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A kind of expanded interlayer spacing microcrystalline graphite material and its preparation method and application in sodium ion battery

A technology of microcrystalline graphite and interlayer spacing, applied in battery electrodes, secondary batteries, chemical instruments and methods, etc., to achieve the effects of long cycle stability, high tap density, and improved rate performance

Active Publication Date: 2020-10-27
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the existing problems of using microcrystalline graphite as negative electrode material of secondary batteries, the purpose of the present invention is to provide a kind of enlarged interlayer spacing with the characteristics of large interlayer spacing, suitable specific surface area, good electrical conductivity, excellent electrical conductivity and mechanical strength, etc. Microcrystalline graphite material

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  • A kind of expanded interlayer spacing microcrystalline graphite material and its preparation method and application in sodium ion battery

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Take 20g of microcrystalline graphite and add it to the crusher for cutting and crushing, and then sieve through a 200-mesh sieve to obtain microcrystalline graphite powder; the volume ratio of industrial grade hydrochloric acid: industrial grade hydrofluoric acid: deionized water is 5:3:2 Prepare 100ml of mixed acid solution, pour microcrystalline graphite powder into the mixed acid solution, heat and stir with a magnetic stirrer, the stirring temperature is 80°C, and the mixed acid treatment time is 12h; filter and wash with deionized water for 3 times, and then use 100ml of absolute ethanol was used for ultrasonic cleaning to remove the ash impurities remaining in the micropores. The ultrasonic oscillation time was 20 minutes; then filtered and washed with deionized water for 3 times; placed in an oven at 60°C for 6 hours to obtain purified microcrystals Graphite powder; the microcrystalline graphite obtained is mixed with 6g sodium nitrate, 160g (100mL) concentrated ...

Embodiment 2

[0046] Take 20g of microcrystalline graphite and add it to the crusher for cutting and crushing, and then sieve through a 200-mesh sieve to obtain microcrystalline graphite powder; the volume ratio of industrial grade hydrochloric acid: industrial grade hydrofluoric acid: deionized water is 5:3:2 Prepare 100ml mixed acid solution, pour the microcrystalline graphite powder into the mixed acid solution, heat and stir with a magnetic stirrer, the stirring temperature is 70°C, and the mixed acid treatment time is 18h; filter and wash with deionized water for 3 times, and then use 100ml of absolute ethanol was used for ultrasonic cleaning to remove the ash impurities remaining in the micropores. The ultrasonic oscillation time was 20 minutes; then filtered and washed with deionized water for 3 times; placed in an oven at 60°C for 6 hours to obtain purified microcrystals Graphite powder; the obtained microcrystalline graphite is mixed with 5g sodium nitrate, 140g (87.5mL) concentrate...

Embodiment 3

[0049] Take 30g of microcrystalline graphite and add it to the crusher for cutting and crushing, and then sieve through a 200-mesh sieve to obtain microcrystalline graphite powder; the volume ratio of industrial grade hydrochloric acid: industrial grade hydrofluoric acid: deionized water is 4:4:2 Prepare 100ml mixed acid solution, pour the microcrystalline graphite powder into the mixed acid solution, heat and stir with a magnetic stirrer, the stirring temperature is 90°C, and the mixed acid treatment time is 12h; filter and wash with deionized water for 3 times, and then use 100ml of absolute ethanol was used for ultrasonic cleaning to remove the ash impurities remaining in the micropores. The ultrasonic oscillation time was 20 minutes; then filtered and washed with deionized water for 3 times; placed in an oven at 60°C for 6 hours to obtain purified microcrystals Graphite powder; the microcrystalline graphite obtained is mixed with 4.2g sodium nitrate, 120g (75mL) concentrate...

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Abstract

The invention discloses an interlayer spacing-amplified microcrystalline graphite material, a preparation method thereof and application thereof in a sodium-ion battery. The preparation method comprises the following steps: carrying out acid liquid purification on microcrystalline graphite micro-powder, so as to obtain purified microcrystalline graphite; carrying out oxidation intercalation on thepurified microcrystalline graphite, so as to obtain oxidized microcrystalline graphite; and carrying out reduction on the oxidized microcrystalline graphite, so as to obtain the interlayer spacing-amplified microcrystalline graphite material, wherein the specific surface area of the material is 10m<2> / g-100m<2> / g, and the interlayer spacing is 0.373mm-0.394mm. The preparation method has the beneficial effects that the raw materials are easily available, and the preparation process is simple and good in repeatability; and the prepared interlayer spacing-amplified microcrystalline graphite material has the characteristics of large interlayer spacing, rich surface functional groups, moderate specific surface area, excellent electrical conductivity, good mechanical strength and the like, is taken as a cathode of a sodium-ion secondary battery and has relatively high coulombic efficiency, excellent rate capability, long-term cycling stability, high tap density and low cost.

Description

technical field [0001] The present invention relates to a modified microcrystalline graphite material, in particular to a microcrystalline graphite material for expanding interlayer spacing, and also to a method for preparing microcrystalline graphite material for expanding interlayer spacing through oxidation intercalation and reduction, and to expanding interlayer spacing microcrystalline The application of graphite as a carbon negative electrode material for sodium ion batteries belongs to the field of secondary batteries. Background technique [0002] Graphite is a carbon material with a good layered structure, high temperature resistance, corrosion resistance, good electrical conductivity, thermal conductivity and stable chemical properties. At the same time, graphite has the advantages of high electronic conductivity, small volume change of layered structure before and after lithium intercalation, high lithium intercalation capacity and low lithium intercalation potent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/205C01B32/215H01M4/587H01M10/054
CPCC01B32/205C01B32/215H01M4/587H01M10/054Y02E60/10
Inventor 张治安尹盟胡均贤谢杨洋
Owner CENT SOUTH UNIV
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