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Preparation method of iron-doped cobalt diselenide nanosheet/reduced graphene composite electrode material

A technology of graphene composite and cobalt diselenide, which is applied in battery electrodes, nanotechnology, secondary batteries, etc., can solve the problems of large volume expansion effect, long battery activation cycle, and poor cycle stability, so as to improve conductivity, Effect of reduced electrochemical activation time and good rate performance

Inactive Publication Date: 2020-03-06
ZHONGYUAN ENGINEERING COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention proposes an iron-doped cobalt diselenide for the problems or improvement needs of a single cobalt diselenide sodium battery electrode material in the charging and discharging process, such as large volume expansion effect, long battery activation cycle, and complicated preparation process. A method for preparing a nanosheet / reduced graphene composite electrode material. The composite material is prepared by a one-step method, which can avoid the agglomeration of nanoparticles caused by high-temperature sintering treatment, etc., and improve the composite uniformity of iron-doped cobalt diselenide and graphene. degree, and then improve the problems of long activation cycle, poor cycle stability and poor rate performance when cobalt diselenide is used as the anode material of sodium ion battery

Method used

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  • Preparation method of iron-doped cobalt diselenide nanosheet/reduced graphene composite electrode material
  • Preparation method of iron-doped cobalt diselenide nanosheet/reduced graphene composite electrode material
  • Preparation method of iron-doped cobalt diselenide nanosheet/reduced graphene composite electrode material

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Embodiment 1

[0029] A preparation method of iron-doped cobalt diselenide nanosheet / reduced graphene composite electrode material, the steps are as follows:

[0030] Weigh 0.291 g of cobalt nitrate hexahydrate and ferric nitrate of different masses (0, 0.007, 0.0103, 0.014, 0.0175 g) and dissolve them in a mixed solvent of 14 mL of water and 26 mL of ethylenediamine, and stir until dissolved; weigh 0.158 g Selenium powder (the mass ratio of mixed dispersion liquid and selenium salt is 155:1) was stirred and dispersed for 2 h at 25 ° C under the control of the stirring speed of 200 r / min. o The reaction was performed at C for 16 h. After the reaction, the product was centrifuged and washed with a mixed solvent of water and ethanol, and then the sample was dried in a blast drying oven for 60 o C was dried overnight to obtain the final product.

[0031] like figure 2 As shown in the figure, it can be seen from the figure that all the diffraction peaks are consistent with the standard patter...

Embodiment 2

[0035] A preparation method of iron-doped cobalt diselenide nanosheet / reduced graphene composite electrode material, the steps are as follows:

[0036] 0.05 g of graphene oxide was weighed and dissolved in a mixed solvent of 14 mL of water and 26 mL of ethylenediamine, and ultrasonically dispersed for 2 hours, then 0.268 g of cobalt nitrate hexahydrate and 0.032 g of ferric nitrate nonahydrate were added to the above solution, and stirred until Dissolve, the stirring speed is 100 rpm, the dispersion temperature is 50 °C, and the dispersion time is 0.1 h; 0.158 g of selenium powder (the ratio of dispersion liquid and selenium salt is 155:1) is weighed, and the stirring speed is controlled at 25 °C Stir and disperse at 200 r / min for 2 h, put the above solution in a reaction kettle, and react at 180 °C for 16 h. After the reaction, the product is centrifuged and washed with a mixed solvent of water and ethanol, and then the sample is dried in a blast drying oven for 60 Dry at °C ...

Embodiment 3

[0039] A preparation method of iron-doped cobalt diselenide nanosheet / reduced graphene composite electrode material, the steps are as follows:

[0040] 0.05 g of graphene oxide was weighed and dissolved in a mixed solvent of 14 mL of water and 26 mL of diethylenetriamine, and ultrasonically dispersed for 2 hours, then 0.312 g of cobalt acetate tetrahydrate and 0.003 g of ferric acetate were added to the above solution, and stirred. To dissolve, the stirring speed is 200 rpm, the dispersion temperature is 30 °C, and the dispersion time is 3 h; 0.667 g of selenium powder (the ratio of dispersion liquid and selenium salt is 60:1) is weighed, and the stirring speed is controlled at 50 °C. Stir and disperse at 500 r / min for 5 h, place the above solution in a reaction kettle, and react at 200 °C for 24 h. After the reaction, the product is centrifuged and washed with a mixed solvent of water and ethanol, and then the sample is dried in a blast drying oven for 60 Dry at °C overnight ...

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Abstract

The invention provides a preparation method of an iron-doped cobalt diselenide nanosheet / reduced graphene composite electrode material. The preparation method comprises the following steps: (1) dispersing graphene oxide in a mixed solvent and carrying out ultrasonic dispersion to obtain a graphene oxide dispersion liquid; (2) adding cobalt salt and ferric salt into the graphene oxide dispersion liquid in the step (1) and stirring and dispersing to obtain a mixed dispersion liquid; and (3) adding selenium salt into the mixed dispersion liquid obtained in the step (2), stirring, soaking, heating, reacting, centrifuging, washing and drying to obtain the composite electrode material. The simple method is adopted, the iron-doped cobalt diselenide nanosheet and the composite material of the iron-doped cobalt diselenide nanosheet and graphene are prepared by taking low-cost transition metal salt as a precursor and adopting a one-step solvothermal method through optimization of the structure and composition of the material, and the material has the advantages of high specific capacity, good rate capability, long cycle life and the like as the negative electrode material of the sodium ion battery.

Description

technical field [0001] The invention relates to the field of electrode materials for sodium ion batteries, in particular to a preparation method of an iron-doped cobalt diselenide nanosheet / reduced graphene composite electrode material. Background technique [0002] Compared with lithium-ion batteries, sodium-ion batteries have the advantage of abundant sodium resources and are expected to be used in the field of large-scale energy storage. Therefore, the preparation of high-performance Na-ion battery electrode materials by a simple method has attracted much attention. Transition metal oxygen (sulfur) compounds have the advantages of abundant raw material sources and low cost, and are widely used in the field of anode materials for sodium-ion batteries. Compared with transition metal oxygen (sulfur) compounds, transition metal selenides have better electrical conductivity, larger lattice spacing, and easier de-intercalation / insertion behavior of sodium ions. They are potent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054B82Y40/00
CPCB82Y40/00H01M4/366H01M4/581H01M4/62H01M4/625H01M4/628H01M10/054Y02E60/10
Inventor 王艳杰米立伟郭帅立孙浩洋陈孔耀何诚宗耀
Owner ZHONGYUAN ENGINEERING COLLEGE
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