Preparation method of molybdenum carbide/nitrogen-sulfur codoped spongy graphene cathode composite for sodium-ion battery

A nitrogen-sulfur co-doped, sodium-ion battery technology, applied in battery electrodes, secondary batteries, electrochemical generators, etc., can solve the problems of fast capacity decay and poor rate performance, and achieve low cost, guaranteed specific capacity, Environmentally friendly effect

Active Publication Date: 2016-05-18
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] In the past period of time, researchers have carried out extensive research on electrode materials for sodium-ion batteries. Among them, carbon materials, alloy materials, sulfides, oxides and ot

Method used

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  • Preparation method of molybdenum carbide/nitrogen-sulfur codoped spongy graphene cathode composite for sodium-ion battery
  • Preparation method of molybdenum carbide/nitrogen-sulfur codoped spongy graphene cathode composite for sodium-ion battery
  • Preparation method of molybdenum carbide/nitrogen-sulfur codoped spongy graphene cathode composite for sodium-ion battery

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Experimental program
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Effect test

Embodiment 1

[0041]First take by weighing 3g of flaky graphite with a purity of 99.5%, join in the mixed solution containing 350mL mass fraction of concentrated sulfuric acid of 98% and 50mL of mass fraction of phosphoric acid of 85%, add 18g of potassium permanganate in batches for oxidation, and The mixed solution was kept at 0°C under ice bath and stirred for 2h, then heated to 45°C in a water bath and reacted under magnetic stirring for 12h to obtain a mixed solution; then, 400mL of deionized water was slowly added to the mixture under ice bath After the reaction is stable, slowly add 20mL of hydrogen peroxide to remove unreacted potassium permanganate, and then the color of the mixed solution turns bright yellow; finally, the resulting mixed solution is repeatedly washed with a large amount of deionized water, centrifuged and put into a dialysis bag for dialysis A pure graphene oxide solution can be obtained in 5-7 days. The concentration of graphene oxide in the prepared graphene oxi...

Embodiment 2

[0051] Measure 10 mL of the above graphene oxide solution (the graphene oxide content is 10×5 mg / mL=50 mg) with a measuring cylinder, pour it into a 150 mL beaker and stir it magnetically at room temperature. Then take thiourea 0.3g according to the nitrogen source sulfur source and graphene oxide mass ratio 6:1, add in the graphene oxide solution being stirred, continue stirring for 1h after the thiourea and graphene oxide solution are fully mixed to obtain the Nitrogen-sulfur graphene oxide solution.

[0052] According to the molybdenum source and carbon source mass ratio of 4:1, respectively weigh 1.0 g of ammonium paramolybdate and 0.25 g of glucose, and add them to 40 mL of deionized water successively, and slowly add the mixed solution to the above-mentioned nitrogen-containing solution under magnetic stirring conditions. In the graphene oxysulfide solution, after fully stirring and dispersing for 1 h, the mixed solution was adjusted to a pH of 10 with tris(hydroxymethyl...

Embodiment 3

[0056] Measure 10 mL of the above graphene oxide solution (the graphene oxide content is 10×5 mg / mL=50 mg) with a measuring cylinder, pour it into a 150 mL beaker and stir it magnetically at room temperature. Then take thiourea 0.4g according to the nitrogen source sulfur source and graphene oxide mass ratio 8:1, add in the graphene oxide solution being stirred, continue to stir for 1h after the thiourea and graphene oxide solution are fully mixed to obtain the Nitrogen-sulfur graphene oxide solution.

[0057] According to the molybdenum source and carbon source mass ratio of 2:1, respectively weigh 1.0 g of ammonium paramolybdate and 0.5 g of glucose, and add them to 40 mL of deionized water successively, and slowly add the mixed solution to the above-mentioned nitrogen-containing solution under magnetic stirring conditions. In the graphene oxysulfide solution, after fully stirring and dispersing for 1 h, the mixed solution was adjusted to a pH of 10 with tris(hydroxymethyl)a...

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Abstract

The invention discloses a preparation method of a molybdenum carbide/nitrogen-sulfur codoped spongy graphene cathode composite for a sodium-ion battery. According to the molybdenum carbide/nitrogen-sulfur codoped spongy graphene cathode composite prepared through the preparation method, molybdenum carbide particles are uniformly distributed in carbide/nitrogen-sulfur codoped spongy graphene which has a great number of surface folds, has a great number of active sites and is of a three-dimensional structure. The preparation method comprises the steps of dissolving a molybdenum source and a carbon source into a graphene oxide solution, adding a nitrogen source and a sulfur source, adjusting ph value, then conducting a hydrothermal reaction on an obtained mixed solution, conducting freeze-drying on a product, then putting the product in a quartz crucible for high temperature heat treatment, and conducting natural cooling after a reaction is ended, so that the composite is obtained. In the hydrothermal reaction process, graphene doping and reduction, formation of a precursor and composition of the precursor and doped graphene are conducted synchronously. The composite can be obtained by combining the hydrothermal method with the subsequent heat treatment process, and the preparation method is simple in process and low in cost and has good research prospect.

Description

technical field [0001] The invention relates to a preparation method of a negative electrode material of a sodium ion battery, belonging to the field of sodium ion batteries. Background technique [0002] With the rapid changes in the information age, lithium-ion batteries have achieved rapid development in portable electronic products (notebook computers, smart mobile devices, tablet computers, etc.) and electric vehicles, and have shown good development prospects. However, its development is inevitably challenged due to limiting factors such as the scarcity of metallic lithium resources, the cost of battery manufacturing, and the capacity of mature lithium-ion batteries. Sodium, which is in the same main group as lithium in the periodic table, has similar physical and chemical properties to lithium, and has abundant reserves compared with lithium. This makes Na-ion batteries one of the most promising battery systems for large-scale commercial applications. However, becau...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/587H01M10/054
CPCH01M4/362H01M4/587H01M10/054Y02E60/10
Inventor 张治安宋俊肖史晓东赵星星吕晓军赖延清李劼张凯
Owner CENT SOUTH UNIV
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