed and dissolved in 10mL methanol and mixed evenly to make organic ligand solution B; the metal ion Ni 2+ with Co 2+ The total molar concentration in the organic reagent is 0.10mol / L; NiCo(1:4)@N-C bifunctional oxygen electrode catalyst is prepared. The surface area of ​​the catalyst obtained in the embodiment 3 tested by BET method is 265.7 m 2 / g, the total pore volume is 0.20cm 3 / g. The atomic ratio of C:N:O:Co:Ni on the surface of the catalyst obtained in Example 3 by XPS test is 83.90:3.87:10.1:1.61:0.52, combined with XRD analysis, it can be known that the catalyst is a...

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Abstract

The invention discloses an MOFs (Metal Organic Frameworks)-based NiCo@N-C dual-function oxygen electrode catalyst and a preparation method thereof. The NiCo@N-C dual-function oxygen electrode catalystis a rhombic polyhedral having a carbon nano tube structure on the surface. The NiCo@N-C dual-function oxygen electrode catalyst has the BET superficial area of 169.9-268.7m<2> / g and the total pore volume of 0.26-0.20cm<3> / g, and is of an N-doped C cage coated NiCo alloy structure. The preparation method disclosed by the invention comprises the following steps: performing coordination on a cobaltsalt and a nickel salt with dimethylimidazole in an organic reagent so as to obtain NiCo bimetallic MOFs of different atomic ratios, performing high-temperature pyrolysis under inert gas shielding bytaking the bimetallic MOFs as a template, performing one-step carbonization on N-containing organic ligands to produce an N-doped coating structure coated with the NiCo alloy. Therefore, electronic structure control of metal catalytic activity is realized, highly regular porous structure and high specific surface area are remained, and the high N doping amount and conductivity of the obtained N-Cmaterial are improved.

Description

technical field [0001] The invention relates to the technical field of oxygen electrode catalysts and preparation methods thereof, in particular to a MOFs-based NiCo@N-C bifunctional oxygen electrode catalyst and a preparation method thereof. Background technique [0002] With the increasing demand for clean and sustainable energy, efforts have been made to develop efficient, low-cost, and environmentally friendly alternative energy conversion and storage systems, such as integrated renewable fuel cells, metal-air batteries, and water splitting systems. Bifunctional oxygen electrode reaction catalysts with both oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) catalytic activities are undoubtedly the key to various renewable energy technologies. [0003] Although PtIrRu alloys can be used as bifunctional catalysts for oxygen electrodes, the scarcity and high cost of raw materials hinder their large-scale application, and the development of high-efficiency, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10B01J37/08
CPCB01J27/24B01J37/08B01J37/086B01J35/33B01J35/615B01J35/633
Inventor 胡玮宁红辉聂仁峰龚壮
Owner HUBEI UNIV
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