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Preparation method of difunctional molybdenum-doped cobalt sulfide/nitrogen-carbon array electrode

A technology of array electrodes and cobalt sulfide, which is applied to battery electrodes, fuel cell half-cells, primary battery-type half-cells, circuits, etc., can solve the problems of limited commercial application of earth reserves, high cost, etc.

Active Publication Date: 2020-08-04
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, their commercial applications are severely limited due to their high cost and scarcity of earth reserves

Method used

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  • Preparation method of difunctional molybdenum-doped cobalt sulfide/nitrogen-carbon array electrode
  • Preparation method of difunctional molybdenum-doped cobalt sulfide/nitrogen-carbon array electrode
  • Preparation method of difunctional molybdenum-doped cobalt sulfide/nitrogen-carbon array electrode

Examples

Experimental program
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Effect test

Embodiment 1

[0025] CoCl 2 ∙6H 2 O and urea were dissolved in 40 mL of deionized water at room temperature, in which CoCl 2 The concentration of urea was 0.15 M, and the mass fraction of urea was 6.25 wt.%. After immersing the hydrophilic carbon paper in the solution, it was incubated at 90°C for 2 h. After natural cooling to room temperature, the carbon paper was taken out and rinsed with deionized water. Three times, dry and set aside. Soak the above-mentioned carbon paper grown with basic cobalt salt arrays in 50 mL of Tris base with a concentration of 0.01 M and a pH of 8.5, add 0.01 g of dopamine, stir at room temperature for 24 h, and rinse the sample three times with deionized water dry. Dissolve molybdenum chloride in ethanol solution, stir to dissolve, and obtain 400 mM molybdenum chloride ethanol solution. The above-mentioned carbon paper on which the basic cobalt salt array@PDA array was grown was soaked in the molybdenum chloride solution for about 1 min at room temperature...

Embodiment 2

[0028] CoCl 2 ∙6H 2 O and urea were dissolved in 40 mL of deionized water at room temperature, in which CoCl 2 The concentration of urea was 0.15 M, and the mass fraction of urea was 6.25 wt.%. After immersing the hydrophilic carbon paper in the solution, it was incubated at 90°C for 2 h. After natural cooling to room temperature, the carbon paper was taken out and rinsed with deionized water. Three times, dry and set aside. Soak the carbon paper on which the basic cobalt salt array was grown above in 50 mL of Tris base with a concentration of 0.01 M and a pH of 8.5, add 0.02 g of dopamine, stir at room temperature for 24 h, and rinse the sample three times with deionized water dry. Dissolve molybdenum chloride in ethanol solution, stir to dissolve, and obtain 400 mM molybdenum chloride ethanol solution. The above-mentioned carbon paper on which the basic cobalt salt array@PDA array was grown was soaked in the molybdenum chloride solution for about 1 min at room temperatur...

Embodiment 3

[0032] CoCl 2 ∙6H 2 O and urea were dissolved in 40 mL of deionized water at room temperature, in which CoCl 2 The concentration of urea was 0.15 M, and the mass fraction of urea was 6.25 wt.%. After immersing the hydrophilic carbon paper in the solution, it was incubated at 90°C for 2 h. After natural cooling to room temperature, the carbon paper was taken out and rinsed with deionized water. Three times, dry and set aside. The carbon paper with the basic cobalt salt array grown was placed in the air at 400°C for 0.5 h to obtain the carbon paper substrate with the cobalt oxide array grown, which was taken out after natural cooling for use. Soak the above-mentioned carbon paper with cobalt oxide arrays grown in 50 mL of Tris base with a concentration of 0.01 M and a pH of 8.5, add 0.02 g of dopamine, stir at room temperature for 24 h, rinse the sample three times with deionized water and then dry it. Dissolve molybdenum chloride in ethanol solution, stir to dissolve, and ob...

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Abstract

The invention provides a preparation method of a difunctional molybdenum-doped cobalt sulfide / nitrogen carbon array electrode. A cobalt-based precursor array structure is obtained through chemical bath deposition assisted drying or pre-oxidation or pre-vulcanization, then a layer of polydopamine grows on the surface of the cobalt-based precursor, molybdenum ions are adsorbed, and finally an annealing reaction is conducted in the sulfur atmosphere. In the annealing process, polydopamine is gradually converted into a nitrogen-doped carbon material, and the cobalt-based precursor reacts with sulfur vapor to form cobalt sulfide. Meanwhile, molybdenum ions are dispersed due to coordination and adsorption of nitrogen in polydopamine and are located on the surface of polydopamine to be isolated from the cobalt element, molybdenum disulfide and cobalt sulfide / molybdenum disulfide contact type structures with high crystalline state degree are formed in the vulcanization process, and then the molybdenum-doped cobalt sulfide / nitrogen carbon structure is formed. According to the technical scheme, a Co-N-C bond type structure formed by a cobalt sulfide / nitrogen-carbon interface has good ORR andOER performance; in addition, Co-O-Mo formed by molybdenum-doped cobalt sulfide and Mo-N formed by molybdenum-doped nitrogen carbon are also respectively an OER high-activity center and an ORR high-activity center.

Description

technical field [0001] The invention relates to a doped and composite in-situ electrode and its preparation, and belongs to the field of energy storage and conversion materials and devices. Background technique [0002] As a new class of energy storage devices, reversible metal-air batteries and fuel cells have attracted extensive attention in the field of new energy. Among them, the electrocatalytic oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) are two core reactions in reversible metal-air batteries. Therefore, the development of OER / ORR bifunctional electrocatalysts with high catalytic activity, high stability and low cost will greatly promote the application of metal-air batteries. So far, these cheap and efficient OER and ORR catalysts are based on noble metal materials, such as: Pt has good ORR performance, Ru, Ir and their oxides have good OER performance. However, their commercial applications are severely limited due to their high cost and sc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/86H01M4/88H01M4/90H01M12/06
CPCH01M4/8652H01M4/8885H01M4/9008H01M12/06
Inventor 黄妞骆禅闫术芳杨柳
Owner CHINA THREE GORGES UNIV
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