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Hollow microspheres with multilayer nickelous sulfide shells, preparation method and application thereof

A technology of micron spheres and nickel sulfide, applied in the direction of nickel sulfide, hybrid capacitor electrodes, etc., can solve the problem of less nickel sulfide materials, and achieve the effect of low price, wide source, and simple vulcanization process

Inactive Publication Date: 2017-01-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, there are few reports on nickel sulfide materials with multilayer hollow structures, and few literatures report the conversion technology of oxides and sulfides.

Method used

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  • Hollow microspheres with multilayer nickelous sulfide shells, preparation method and application thereof
  • Hollow microspheres with multilayer nickelous sulfide shells, preparation method and application thereof
  • Hollow microspheres with multilayer nickelous sulfide shells, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 50 mg of carbon spheres with a diameter of 1 μm were ultrasonically dispersed in a mixed solution of 100 ml of water and ethanol (volume ratio 1:1), 0.2 g of nickel nitrate and 1 g of urea were added and mixed evenly, the mixed solution was stirred at 80 °C for 12 h, and the obtained product was centrifuged. It was separated and washed with deionized water and ethanol, and then dried in an incubator at 60 °C for 12 h. The obtained powder was heat-treated in air at 450 °C for 2 h, and the heating rate was 3 °C / min. The obtained nickel oxide hollow structure microspheres were mixed with sulfur powder (the Ni / S molar ratio was 1:1), transferred to a tube furnace, and calcined at 400 °C for 4 h in an argon atmosphere, that is, the hollow shell of multi-layer nickel sulfide shell. Microspheres. The prepared nickel sulfide material is uniformly mixed according to 80wt.%, acetylene black 10wt.% and FVDF10wt.% to make a slurry, which is uniformly coated on a nickel mesh (1*2cm...

Embodiment 2

[0032] 50 mg of carbon spheres with a diameter of 1 μm were ultrasonically dispersed in 100 ml of a mixed solution of water and ethanol (volume ratio 2:1), 0.3 g of nickel sulfate and 1 g of urea were added to mix well, the mixed solution was stirred at 100 ° C for 12 h, and the resulting product was centrifuged. It was separated and washed with deionized water and ethanol, and then dried in an incubator at 60 °C for 12 h. The obtained powder was heat-treated in air at 450 °C for 2 h, and the heating rate was 3 °C / min. The obtained hollow-structured nickel oxide microspheres were mixed with sulfur powder (Ni / S molar ratio of 1:2), transferred to a tube furnace, and calcined at 400 °C for 4 h in an argon atmosphere, that is, a hollow core with a multi-layer nickel sulfide shell. Microspheres.

Embodiment 3

[0034] 50 mg of carbon spheres with a diameter of 1 μm were ultrasonically dispersed in 100 ml of a mixed solution of water and methanol (volume ratio 1:1), 0.2 g of nickel nitrate and 1 g of urea were added, and the mixture was evenly mixed. It was separated and washed with deionized water and ethanol, and then dried in an incubator at 60 °C for 12 h. The obtained powder was heat-treated in air at 500 °C for 2 h, and the heating rate was 3 °C / min. The obtained nickel oxide hollow microspheres were mixed with thiourea (the molar ratio of Ni / S was 1:2), transferred to a tube furnace, and calcined at 400 °C for 4 h in an argon atmosphere to obtain a hollow multi-layer nickel sulfide shell. Microspheres.

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Abstract

The invention discloses hollow microspheres with multilayer nickelous sulfide shells, a preparation method and application thereof. The preparation method comprises the following steps: growing a nickel precursor on the carbon sphere surfaces by low-temperature solution precipitation, calcining in air to obtain the hollow microspheres with multilayer nickel oxide shells, and vulcanizing the nickel oxide microspheres in a pipe furnace to obtain the complete hollow microspheres with multilayer nickelous sulfide shells. The unique multilayer-shell hollow structure is beneficial to effective infiltration of the electrolyte, and the electrolyte can sufficiently contact the active substances, thereby enhancing the electrochemical properties of the material. The supercapacitor electrode material prepared from the multilayer-shell hollow nickelous sulfide microspheres has the advantages of favorable electrochemical properties, simple technique and mild conditions.

Description

technical field [0001] The invention relates to a hollow microsphere with a multi-layer nickel sulfide shell, its preparation method and its application in a super capacitor. Background technique [0002] Supercapacitors, also known as electrochemical capacitors, are power sources with special properties between traditional capacitors and batteries. Supercapacitors have the advantages of long cycle life, short charging time, wide operating temperature range, high power density, and no environmental pollution. [0003] Pseudocapacitors with sulfide electrode materials have higher capacitances compared to carbon-based electric double-layer capacitors. When nickel sulfide is used as an electrode material, underpotential deposition is carried out on the electrode surface or in the bulk phase, and energy storage by highly reversible chemical adsorption or electrochemical redox reaction occurs. The process is: [0004] Since nickel sulfide is used in the energy field, researc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11H01G11/30
CPCY02E60/13C01G53/11C01P2002/72C01P2004/03C01P2004/04C01P2004/34H01G11/30
Inventor 潘安强王亚平
Owner CENT SOUTH UNIV
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