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Foam cobalt in-situ vulcanization nanoflower spherical Co4S3@Co hydrogen evolution material and method for preparing same

A foam, hydrogen evolution technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of poor material cycle stability, high hydrogen evolution overpotential, and achieve high stability, simple process, The effect of excellent electrocatalytic hydrogen production performance

Active Publication Date: 2018-11-27
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a foamed cobalt in situ vulcanization synthesis of nano-spherical Co 4 S 3 Preparation method of @Co hydrogen evolution composite negative electrode material to solve the problems of high hydrogen evolution overpotential and poor cycle stability of current electrocatalytic hydrogen production materials

Method used

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  • Foam cobalt in-situ vulcanization nanoflower spherical Co4S3@Co hydrogen evolution material and method for preparing same
  • Foam cobalt in-situ vulcanization nanoflower spherical Co4S3@Co hydrogen evolution material and method for preparing same
  • Foam cobalt in-situ vulcanization nanoflower spherical Co4S3@Co hydrogen evolution material and method for preparing same

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Experimental program
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Effect test

Embodiment 1

[0031] (1) Cut the foamed cobalt into 2×2.5 cm strips, place them in acetone, absolute ethanol and distilled water for ultrasonic cleaning for 10 min, and etch the cleaned foamed cobalt in 1% nitric acid for 15 minutes. min, washed with distilled water; (2) Accurately weigh the product obtained in step (1), and weigh thiosemicarbazide according to the ratio of cobalt source to sulfur source material as 2: 3; (3) Weigh the product in step (2) Dissolve the obtained thiosemicarbazide into 140 mL of deionized water and absolute ethanol (equal volume) mixed solution, add 0.5% galactose with a molar mass of thiosemicarbazide dropwise, stir evenly and immerse the cobalt foam obtained in step (1) into Wherein; (4) Transfer 200 mL of the mixture obtained in step (3) to a polytetrafluoroethylene-lined autoclave, and ° After performing solvothermal reaction at C for 10 h, cool down to room temperature naturally, wash with deionized water repeatedly, then wash with absolute ethanol, and d...

Embodiment 2

[0033] (1) Cut the foamed cobalt into 2×2.5 cm strips, place them in acetone, absolute ethanol and distilled water for cleaning and ultrasonic cleaning for 10 min, and etch the cleaned foamed cobalt in 1% hydrochloric acid for 10 minutes. min, washed with distilled water; (2) Accurately weigh the product obtained in step (1), and weigh thiourea according to the ratio of cobalt source to sulfur source material as 3:2; (3) Weigh the product in step (2) thiourea was dissolved in 140 mL of deionized water and absolute ethanol (equal volume) mixed solution, 1.0% thiourea molar glucose was added dropwise, and after stirring evenly, the foamed cobalt obtained in step (1) was immersed in it; (4 ) Transfer 200 mL of the mixture obtained in step (3) to a polytetrafluoroethylene-lined autoclave at 160 ° After solvothermal reaction at C for 8 h, cool down to room temperature naturally, wash with deionized water repeatedly, then wash with absolute ethanol, and dry for later use; (5) Place ...

Embodiment 3

[0035] (1) Cut the foamed cobalt into 2×2.5 cm strips, place them in acetone, absolute ethanol and distilled water for ultrasonic cleaning for 10 min respectively, and etch the cleaned foamed cobalt in 2% sulfuric acid for 20 minutes. min, washed with distilled water; (2) Accurately weigh the product obtained in step (1), and weigh thiourea dioxide according to the ratio of cobalt source and sulfur source material as 1:1; (3) Weigh the product obtained in step (2) Dissolve thiourea dioxide in 140 mL of deionized water and absolute ethanol (equal volume) mixed solution, add 2.0% thiourea dioxide molar amount of fructose dropwise, stir well and immerse the cobalt foam obtained in step (1); (4 ) Transfer 200 mL of the mixture obtained in step (3) to a polytetrafluoroethylene-lined autoclave at 170 ° After solvothermal reaction at C for 8 h, cool down to room temperature naturally, wash with deionized water repeatedly, then wash with absolute ethanol, and dry for later use; (5) Pl...

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Abstract

The invention discloses a method for preparing a flower spherical Co4S3@Co hydrogen evolution composite material grown on foam cobalt in an in-situ manner. The method particularly includes steps of ultrasonically cleaning the foam cobalt to carry out surface acid etching; weighing sulfur-containing compounds, dissolving the sulfur-containing compounds in deionized water and absolute ethyl alcoholmixed solution, adding a few reducing carbohydrate into the deionized water and absolute ethyl alcohol mixed solution, uniformly stirring the sulfur-containing compounds, the deionized water and absolute ethyl alcohol mixed solution and the reducing carbohydrate and then immersing the treated foam cobalt in the sulfur-containing compounds, the deionized water and absolute ethyl alcohol mixed solution and the reducing carbohydrate; transferring mixtures into high-pressure reaction kettles, carrying out solvothermal vulcanization reaction and then cooling, cleaning and drying reaction products;placing vulcanized foam cobalt in tube furnaces, carrying out programmed heating and calcining under gas protection, and preserving heat in reducing mixed protective gas to obtain flower spherical Co4S3 composite materials closely grown on the foam cobalt. The method has the advantages that the flower spherical Co4S3@Co hydrogen evolution composite material prepared by the aid of the method growsin the in-situ manner, is in close contact with the foam cobalt, is favorable for electric charge transfer and utilization and is excellent in electro-catalytic hydrogen production performance; the method includes simple processes, reaction conditions are mild, products are high in hydrogen evolution stability, and the like.

Description

technical field [0001] The invention relates to in-situ growth of nano-spherical Co on foamed cobalt 4 S 3 @Co hydrogen evolution material and preparation method, specifically involves using foamed cobalt as cobalt source, sulfur compound as sulfur source, obtained after temperature-programmed roasting under certain hydrothermal conditions and required atmosphere, the material has good electrochemical stability and electrochemical stability. Catalytic hydrogen evolution ability. Background technique [0002] Energy, as a strategic resource, is highly concerned by countries all over the world. With the global climate change and environmental pollution problems brought about by traditional fossil energy represented by coal, oil, and natural gas becoming increasingly prominent, people's urgency to develop environmentally friendly new energy sources to replace fossil fuels has increased sharply. More and more Scientists have devoted themselves to basic research and applicatio...

Claims

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Application Information

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IPC IPC(8): B01J27/043B01J35/08B01J35/10C25B1/04C25B11/06
CPCC25B1/04C25B11/04B01J27/043B01J35/51B01J35/61Y02E60/36
Inventor 张丽粱青满杨海华阎建辉黄杨杨鹏
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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