A low-layer MOS 2 Preparation method of phosphorus-doped graphene electrochemical sodium storage composite electrode

A composite electrode, graphene electrochemical technology, applied in battery electrodes, electrochemical generators, nanotechnology for materials and surface science, etc. Adsorption of graphene oxide, uneven doping and other problems, to achieve the effect of convenient expansion of industrial application, easy to expand industrial application, high electrochemical sodium storage capacity

Active Publication Date: 2017-04-26
LINGNAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the liquid-phase synthesis method, the water solubility of inorganic phosphate is very good, but because the phosphate or hydrogen phosphate itself is negatively charged, it is difficult to adsorb on the graphene oxide with the same load; and the phosphorus in the phosphate - The bond energy of the oxygen bond is relatively large, and it needs to be broken at high temperature, so the doping degree of phosphorus in the phosphorus-doped graphene prepared by using phosphate or hydrogen phosphate as the phosphorus source is not high
Although organic phosphine such as butyl phosphate and triphenylphosphine are not strong in phosphorus-carbon bonds and are easy to break, because organic phosphorus has poor solubility in water and does not have a positive charge, it cannot be combined with negatively charged ones in aqueous solution. Graphene oxide and molybdate produce strong electrostatic interaction, resulting in poor composite material or uneven doping
If the reaction is carried out in an organic solvent, and the solubility of molybdate in an organic solvent is relatively poor, it will not only be difficult to react, but also produce more organic waste and pollute the environment

Method used

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  • A low-layer MOS <sub>2</sub> Preparation method of phosphorus-doped graphene electrochemical sodium storage composite electrode
  • A low-layer MOS <sub>2</sub> Preparation method of phosphorus-doped graphene electrochemical sodium storage composite electrode

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Embodiment 1

[0031] A Few-Layer MoS 2 The preparation method of phosphorus-doped graphene electrochemical sodium storage composite electrode, comprises the steps:

[0032] S1. Ultrasonic disperse 3 mmol graphene oxide in 60 mL deionized water, then add 2 mmol tetrabutylphosphine bromide and stir thoroughly for 12 hours, then add 1.5 mmol sodium molybdate and 5 mmol L-cysteine ​​in sequence , and keep stirring to dissolve it completely;

[0033] S2. Transfer the mixed solution obtained in S1 to a 100 mL hydrothermal reaction kettle, put the reaction kettle in a constant temperature oven, conduct a hydrothermal reaction at 240°C for 24 hours, let it cool down to room temperature naturally, and collect the solid by centrifugation product, and fully washed with deionized water, and dried in vacuum at 80°C; then the solid product obtained above was heat-treated at 800°C for 2 hours in a nitrogen atmosphere to prepare a few-layer MoS 2 / Phosphorus-doped graphene composite nanomaterials;

[00...

Embodiment 2

[0039] A Few-Layer MoS 2 The preparation method of phosphorus-doped graphene electrochemical sodium storage composite electrode, comprises the steps:

[0040] S1. Ultrasonic disperse 3 mmol graphene oxide in 60 mL deionized water, then add 4.5 mmol tetrabutylphosphine bromide and stir thoroughly for 12 hours, then add 1.5 mmol sodium molybdate and 6 mmol thiourea in sequence, and keep stirring Let it dissolve completely.

[0041] S2. Transfer the mixed solution obtained in S1 to a 100 mL hydrothermal reaction kettle, put the reaction kettle in a constant temperature oven, and let it cool down to room temperature naturally after hydrothermal reaction at 220°C for 24 hours, and collect the solid by centrifugation product, and fully washed with deionized water, dried in vacuum at 80°C; then the solid product obtained above was heat-treated at 700°C for 2 hours in a nitrogen atmosphere to prepare a few-layer MoS 2 / Phosphorus-doped graphene composite nanomaterials;

[0042] S3. T...

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Abstract

The invention discloses a preparation method of a less-layer MoS2 / phosphorus-doped graphene electrochemical sodium-storage combined electrode. The method comprises steps as follows: S1, dispersing graphene oxide into water, adding quaternary phosphonium salt, evenly mixing the mixture, then sequentially adding molybdate and a sulfur source, and evenly mixing the mixture; S2, subjecting a mixed disperse system obtained in S1 to a hydrothermal reaction, performing cooling, performing centrifugal collection of a solid product, performing washing and drying, performing heat treatment in the argon or nitrogen atmosphere, and a less-layer MoS2 / phosphorus-doped graphene composite nanomaterial is prepared; S3, taking the composite nanomaterial obtained in S2 as an electrochemical sodium-storage substance to prepare the composite electrode. The graphene oxide, the molybeate and the sulfur source are used as raw materials, and the less-layer MoS2 / phosphorus-doped graphene electrochemical sodium-storage combined electrode is successfully prepared with a hydrothermal method, the heat treatment method and the like assisted by quaternary phosphonium salt. The method has the advantages of simplicity, convenience and easiness of industrial application enlargement.

Description

technical field [0001] The invention belongs to the technical field of new energy materials and energy storage and conversion, and in particular relates to a MoS with few layers 2 The preparation method of phosphorus-doped graphene electrochemical sodium storage composite electrode. Background technique [0002] New energy vehicles are an important development direction of the future automotive industry, and power batteries are one of the core components of new energy vehicles. At present, lithium-ion batteries are the most promising high-energy battery system. However, with the advent of the era of electric vehicles and smart grids, global lithium resources will not be able to effectively meet the huge demand for power lithium-ion batteries, which will further push up the price of lithium-related materials, increase battery costs, and ultimately hinder new energy. industry development. Therefore, it is critical to develop other related energy storage technologies that ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/583H01M4/58H01M4/139H01M10/054B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00H01M4/139H01M4/362H01M4/5815H01M4/583H01M10/054Y02E60/10
Inventor 马琳许丽梅徐旭耀周晓平罗金张玲玲
Owner LINGNAN NORMAL UNIV
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