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Surface controllable oxidation graphitization mesophase carbon nanosphere negative electrode material and preparation method

A technology of mesocarbon microspheres and negative electrode materials, applied in battery electrodes, electrochemical generators, electrical components, etc., can solve the problems of reduced degree of graphitization, reduced cycle performance, reduced bulk density, etc., to promote immersion, The effect of increasing lithium storage sites and high platform capacity

Active Publication Date: 2016-02-17
广西卓能新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although oxidation treatment can modify GMCMB, it is prone to excessive oxidation.
Due to excessive oxidation, the spherical structure of mesophase carbon microspheres is destroyed, the bulk density is reduced, the degree of graphitization is reduced, the conductivity is reduced when used as a negative electrode, and the cycle performance is reduced.

Method used

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  • Surface controllable oxidation graphitization mesophase carbon nanosphere negative electrode material and preparation method
  • Surface controllable oxidation graphitization mesophase carbon nanosphere negative electrode material and preparation method
  • Surface controllable oxidation graphitization mesophase carbon nanosphere negative electrode material and preparation method

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Experimental program
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Effect test

Embodiment 1

[0025] Measure 150mLH respectively 2 SO 4 and 180mLHNO 3 Place in a round bottom flask with a volume of 500mL, stir for 5min and mix well. Weigh 8g of graphitized mesocarbon microspheres, add them into the mixed acid, and ultrasonicate for 20min. Then add 3gCrO to the mixture 3 , at 40 oC Stirring for 7h at high temperature. After the reaction was completed, it was cooled to room temperature and filtered to obtain a black solid. Use 5% hydrochloric acid solution to wash five times, then wash repeatedly with distilled water until neutral, and in a vacuum environment, 80 oC drying temperature. The dried black solid was then placed in a quartz tube furnace. Introduce argon as a protective gas, the gas flow rate is 100mL / min, with 10 o C / min heating rate from room temperature to 800 o C, keep warm for 10min, and then rapidly cool down to room temperature, so as to obtain a calcined product. The obtained calcined product is collected and set aside.

[0026] The morpholo...

Embodiment 2

[0035] Measure 130mLH respectively 2 SO 4 and 200mLHNO 3 Place in a round-bottomed flask with a volume of 500mL, and mix well by ultrasonication for 5min. Weigh 8 g of graphitized mesocarbon microspheres, add them into the mixed acid, and stir for 20 min. Then add 5gCrO to the mixture 3 , at 40 oC Stirring for 7h at high temperature. After the reaction was completed, it was cooled to room temperature and filtered to obtain a black solid. Use 5% hydrochloric acid solution to wash five times, then wash repeatedly with distilled water until neutral, and in a vacuum environment, 80 oC drying temperature. The dried black solid was then placed in a quartz tube furnace. Introduce argon as a protective gas, the gas flow rate is 200mL / min, with 10 o C / min heating rate from room temperature to 950 o C, keep warm for 15min, and then rapidly cool down to room temperature to obtain a calcined product. The obtained calcined product is collected and set aside.

Embodiment 3

[0037] Measure 150mLH respectively 2 SO 4 and 100mLH 3 PO 4 Place in a round bottom flask with a volume of 500mL, stir for 10min and mix well. Weigh 5 g of graphitized mesocarbon microspheres, add them into the mixed acid, and ultrasonicate for 20 min. Then add 2gCrO to the mixture 3 , at 60 oC Stirring at temperature for 24h. After the reaction was completed, it was cooled to room temperature and filtered to obtain a black solid. Use 10% hydrochloric acid solution to wash five times, then wash repeatedly with distilled water until neutral, and in a vacuum environment, 80 oC drying temperature. The dried black solid was then placed in a quartz tube furnace. Introduce helium as a protective gas, the gas flow rate is 150mL / min, with 15 o C / min heating rate from room temperature to 1000 o C, keep warm for 10min, and then rapidly cool down to room temperature, so as to obtain a calcined product. The obtained calcined product is collected and set aside.

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Abstract

The present invention discloses a surface controllable oxidation graphitization mesophase carbon nanosphere negative electrode material and a preparation method. The method comprises the following steps: 1) measuring a certain volume of sulfuric acid to mix with one or more than one of nitric acid, perchloric acid and phosphoric acid, and ultrasonically processing or stirring for a certain time; 2) measuring a certain amount of graphitization mesophase carbon nanospheres to add into the mixed acid, ultrasonically processing or mechanically stirring for a certain time; 3) adding a certain amount of chromium trioxide into the liquid mixture, ultrasonically processing or mechanically stirring for oxidation for a certain time, and after completion of the reaction, filtering to obtain a black solid; 4 ) after filtration, using repeatedly washing with a certain concentration of hydrochloric acid and distilled water to clean, and drying; and 5) putting the dried solid into a tube furnace for high temperature heat treatment for some time a certain time in a protective atmosphere and cooling to room temperature. The surface controllable oxidation graphitization mesophase carbon nanosphere has lower lithium-intercalation removal platform and high platform capacity, and has a good degree of graphitization and excellent cycle performance.

Description

technical field [0001] The invention relates to a lithium battery negative electrode material and a preparation method thereof, in particular to a graphitized mesophase carbon microsphere negative electrode material with controlled surface oxidation and a preparation method thereof. Background technique [0002] As an important part of electronic products, lithium-ion batteries play an increasingly important role in people's lives. In recent years, due to the rapid development of electric vehicles and hybrid electric vehicles, people are eager to develop power lithium-ion batteries with high specific capacity and high energy density. The research on anode materials for lithium-ion batteries is crucial to the development of power-type lithium-ion batteries. High-performance anode materials must first meet two basic requirements: (1) have a lower redox potential platform, so that the battery has a higher output voltage; (2) insert and extract as many lithium ions as possible,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/587H01M10/0525C01B31/02
CPCC01P2002/72C01P2004/03H01M4/587H01M10/0525Y02E60/10
Inventor 王红强杨观华李庆余颜志雄黄有国潘齐常
Owner 广西卓能新能源科技有限公司
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