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Preparation method and application of hollow carbon sphere micro-nano agglomerate/sulfur composite material

A hollow carbon sphere and composite material technology, which is applied to sulfur compounds, chemical instruments and methods, carbon fluoride, etc., can solve the problem of low tap density of nano hollow carbon spheres, reduced active substance content, and easy cracking and powder removal of pole pieces. problem, to achieve the effects of good cycle performance, improved tap density, and simple and convenient preparation method

Active Publication Date: 2018-10-12
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, nano hollow carbon spheres have the characteristics of low tap density, which leads to poor manufacturability during the preparation of battery pole pieces. When the pole piece is thickly coated, it is easy to crack and drop powder, and more binders are required, which reduces the active material in the pole piece. Tablet content

Method used

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  • Preparation method and application of hollow carbon sphere micro-nano agglomerate/sulfur composite material

Examples

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Embodiment 1

[0035]A method for preparing hollow carbon sphere micro-nano aggregates, comprising the following steps:

[0036] (1) Add 15ml of tetraethyl orthosilicate to a mixed solvent consisting of 10ml of ammonia water, 200ml of ethanol, and 100ml of water under magnetic stirring, stir at 30°C for 2h, then add 10g of glucose, stir for 2h, place in water React in a hot kettle at 190°C for 12 hours, and centrifugally filter the product to obtain caramelized glucose-coated silicon dioxide nanosphere powder.

[0037] (2) Disperse 2.0 g of caramelized glucose-coated silica nanosphere powder in 20 ml of water, ultrasonicate for 3 h, and then dissolve 10 g of LA133 (multi-component polyacrylonitrile copolymer water-based adhesive) aqueous solution with a solid content of 10% Add dropwise to the above dispersion liquid and stir evenly, and stir at 80°C until evaporated to dryness to obtain a hollow carbon sphere micro-nano structure precursor.

[0038] (3) The hollow carbon sphere micro-nano ...

Embodiment 2

[0043] A method for preparing hollow carbon sphere micro-nano aggregates, comprising the following steps:

[0044] (1) Add 15ml of tetraethyl orthosilicate to a mixed solvent of 10ml of ammonia, 200ml of ethanol, and 10ml of water under magnetic stirring, stir at 30°C for 10min, then add 10ml of resorcinol in ethanol ( Containing 1.44g resorcinol), 2.12g formaldehyde aqueous solution (mass fraction of formaldehyde is 37wt%), continue to stir for 12h, then react at 80°C-120°C for 12h-24h, separate the solid-liquid of the obtained product, and obtain yellow phenolic aldehyde Resin-coated silica nanosphere powder.

[0045] (2) Disperse 2.0 g of phenolic resin-coated silica nanosphere powder in 20 ml of water, ultrasonicate for 3 h, then add 10 g of an aqueous solution of polyurethane adhesive with a solid content of 10% to the above dispersion and stir evenly, 100 °C until evaporated to dryness to obtain a hollow carbon sphere micro-nano structure precursor.

[0046] (3) The ho...

Embodiment 3

[0050] A method for preparing a hollow carbon sphere micro-nano aggregate / sulfur composite material, comprising the following steps:

[0051] (1) Add 15ml of tetraethyl orthosilicate to a mixed solvent of 10ml of ammonia, 200ml of ethanol, and 10ml of water under magnetic stirring, stir at 30°C for 10min, then add 10ml of resorcinol in ethanol ( Containing 1.44g resorcinol), 2.12g formaldehyde aqueous solution (mass fraction of formaldehyde is 37wt%), continue to stir for 12h, then react at 80°C-120°C for 12h-24h, separate the solid-liquid of the obtained product, and obtain yellow phenolic aldehyde Resin-coated silica nanosphere powder.

[0052] (2) Disperse 2.0g of phenolic resin-coated silica nanosphere powder in 20ml of water, ultrasonicate for 3h, and then add 10g of LA133 (multi-component polyacrylonitrile copolymer water-based adhesive) solution with a solid content of 10% dropwise into the Stir in the above dispersion liquid evenly, and stir at 80° C. until evaporated...

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Abstract

A preparation method of a hollow carbon sphere micro-nano agglomerate / sulfur composite material comprises the following steps: a) uniformly dispersing organic material-coated inorganic nano-spheres inwater or a water and alcohol solvent to obtain a mixed solution; b) completely dissolving a certain mass of an aqueous binder in water, adding the obtained aqueous solution to the mixed solution under stirring, and carrying out heating drying to evaporate away the solvent in order to obtain a nano-hollow carbon sphere micro-nano structure precursor; c) carrying out high-temperature sintering in an inert atmosphere or a hydrogen-containing reduction atmosphere to obtain nano-hollow carbon sphere micro-nano structure precursor carbide; d) placing the nano-hollow carbon sphere micro-nano structure precursor carbide in an aqueous hydrofluoric acid solution or a hot aqueous sodium hydroxide solution to etch away the above inorganic material in the nano-hollow carbon spheres, and washing and drying the obtained carbide to obtain a nano-hollow carbon sphere micro-nano agglomerate; and e) mixing the nano-hollow carbon sphere micro-nano agglomerate with a certain mass of sulfur powder, uniformly grinding the obtained mixture, placing the ground mixture in an oven full of N2, heating the ground mixture to 155 DEG C, keeping the temperature for 6-24 h, and cooling the obtained material to obtain the product.

Description

technical field [0001] The invention belongs to the field of micro-nano carbon materials and their preparation, in particular to a method for preparing hollow carbon sphere micro-nano aggregates by a binder granulation method, and hollow carbon sphere micro-nano aggregates obtained from hollow carbon sphere micro-nano aggregates / Sulfur composites and their applications in hollow carbon sphere micro-nano aggregates / sulfur composite lithium-sulfur cathodes. Background technique [0002] Porous carbon materials have broad application prospects in lithium-ion batteries, supercapacitors, chemical catalysis, gas adsorption and other fields. Nano hollow carbon spheres have rich micropore and mesoporous structure, and also have good chemical stability and thermal stability, and the hollow spherical shell can provide a closed "nano reaction space". The application of nano hollow carbon spheres in the sulfur cathode of lithium-sulfur batteries can improve its conductivity and inhibi...

Claims

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Application Information

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IPC IPC(8): C01B32/15C01B32/10C01B17/00B82Y40/00H01M4/36H01M4/38H01M4/62H01M10/052
CPCB82Y40/00C01B17/00C01B32/10C01B32/15H01M4/362H01M4/38H01M4/62H01M4/625H01M10/052Y02E60/10
Inventor 刘双科谢凯唐彪洪晓斌王丹琴许静郑春满李宇杰
Owner NAT UNIV OF DEFENSE TECH
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