Molybdenum disulfide/graphene composite material and preparation method and application thereof

A technology of molybdenum disulfide and composite materials, applied in secondary batteries, electrochemical generators, electrical components, etc., can solve the problems of molybdenum disulfide composite materials such as complex process, low cycle efficiency, and poor stability, and achieve excellent cycle stability Good reproducibility and repeatability, the effect of inhibiting agglomeration

Inactive Publication Date: 2019-01-22
山西焦煤集团科学技术研究院有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to provide a molybdenum disulfide / graphene composite material and its preparation method and application, which solves the problems of complicated preparation process, poor controllability and poor controllability of the molybdenum disulfide composite material in the prior art and when it is used as a lithium-ion battery negative electrode material. Problems of low cycle efficiency and poor stability

Method used

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  • Molybdenum disulfide/graphene composite material and preparation method and application thereof
  • Molybdenum disulfide/graphene composite material and preparation method and application thereof
  • Molybdenum disulfide/graphene composite material and preparation method and application thereof

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Embodiment 1

[0039] S1. Preparation of ammonium tetrathiomolybdate: Dissolve 5 g of ammonium molybdate tetrahydrate in 30 mL of deionized water, adjust the pH to 11 with ammonia water, add 70 mL of ammonium sulfide solution, stir and reflux at 80°C for 2.5 h, cool to room temperature , standing for crystallization for 42h, the crystallization was filtered, washed with absolute ethanol, and dried at room temperature for 24h to obtain ammonium tetrathiomolybdate crystals.

[0040] S2. Preparation of graphene slurry by electrochemical method: using graphite rod as working electrode, N-butylpyridinium tetrafluoroborate and 1-hexyl-3-methylimidazolium hexafluorophosphate at a volume ratio of 1:1 The mixture was used as an electrolyte, electrolyzed at a voltage of 8.5V for 18h, and then subjected to solid-liquid separation, ultrasonic dispersion, and washing to obtain a graphene slurry with a mass concentration of 1.5%.

[0041]S3. Graphene surface modification: Accurately weigh 3.644g (0.01mol)...

Embodiment 2

[0047] S1. Preparation of ammonium tetrathiomolybdate: Dissolve 5 g of ammonium molybdate tetrahydrate in 30 mL of deionized water, adjust the pH to 12 with ammonia water, add 90 mL of ammonium sulfide solution, stir and reflux at 90°C for 1.5 h, cool to room temperature , standing for crystallization for 36h, the crystallization was filtered, washed with absolute ethanol, and dried at room temperature for 24h to obtain ammonium tetrathiomolybdate crystals.

[0048] S2. Preparation of graphene slurry by electrochemical method: using graphite rod as working electrode, N-butylpyridinium tetrafluoroborate and 1-octyl-3-methylimidazolium bromide with a volume ratio of 1:1:1 The mixture of salt and 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the electrolyte, electrolyzed at a voltage of 7V for 24h, and then subjected to solid-liquid separation, ultrasonic dispersion, and washing, and finally obtained graphene with a mass concentration of 2.0%. slurry.

[0049] S3. ...

Embodiment 3

[0053] S1. Preparation of ammonium tetrathiomolybdate: Dissolve 5 g of ammonium molybdate tetrahydrate in 30 mL of deionized water, adjust the pH to 9.5 with ammonia water, add 85 mL of ammonium sulfide solution, stir and reflux at 85°C for 2 h, cool to room temperature, Stand for crystallization for 30 hours, filter the crystals, wash with absolute ethanol, and dry at room temperature for 24 hours to obtain ammonium tetrathiomolybdate crystals.

[0054] S2. Preparation of graphene slurry by electrochemical method: using graphite rod as working electrode, N-butylpyridine tetrafluoroborate and 1-octyl-3-methylimidazolium bromide with a volume ratio of 1:1 The mixture was used as an electrolyte, electrolyzed at a voltage of 6V for 36h, and then subjected to solid-liquid separation, ultrasonic dispersion, and washing to obtain a graphene slurry with a mass concentration of 2.5%.

[0055] S3. Graphene surface modification: Accurately weigh 3.644g (0.01mol) of hexadecyltrimethylamm...

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Abstract

The invention discloses a molybdenum disulfide/graphene composite material and a preparation method and application thereof, belonging to the field of electrochemistry and new energy material. The preparation method of the invention comprises the following steps: (1) preparing ammonium tetrathiomolybdate; (2) preparation of graphene slurry by electrochemical method; (3) surface modification of graphene; (4) Preparation of molybdenum disulfide/graphene composites. The process of the invention is simple and easy to operate, the condition is mild, the repeatability is high, the yield is high, andthe invention is suitable for batch production. The conductivity of MoS 2 was improved and the aggregation of MoS 2 and graphene was inhibited by the composites. When the composites were used as cathode materials for lithium ion batteries, they showed high specific capacity and excellent cycle stability. The first discharge specific capacity reaches 700-1200 mAh/g at 0.01- 3.0 V and 200 mA/g current density, and the discharge specific capacity maintains at 550 -850 mAh/g after 200 cycles. The results show that the first discharge specific capacity reaches 700-1200 mAh/g at 200 mA/g current density.

Description

technical field [0001] The invention relates to a molybdenum disulfide / graphene composite material and a preparation method and application thereof, belonging to the technical field of new energy battery materials. Background technique [0002] Due to the prominent energy and environmental crisis issues, the chemical energy storage technology of safe, efficient and environment-friendly secondary battery system has received extensive attention and research and development investment. Among them, lithium-ion battery is the most competitive green energy in the secondary battery system. Lithium-ion batteries have the advantages of high energy density, stable working voltage, good safety performance, long cycle life, and no memory effect. They are widely used in transportation, home appliances, office, mobile communications and other fields. However, the low specific capacity (372 mA h / g) of conventional graphite anode greatly limits the application of lithium-ion batteries. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525
CPCH01M4/362H01M4/5815H01M4/62H01M4/625H01M4/628H01M10/0525Y02E60/10
Inventor 霍晓东刘小宇鱼殊鲲邢欢李婕卫欣
Owner 山西焦煤集团科学技术研究院有限公司
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