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

A technology of carbon anode materials and ferrous sulfide, applied in battery electrodes, electrochemical generators, electrical components, etc., can solve problems such as poor cycle performance, shorten the transmission path, facilitate stable shuttle, and facilitate effective contact Effect

Active Publication Date: 2018-09-28
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 Applications(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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