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Sulfur-vacancy-rich hollow sulfide microspheres and preparation method and application thereof

A sulfide and hollow technology, applied in the field of chemical materials, can solve the problems of low conductivity, poor rate and stability, and expansion of the lattice structure system of transition metal sulfides, so as to increase electrochemical active sites and improve stability. The effect of improving the electrical conductivity

Pending Publication Date: 2021-06-18
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the conductivity of transition metal sulfides is still low, and during the electrochemical test, there will be problems such as the system expansion of the lattice structure, resulting in poor rate and stability.

Method used

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  • Sulfur-vacancy-rich hollow sulfide microspheres and preparation method and application thereof
  • Sulfur-vacancy-rich hollow sulfide microspheres and preparation method and application thereof
  • Sulfur-vacancy-rich hollow sulfide microspheres and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Dissolve 0.2mmol of cobalt nitrate and 0.1mmol of nickel nitrate in a mixed solution of 15ml of N,N-dimethylformamide and 15ml of acetone; add 0.15mmol of isophthalic acid, stir at room temperature for 6h, transfer to water In the hot kettle, set the solvothermal reaction temperature to 160° C., and the reaction time to 4 hours; after the hydrothermal kettle is cooled, centrifuge, wash and vacuum-dry to obtain nickel-cobalt ion coordination polymer microspheres. Its particle size is about 1-2 μm and it is a solid sphere.

Embodiment 2

[0039] Dissolve 0.2mmol of cobalt nitrate and 0.1mmol of nickel nitrate in a mixed solution of 15ml of N,N-dimethylformamide and 15ml of acetone; add 0.15mmol of isophthalic acid, stir at room temperature for 6h, transfer to water In the hot kettle, set the solvothermal reaction temperature to 160 ° C, and the reaction time to 4 h; after the hydrothermal kettle is cooled, centrifuge, wash and vacuum dry to obtain nickel-cobalt ion coordination polymer microspheres; weigh 30 mg of nickel-cobalt ion coordination polymer microspheres; Polymer microspheres and 60 mg of thioacetyl were dispersed in 30 ml of absolute ethanol. After ultrasonic treatment for 15 min, they were transferred to a hydrothermal kettle. The solvothermal reaction temperature was 160 ° C and the reaction time was 2 h. The sulfide obtained by the reaction presents a core-shell structure with a particle size of 1-2 μm, and the surface is no longer smooth.

Embodiment 3

[0041] Dissolve 0.133mmol of cobalt nitrate and 0.067mmol of nickel nitrate in a mixed solution of 15ml of N,N-dimethylformamide and 15ml of acetone; add 0.2mmol of isophthalic acid, stir at room temperature for 6h, transfer to water In the hot kettle, set the solvothermal reaction temperature to 160 ° C, and the reaction time to 4 h; after the hydrothermal kettle is cooled, centrifuge, wash and vacuum dry to obtain nickel-cobalt ion coordination polymer microspheres; weigh 30 mg of nickel-cobalt ion coordination polymer microspheres; Polymer microspheres and 60 mg of thioacetyl were dispersed in 30 ml of absolute ethanol. After ultrasonic treatment for 15 min, they were transferred to a hydrothermal kettle. The solvothermal reaction temperature was 160 ° C and the reaction time was 6 h. The sulfide obtained by the reaction is in the shape of hollow microspheres, with a particle size of 1-2 μm and a shell thickness of about 20-30 nm; at the same time, according to the peak area...

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Abstract

The invention relates to a preparation method of sulfur-vacancy-rich hollow sulfide microspheres. The method specifically comprises the following steps: dissolving cobalt nitrate and nickel nitrate in equal volume of N, N-dimethylformamide and acetone, adding a chelating agent, and carrying out solvothermal reaction to obtain coordination polymer microspheres containing nickel and cobalt ions; secondly, dispersing the obtained coordination polymer microspheres and a vulcanizing agent into an organic solvent, and reacting to obtain hollow sulfide microspheres; and performing sodium borohydride reduction treatment on the prepared hollow sulfide, performing centrifugation, washing and drying, and then obtaining the hollow sulfide microspheres rich in sulfur vacancies. The particle size is 1-2.5 [mu] m, the shell thickness is 15-30 nm, and the specific capacity of the material can reach 763.4 C g <-1 > (the current density is 1A g <-1 >).

Description

technical field [0001] The invention relates to the field of chemical materials, in particular to a hollow sulfide microsphere rich in sulfur vacancies and its preparation method and application. Background technique [0002] Supercapacitors have attracted extensive attention due to their high power density and long cycle life. However, its energy density is between secondary batteries and traditional capacitors. How to improve the performance of supercapacitors as much as possible without sacrificing the advantages of supercapacitors is the mainstream of current research. The hybrid capacitor is constructed, and the negative electrode material uses the active material with electric double layer capacitance, and the positive electrode uses the battery-grade electrode material with redox behavior, which can achieve high energy density under the premise of ensuring high power density. Therefore, the performance improvement of supercapacitors mainly focuses on the design and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00B82Y40/00B01J13/02H01G11/26H01G11/30H01G11/86
CPCC01G53/006B82Y40/00B01J13/02H01G11/86H01G11/26H01G11/30C01P2004/34C01P2004/61C01P2004/64C01P2006/40C01P2002/72C01P2004/03C01P2004/04C01P2002/85C01P2004/80H01M4/5815Y02E60/10C01G53/11H01M2004/021
Inventor 邵自强贾帅魏洁黄珍龚白雪
Owner BEIJING INSTITUTE OF TECHNOLOGYGY