Macroporous spherical zinc sulfide/ferrous sulfide/carbon negative electrode material and preparation method thereof

A carbon anode material, ferrous sulfide technology

Active Publication Date: 2020-11-20
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the preparation method of this material is simple, the obtained ferrous carbonate negative electrode material is applied to lithium-ion batteries for the first time, and the first discharge specific capacity reaches 900-1110mAh / g at 0.05-3.0V, 200mA / g current density, and after 100 cycles The discharge specific capacity is only 585-640mAh / g, and the cycle performance of the material is poor

Method used

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  • Macroporous spherical zinc sulfide/ferrous sulfide/carbon negative electrode material and preparation method thereof
  • Macroporous spherical zinc sulfide/ferrous sulfide/carbon negative electrode material and preparation method thereof
  • Macroporous spherical zinc sulfide/ferrous sulfide/carbon negative electrode material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Add 2 mmol of iron acetylacetonate, 3 mmol of zinc nitrate hexahydrate, 5 mmol of thioacetamide and 2.5 g (13 mmol) of citric acid into 50 mL of deionized water, stir and dissolve to a homogeneous solution;

[0045] (2) Pour the solution obtained in step (1) into a 100 mL polytetrafluoroethylene high-temperature reaction kettle, seal the steel shell, place in a blast oven, heat to 180 °C, react for 16 h, cool naturally to room temperature, filter, The filtrate was cross-washed four times with ethanol and deionized water respectively, and then placed in a blast oven at 60°C for 24 h to obtain a black powder;

[0046] (3) Calcining the black powder obtained in step (2) at 600°C for 3 hours in a high-purity argon atmosphere, and cooling naturally to room temperature to obtain a macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material.

[0047] Such as figure 1 As shown, the zinc sulfide and ferrous sulfide in the macroporous spherical zinc...

Embodiment 2

[0052] (1) Add 2 mmol of iron acetylacetonate, 3 mmol of zinc nitrate hexahydrate, 5 mmol of thioacetamide and 2 g (9.52 mmol) of trimesic acid into 50 mL of deionized water, stir and dissolve to a homogeneous solution;

[0053] (2) Pour the solution obtained in step (1) into a 100 mL polytetrafluoroethylene high-temperature reaction kettle, seal the steel shell, place in a blast oven, heat to 200 °C, react for 10 h, cool naturally to room temperature, filter, Wash the filtrate three times successively with ethanol and deionized water, then place it in a blast oven at 100°C, and dry it for 20 h to obtain a black powder;

[0054] (3) Calcining the black powder obtained in step (2) at 450° C. for 5 hours in a high-purity argon atmosphere, and naturally cooling to room temperature to obtain a macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material.

[0055] After testing, the zinc sulfide and ferrous sulfide in the macroporous spherical zinc sulfide / ...

Embodiment 3

[0061] (1) Add 2.5 mmol of ferric citrate, 5 mmol of zinc chloride hexahydrate, 22.5 mmol of thiourea and 1.5 g (7.81 mmol) of citric acid into 50 mL of deionized water, stir and dissolve to a homogeneous solution;

[0062] (2) Pour the solution obtained in step (1) into a 100 mL polytetrafluoroethylene high-temperature reaction kettle, seal the steel shell, place in a blast oven, heat to 160 °C, react for 20 h, cool naturally to room temperature, filter, The filtrate was cross-washed four times with ethanol and deionized water respectively, and then placed in a blast oven at 80°C for 12 h to obtain a black powder;

[0063] (3) The black powder obtained in step (2) was roasted at 500 °C for 4 hours in a high-purity nitrogen atmosphere, and cooled naturally to room temperature to obtain a macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material.

[0064] After testing, the zinc sulfide and ferrous sulfide in the macroporous spherical zinc sulfide / fe...

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Abstract

The invention discloses a macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material and a preparation method thereof. The negative electrode material is prepared by the following steps: (1) adding an iron source, a zinc source, a sulfur source and ternary organic carboxylic acid into water, and stirring for dissolving to obtain a homogeneous solution; (2) sealing, performing a heating reaction, cooling, filtering, washing and drying to obtain black powder; and (3) sintering and cooling in an inert atmosphere to obtain the macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material. In the macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material, zinc sulfide and ferrous sulfide are pure phases, the secondaryparticle size is 5 to 8[mu]m, and a pore canal which is 0.1 to 2.0[mu]m in diameter is included. A battery assembled with the macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material has the advantages of stable structure in a charging and discharging process, small volume expansion, high conductivity, highly-reversible charging-discharging reaction and high rate capability. The method is simple, convenient, low in raw material cost, and suitable for industrial production.

Description

technical field [0001] The invention relates to a negative electrode material for a lithium ion battery and a preparation method thereof, in particular to a macroporous spherical zinc sulfide / ferrous sulfide / carbon negative electrode material and a preparation method thereof. Background technique [0002] With the increase of people's demand for portable devices and the development of commercial lithium-ion batteries, the current mainstream graphite anode has been unable to meet people's demand for lithium-ion battery capacity. Both iron and zinc are cheap metals. When their sulfides are used as anode materials for lithium-ion batteries, they have a high theoretical specific capacity. However, their structures tend to collapse during charging and discharging, which affects specific capacity and cycle performance. [0003] CN104882604B discloses a kind of ZnS-Al 2 o 3 / N-C composite electrode material and preparation method thereof, the composite electrode material is compo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M10/0525
CPCH01M4/362H01M4/5815H01M4/583H01M10/0525Y02E60/10
Inventor 童汇姚赢赢毛高强龚竹月郑俊超张宝喻万景
Owner CENT SOUTH UNIV
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