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Preparation method of in-situ defect modified Co9S8-porous nitrogen-doped carbon electrode

A nitrogen-doped carbon, co9s8- technology, applied in fuel cell type half cells and primary cell type half cells, battery electrodes, circuits, etc., can solve problems such as limited electrocatalytic performance and aggravating the surface of catalyst substrates.

Active Publication Date: 2020-01-14
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the use of insulating polymer binders (e.g., electrolytes) in powdered catalyst substrates, a considerable number of pores (or pores) and active sites will inevitably be blocked, thus limiting electrocatalytic performance while exacerbating the surface of the catalyst substrate.

Method used

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  • Preparation method of in-situ defect modified Co9S8-porous nitrogen-doped carbon electrode

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Experimental program
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Effect test

Embodiment 1

[0022] At room temperature, dissolve cobalt chloride hexahydrate, Tx-100, aniline and thiourea in 2.7 mL N,N-dimethylformamide solution, the concentration of cobalt chloride hexahydrate is 400 mM, Tx-100 The volume is 0.3 mL, the volume of aniline is 0.03 mL, and the concentration of thiourea is 1000 mM. Soak the carbon paper in the precursor solution for 30 minutes, take it out, dry it on a hot table at 80°C for 10 minutes, then apply the precursor solution evenly on the carbon paper, and then continue to dry for 30 minutes. Put the coated substrate into a tube furnace, react at 600°C for 1h under Ar flow, then continue to heat up to 900°C for 30min, and take it out after natural cooling to obtain cobalt sulfide-porous carbon. Subsequently, the above cobalt sulfide-porous carbon was reacted in 1 g of dicyandiamide at 600 °C for 1 h, and taken out after natural cooling to obtain the in-situ defect-modified Co 9 S 8 - Porous nitrogen-doped carbon electrodes.

[0023] figure...

Embodiment 2

[0030] At room temperature, dissolve cobalt chloride hexahydrate, Tx-100, aniline and thiourea in 2.5 mL N,N-dimethylformamide solution, the concentration of cobalt chloride hexahydrate is 400 mM, Tx-100 The volume is 0.5 mL, the volume of aniline is 0.05 mL, and the concentration of thiourea is 1000 mM. Soak the carbon paper in the precursor solution for 30 minutes, take it out, dry it on a hot table at 80°C for 10 minutes, then apply the precursor solution evenly on the carbon paper, and then continue to dry for 30 minutes. Put the coated substrate into a tube furnace, react at 600 °C for 1 h under Ar flow, then continue to heat up to 900 °C for 30 min, and take it out after natural cooling to obtain cobalt sulfide-porous carbon. Subsequently, the above cobalt sulfide-porous carbon was reacted in 1 g of dicyandiamide at 500 °C for 1 h, and taken out after natural cooling to obtain the in-situ defect-modified Co 9 S 8 - Porous nitrogen-doped carbon electrodes.

[0031] F...

Embodiment 3

[0033] At room temperature, dissolve cobalt chloride hexahydrate, Tx-100, aniline and thiourea in 2.0 mL N,N-dimethylformamide solution, the concentration of cobalt chloride hexahydrate is 400 mM, Tx-100 The volume is 1 mL, the amount of aniline is 0.03 mL, and the concentration of thiourea is 1000 mM. Soak the carbon paper in the precursor solution for 30 minutes, take it out, dry it on a hot table at 80°C for 10 minutes, then apply the precursor solution evenly on the carbon paper, and then continue to dry for 30 minutes. The coated substrate was put into a tube furnace, reacted at 600 °C for 1 h under Ar flow, then continued to heat up to 900 °C for 30 min, and took it out after natural cooling to obtain cobalt sulfide-porous carbon. Subsequently, the above cobalt sulfide-porous carbon was reacted in 1 g of dicyandiamide at 700 °C for 1 h, and taken out after natural cooling to obtain the in-situ defect-modified Co 9 S 8 - Porous nitrogen-doped carbon electrodes.

[0034...

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Abstract

The invention provides a preparation method of an in-situ defect modified Co9S8-porous nitrogen-doped carbon electrode. The method comprises the steps of: dissolving cobalt salt, Tx-100, aniline and other carbon-containing organic matters in a volatile non-aqueous solvent, and adding thiourea as a sulfur source to obtain a Co-C-S precursor solution; and coating a carbon substrate with the precursor solution, performing drying and then annealing in Ar or N2 airflow to obtain an in-situ cobalt sulfide-carbon electrode, and continuously carrying out CVD calcination annealing on the in-situ cobaltsulfide electrode under dicyandiamide airflow to finally form the in-situ defect modified Co9S8-porous nitrogen-doped carbon electrode. The product obtained by the technical scheme provided by the invention has the advantages of the low equipment requirement, the low cost of required raw materials, the easily controlled reaction conditions, the simple production process, the good consistency of the formed product, the small environmental pollution and the like, and can be used for multifunctional electrocatalysts of OER and ORR.

Description

technical field [0001] The invention relates to an in-situ electrode and its preparation, and belongs to the field of energy storage and conversion materials and devices. Background technique [0002] In order to meet the challenges of traditional energy emissions and environmental pollution, the development of efficient electrocatalysts plays a vital role in the application of green and sustainable energy storage and conversion devices. General energy storage and conversion devices involve two reactions, namely OER and ORR, so it is imminent to develop corresponding catalysts. Transition metal-nitrogen-carbon (M-N-C) or related catalysts have proven to be the most promising bifunctional OER and ORR catalysts. Such catalysts can be classified into single-atom electrocatalysts, transition metal-based particles (including metals, alloys, oxides, nitrides, sulfides, etc.) and composite electrocatalysts composed of carbon materials. For example, Meng et al. prepared Co from ZI...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/96H01M4/88H01M12/06
CPCH01M4/96H01M4/88H01M4/8605H01M12/06Y02E60/50
Inventor 黄妞闫术芳杨柳骆禅张晗
Owner CHINA THREE GORGES UNIV
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