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A preparation method of graphitized mesocarbon microsphere anode material with controlled surface oxidation

A technology of mesophase carbon microspheres and graphitization, which is used in carbon preparation/purification, battery electrodes, electrochemical generators, etc., can solve the problem of insufficient GMCMB specific capacity, etc., to promote ion transport and increase lithium storage potential. point, the effect of ensuring the bulk density

Active Publication Date: 2017-11-10
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

Nevertheless, in practical application, GMCMB still faces the bottleneck problem that the specific capacity is not high enough

Method used

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  • A preparation method of graphitized mesocarbon microsphere anode material with controlled surface oxidation
  • A preparation method of graphitized mesocarbon microsphere anode material with controlled surface oxidation
  • A preparation method of graphitized mesocarbon microsphere anode material with controlled surface oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Measure 150mL H 2 SO 4 and 180 mL HNO 3 Place in a round bottom flask with a volume of 500 mL, stir for 5 min 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 , stirred at a temperature of 40° C. for 7 h. 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 dry at 80°C in a vacuum environment. 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 The heating rate of C / min was raised from room temperature to 800°C, kept for 10 minutes, and then rapidly cooled to room temperature to obtain a calcined product. The obtained calcined product is collected and set aside.

[0026] The morphology of graphitized int...

Embodiment 2

[0035] Measure 130mL H 2 SO 4 and 200 mL HNO 3 Place in a round bottom flask with a volume of 500 mL, stir for 5 min and mix well. Weigh 8g of graphitized mesocarbon microspheres, add them into the mixed acid, and ultrasonicate for 20min. Then add 5gCrO to the mixture 3 , stirred at a temperature of 40° C. for 7 h. 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 dry at 80°C in a vacuum environment. The dried black solid was then placed in a quartz tube furnace. Argon was introduced as a protective gas, the gas flow rate was 200mL / min, and the temperature was raised from room temperature to 950°C at a rate of 10°C / min, kept for 15 minutes, and then rapidly cooled to room temperature to obtain a calcined product. The obtained calcined product is collected and set aside.

Embodiment 3

[0037] Measure 150mL H 2 SO 4 and 100 mL H 3 PO 4 Place in a round bottom flask with a volume of 500 mL, stir for 10 min and mix well. Weigh 5 g of graphitized mesocarbon microspheres, add them into the mixed acid, and ultrasonicate for 20 min. Then add 2g CrO to the mixture 3 , Stirring at a temperature of 60° C. for 24 h. 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 dry in a vacuum environment at a temperature of 80°C. The dried black solid was then placed in a quartz tube furnace. Helium was introduced as a protective gas, the gas flow rate was 150mL / min, the temperature was raised from room temperature to 1000°C at a heating rate of 15°C / min, kept for 10 minutes, and then rapidly cooled to room temperature 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 preparation method of a lithium battery negative electrode material, in particular to a preparation method of a graphitized mesophase carbon microsphere negative electrode material with surface controllable oxidation. 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, so that the bat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/587H01M10/0525C01B32/05
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