Nano-structure CoSx/C cathode electro-catalytic material and preparation method thereof

An electrocatalytic material and nanostructure technology, applied in chemical instruments and methods, physical/chemical process catalysts, structural parts, etc., can solve the problems of small particle size and narrow distribution, and achieve inhibition of agglomeration, good performance, and particle size. Evenly distributed effect

Inactive Publication Date: 2014-08-06
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Literature Zhao Yun, Li Feng, Zhang Rui, Evans, David G., Duan Xue, Chemistry of Materials, 2002, 14, 4286 reported that the layered composite metal hydroxide prepared by the nucleation / crystallization isolation method has a particle size The characteristics of small and narrow distribution, so far there is no report on the application of this method to the preparation of transition metal sulfides

Method used

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  • Nano-structure CoSx/C cathode electro-catalytic material and preparation method thereof
  • Nano-structure CoSx/C cathode electro-catalytic material and preparation method thereof
  • Nano-structure CoSx/C cathode electro-catalytic material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Weigh 0.23g Co(NO 3 ) 2 ·6H 2 O and 0.3g of conductive carbon black are dissolved in 80mL of absolute ethanol to form a solution with a cobalt salt concentration of 0.01mol / L;

[0025] Weigh 0.187g Na 2 Dissolve S in 80mL of absolute ethanol to make S with a concentration of 0.03mol / L 2- solution; the two solutions were simultaneously poured into a rotating liquid film reactor and quickly mixed for 30 seconds; the rotational speed of the liquid film reactor was 4500 rpm, and the gap size between the stator and the rotor was 17 μm.

[0026] Transfer the nucleated slurry to a high-pressure reactor, and crystallize and grow at a constant temperature of 80°C for 8 hours; the reaction slurry is centrifuged and washed with deionized water for more than 5 times, and finally washed once with absolute ethanol, and the filter cake is dried in an oven at 60 Dry at ~100°C for 12 hours to obtain the final product.

[0027] The obtained CoS x / C for electrochemical performance ...

Embodiment 2

[0036] Weigh 0.19g CoCl 2 ·6H 2 O and 0.2g of carbon nanotubes were dissolved in 80mL of absolute ethanol to form a solution with a cobalt salt concentration of 0.01mol / L; weigh 0.164g (NH 4 ) 2 Dissolve S in 80mL of absolute ethanol to make S with a concentration of 0.03mol / L 2- solution; two solutions are simultaneously poured into a rotating liquid film reactor and quickly mixed, nucleating for 30 seconds, the rotating speed of the liquid film reactor is 5000rpm, and the gap size between the stator and the rotor is 17 μm; the slurry after nucleation is transferred to In a high-pressure reactor, crystallize and grow at a constant temperature of 100°C for 6 hours; the reaction slurry is centrifugally washed with deionized water for more than 5 times, and finally washed with absolute ethanol once, and the filter cake is dried in an oven at 60-100°C for 12 hours The final product, CoS x The average particle size of the particles is 2.5 nm.

Embodiment 3

[0038] Weigh 0.22g CoSO 4 ·7H 2 O and 0.3g graphene are dissolved in 80mL absolute ethanol, are made into the solution that cobalt salt concentration is 0.01mol / L; Weigh 0.312g Na 2 Dissolve S in 80mL of absolute ethanol to prepare S with a concentration of 0.05mol / L 2- solution; two solutions are simultaneously poured into a rotating liquid film reactor and quickly mixed, and the nucleation is 60 seconds. The rotating speed of the liquid film reactor is 5000rpm, and the gap size between the stator and the rotor is 15 μm; In a high-pressure reactor, crystallize and grow at a constant temperature of 80°C for 8 hours; the reaction slurry is centrifugally washed with deionized water for more than 5 times, and finally washed once with absolute ethanol, and the filter cake is dried in an oven at 60-100°C for 12 hours The final product, CoS x The average particle size of the particles was 1.3 nm.

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Abstract

The invention provides a nano-structure CoSx / C cathode electro-catalytic material and a preparation method thereof. The material is formed by supporting CoSx on a carbon material, wherein x is greater than or equal to 0.20 and smaller than or equal to 5. The nano-structure CoSx / C cathode electro-catalytic material is characterized in that CoSx nano particles are uniformly dispersed, the particle size distribution is narrow, and the particle size is 1-5 nm; the carbon material is any of amorphous carbon black, carbon nano tubes and graphene. According to the preparation method, soluble cobalt salt, soluble sulfide, absolute ethyl alcohol and a carrier carbon material are taken as raw materials, nucleus formation and crystallization are carried out by rotating a liquid film reactor, the nucleus formation and growth of crystals on the carrier are realized through the metal cation adsorption effect of the carrier carbon material, and finally obtained CoSx nano particles are good in dispersibility and are uniform, and the particle size is smaller than 5nm and is extremely smaller than that of ordinary cobalt sulfide particles. The preparation method is simple, the raw materials are readily available, and industrial production is facilitated. CoSx / C has good cathode electro-catalytic performance, and can be used in the field of cathode catalytic materials of fuel cells.

Description

[0001] Field [0002] The invention relates to a cobalt sulfide cathode electrocatalytic material and a preparation method thereof, in particular to a supported cobalt sulfide and a preparation method thereof. The supported cobalt sulfide can be used as a high-efficiency cathode catalyst material for fuel cells. Background technique [0003] With the escalation of energy problems and the worsening of ecological and environmental problems, developed countries are stepping up the deployment and implementation of hydrogen energy strategies to accelerate the transition from a carbon-based economic energy form - carbon economy to a hydrogen-based economic energy form - hydrogen economic transformation. Hydrogen energy is the most ideal due to its high calorific value (the heat of burning 1kg of hydrogen is equivalent to the heat of burning 3kg of gasoline or 4.5kg of coke), abundant sources, no greenhouse gas and pollutant emissions, and the ability to regenerate solar and wind en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043H01M4/90
CPCY02E60/50
Inventor 冯拥军席静敏李殿卿唐平贵冯俊婷
Owner BEIJING UNIV OF CHEM TECH
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