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A kind of preparation method of negative electrode composite material of lithium ion battery

A technology for lithium ion batteries and composite materials, which is applied in the field of preparation of negative electrode materials for lithium ion batteries, can solve the problems of loss of re-stacking active area, rapid decay of cycle performance, and no good solution, so as to improve cycle stability performance, The effect of stable cycle performance and high specific capacity

Active Publication Date: 2021-05-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] CN107579210A discloses a lithium ion battery negative electrode material GeO x / CNTs preparation method, self-assembled carbon network structure GeO x Although the capacity of / CNTs anode material has been greatly improved, the cycle performance decays rapidly
However, the problems of re-stacking and loss of active regions in MXene nanosheets have not been well resolved.

Method used

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  • A kind of preparation method of negative electrode composite material of lithium ion battery
  • A kind of preparation method of negative electrode composite material of lithium ion battery
  • A kind of preparation method of negative electrode composite material of lithium ion battery

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Embodiment 1

[0044] This embodiment includes the following steps:

[0045] (1) Take 30.0 g hydrofluoric acid aqueous solution (mass fraction 40%), put it into a polytetrafluoroethylene tank, and add 1.0 g Ti 3 AlC 2 , heated and stirred at 600 rpm, constant temperature 90°C for 7 h, etched, removed Al layer, and mixed solution I was obtained;

[0046] (2) Centrifuge the mixed solution I obtained in step (1) at 10,000 rpm, wash with deionized water until the pH of the washing solution reaches neutral, and then sonicate at 350 W for 2 h; at 5,000 rpm Centrifuge again, wash with deionized water and absolute ethanol four times, and dry in vacuum at 80 °C for 24 h to obtain MXene powder-Ti 3 C 2 T x Material;

[0047] (3) Take the Ti obtained in step (2) 3 C 2 T x Add 0.05 g of the material to 40 ml of deionized water, ultrasonicate at 200 W for 10 min to obtain a uniform aqueous suspension, add 2 ml of ammonia water with a concentration of 13.38 mol / L, stir at 600 rpm for 1 h, and then...

Embodiment 2

[0060] This embodiment includes the following steps:

[0061] (1) Take 30.0 g hydrofluoric acid aqueous solution (mass fraction 40%) and add it to a polytetrafluoroethylene tank, and then add 1.0 g Ti 3 AlC 2 , at 1000 rpm, and then at a constant temperature of 120 °C, stirring for 12 h; performing etching to remove the Al layer to obtain a mixed solution I;

[0062] (2) Centrifuge the mixed solution I obtained in step (1) at 10,000 rpm, wash with deionized water until the pH value of the solution is neutral, then sonicate at 400 W for 4 h, at 10,000 rpm, The precipitate was cross-washed with deionized water and absolute ethanol four times, and dried in vacuum at 90 °C for 12 h to obtain Ti 3 C 2 T x material (an MXene material);

[0063] (3) Ti obtained in step (2) 3 C 2 T x Mix 0.25 g of the material with 40 ml of deionized water, sonicate at 400 W for 60 min to obtain a homogeneous aqueous suspension, then add 2.5 ml of 13.38 mol / L ammonia water, stir at 1000 rpm fo...

Embodiment 3

[0072] This embodiment includes the following steps:

[0073] (1) Take 30.0 g hydrofluoric acid aqueous solution (mass fraction 40%) and add it to a polytetrafluoroethylene tank, and then add 1.0 g Ti 3 AlC 2 , at a constant temperature of 50°C at 400 rpm, stirred for 5 h, etched to remove the Al layer, and mixed solution I was obtained;

[0074] (2) Centrifuge the mixed solution I obtained in step (1) at 3000 rpm, wash with deionized water until the pH of the solution is neutral, then sonicate at 200 W for 0.5 h, and at 3000 rpm, dissolve The precipitate was cross-washed four times with deionized water and absolute ethanol, and dried in vacuum at 45 °C for 48 h to obtain Ti 3 C 2 T x material (an MXene material);

[0075] (3) Ti obtained in step (2) 3 C 2 T x Mix 0.025 g of the material with 40 ml of deionized water, sonicate at 200 W for 5 min to obtain a homogeneous aqueous suspension, then add 1 ml of 13.38 mol / L ammonia water, stir at 400 rpm for 1 h, and then tak...

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Abstract

A method for preparing a lithium-ion battery negative electrode composite material, comprising the following steps: (1) taking Ti 3 AlC 2 Add hydrofluoric acid aqueous solution; (2) Centrifuge the mixed solution I, first wash until the pH value of the solution is neutral, sonicate, centrifuge again, second wash, and dry; (3) Ti 3 C 2 T x The material is added to deionized water, ammonia water, GeO 2 powder; (4) NaBH 4 Add water and dissolve in ice bath to get NaBH 4 aqueous solution; drop the mixed solution II into NaBH 4 In the aqueous solution, the negative electrode composite material of the lithium ion battery is obtained. In the present invention, the T with good shape is etched by HF acid 3 iC 2 T x , by adding GeO x It grows relatively uniformly on the interlayer and surface of MXene, effectively confining GeO x The problem of volume expansion during charge and discharge, thus greatly improving the GeO x The cycle stability performance of the material during charge and discharge.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion battery negative electrode material, in particular to a lithium ion battery negative electrode composite material GeO x / The preparation method of MXene. Background technique [0002] In recent years, with the rapid development of electronic equipment, electric vehicles and other industries, research on energy storage materials with high energy efficiency, environmental friendliness and abundant resources has become the only way for human society to achieve sustainable development. In order to meet the huge market demand, it is far from enough to measure the pros and cons of battery materials only by energy density, charge and discharge rate and other properties. The manufacturing cost and energy consumption of batteries, whether they cause pollution to the environment, and the recycling rate of resources will also become important indicators for evaluating battery materials. Therefore, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/48H01M4/62H01M10/0525
CPCH01M4/366H01M4/483H01M4/628H01M10/0525Y02E60/10
Inventor 郑俊超宋生超安长胜左定川汤林波贺振江童汇
Owner CENT SOUTH UNIV