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Preparation method of few-layer MoS2/graphene electrochemical storage lithium composite electrode

A graphene composite and composite electrode technology, which is applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of large organic solvent consumption and long time, and achieve the effect of simple process and high electrochemical lithium storage specific capacity

Active Publication Date: 2012-09-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, so far, few-layer MoS 2 The preparation of lithium ion is mainly based on the method of intercalation and stripping of lithium ions. This method has the following disadvantages: it is highly sensitive to the environment such as air and moisture, it needs to consume a large amount of organic solvent, and it takes a long time.

Method used

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  • Preparation method of few-layer MoS2/graphene electrochemical storage lithium composite electrode
  • Preparation method of few-layer MoS2/graphene electrochemical storage lithium composite electrode

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 1) Ultrasonic disperse 10.76 mmol of graphene oxide in 200 mL of deionized water, add 0.004 mol of octaalkyltrimethylammonium bromide cationic surfactant (concentration: 0.02 M), and stir thoroughly;

[0026] 2) Then add 1.4 g (5.38 mmol) ammonium thiomolybdate into it, stir well, slowly add 20 mL of hydrazine hydrate dropwise under stirring, continue stirring and heat to 95°C, under constant stirring and reflux conditions The reaction time was 7 h, and the ammonium thiomolybdate and graphene oxide were simultaneously reduced to MoS 2 and graphene, the solid product was collected by centrifugation, washed thoroughly with deionization, and then dried under vacuum at 100°C;

[0027] 3) The obtained solid product was heat-treated at 800 °C for 2 h in a nitrogen / hydrogen mixed atmosphere, the volume ratio of hydrogen in the mixed gas was 10%, and a few-layer MoS was prepared after heat treatment 2 Composite nanomaterials with graphene, using XRD and HRTEM to characterize t...

Embodiment 2

[0037] 1) Ultrasonic disperse 5.38 mmol graphene oxide in 200 mL deionized water, add 0.004 mol octaalkyltrimethylammonium bromide cationic surfactant (concentration 0.02 M), and stir thoroughly;

[0038] 2) Then add 1.4 g (5.38 mmol) ammonium thiomolybdate into it, stir well, slowly add 30 mL of hydrazine hydrate dropwise under stirring, continue stirring and heat to 95°C, under constant stirring and reflux conditions The reaction time was 5 h, and the ammonium thiomolybdate and graphene oxide were simultaneously reduced to MoS 2 and graphene, the solid product was collected by centrifugation, washed thoroughly with deionization, and then dried under vacuum at 100°C;

[0039] 3) The obtained solid product was heat-treated at 800 °C for 2 h in a nitrogen / hydrogen mixed atmosphere, and the volume ratio of hydrogen in the mixed gas was 10%, and MoS with few layers was obtained after heat treatment 2 Composite nanomaterials with graphene, using XRD and HRTEM to characterize the ...

Embodiment 3

[0045] 1) Ultrasonic disperse 16.14 mmol of graphene oxide in 200 mL of deionized water, add 0.004 mol of octaalkyltrimethylammonium bromide cationic surfactant (concentration: 0.02 M), and stir thoroughly;

[0046] 2) Then add 1.4 g (5.38 mmol) ammonium thiomolybdate into it, stir well, slowly add 40 mL of hydrazine hydrate dropwise under stirring, continuously stir and heat to 95°C, under constant stirring and reflux conditions The reaction time was 8 h, and the ammonium thiomolybdate and graphene oxide were simultaneously reduced to MoS 2 and graphene, the solid product was collected by centrifugation, washed thoroughly with deionization, and then dried under vacuum at 100°C;

[0047] 3) The obtained solid product was heat-treated at 800 °C for 2 h in a nitrogen / hydrogen mixed atmosphere, and the volume ratio of hydrogen in the mixed gas was 10%, and MoS with few layers was obtained after heat treatment 2 Composite nanomaterials with graphene, using XRD and HRTEM to charac...

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Abstract

The invention relates to a preparation method of a few-layer MoS2 / graphene electrochemical storage lithium composite electrode. The preparation method comprises the following steps of: ultrasonically dispersing graphene oxide in de-ionized water; adding octaalkyl trimethyl ammonium bromide cationic surfactant, then adding ammonium thiomolybdate and dropwise adding hydrazine hydrate with stirring; performing reflow reaction at 95 DEG C to reduce the ammonium thiomolybdate and graphene oxide into MoS2 and graphene at the same time respectively; centrifugally collecting a solid product; washing with de-ionized water; drying; thermally treating in a nitrogen / hydrogen mixed atmosphere to obtain the few-layer (two to four layers) MoS2 / graphene composite nanomaterial; mixing the few-layer MoS2 and graphene composite nanomaterial and acetylene black as well as polyvinylidene fluoride into paste; and coating on a copper foil for rolling. The method provided by the invention has a simple process, and an organic solvent is not consumed. The few-layer MoS2 / graphene composite material is used as the electrochemical storage lithium composite electrode and has high electrochemical storage lithium specific capacity, superior circulation performance and superior high-power charging and discharging characteristic.

Description

technical field [0001] The present invention relates to lithium-ion battery composite electrodes, especially MoS 2 / The preparation method of graphene electrochemical lithium storage composite electrode. Background technique [0002] Lithium-ion batteries have excellent properties such as high specific energy, no memory effect, and environmental friendliness, and have been widely used in portable mobile appliances such as mobile phones and notebook computers. As a power battery, lithium-ion batteries also have broad application prospects in electric bicycles and electric vehicles. At present, graphite materials (such as: graphite microspheres, natural modified graphite and artificial graphite, etc.) are mainly used as negative electrode materials for lithium-ion batteries. These graphite materials have good cycle stability, but their capacity is low. The theoretical capacity of graphite is 372 mAh / g. The new generation of lithium-ion batteries puts forward higher requirem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1393
CPCY02E60/122Y02E60/10
Inventor 陈卫祥王臻黄国创马琳
Owner ZHEJIANG UNIV
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