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Iron diselenide/sulfur-doped graphene anode composite material for sodium-ion battery and preparation method of iron diselenide/sulfur-doped graphene anode composite material

A sulfur-doped graphene and sodium-ion battery technology, applied in battery electrodes, secondary batteries, electrochemical generators, etc., to achieve good dispersion, good stability, and high degree of dispersion

Active Publication Date: 2016-03-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, researchers have not found a method that can effectively slow down the rapid capacity loss of iron diselenide due to volume expansion during the sodium ion deintercalation process.

Method used

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  • Iron diselenide/sulfur-doped graphene anode composite material for sodium-ion battery and preparation method of iron diselenide/sulfur-doped graphene anode composite material
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  • Iron diselenide/sulfur-doped graphene anode composite material for sodium-ion battery and preparation method of iron diselenide/sulfur-doped graphene anode composite material

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Experimental program
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Effect test

Embodiment 1

[0046] 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 ox...

Embodiment 2

[0055] Measure 56ml of the above-mentioned graphene oxide solution (graphene oxide content is 56×7.5mg / ml=420mg=0.42g) with a graduated cylinder, pour it into a 500ml beaker and stir it magnetically at room temperature. Then weigh 0.42 g of thioacetamide according to the mass ratio of sulfur source and graphene oxide 1:1, add in batches to the graphene oxide solution being stirred, and continue stirring after the thioacetamide and graphene oxide solution are fully mixed After 15 hours, a sulfur-containing graphene oxide solution can be obtained.

[0056] According to the molar ratio of selenium source and iron source is 2:1, and the molar ratio of iron source and citric acid (CA) is 1:5, respectively weigh ferrous ammonium sulfate hexahydrate 2.352g, selenium dioxide 1.332g, citric acid (CA) ) 6g, and successively added to 100ml deionized water, after ultrasonic 0.5h dispersed evenly, slowly added the mixed solution into the above-mentioned sulfur-containing graphene oxide sol...

Embodiment 3

[0059] Measure 56ml of the above-mentioned graphene oxide solution (graphene oxide content is 56×7.5mg / ml=420mg=0.42g) with a graduated cylinder, pour it into a 500ml beaker and stir it magnetically at room temperature. Then weigh 0.42 g of thioacetamide according to the mass ratio of sulfur source and graphene oxide 1:1, add in batches to the graphene oxide solution being stirred, and continue stirring after the thioacetamide and graphene oxide solution are fully mixed After 15 hours, a sulfur-containing graphene oxide solution can be obtained.

[0060] According to the molar ratio of selenium source and iron source is 2:1, and the molar ratio of iron source and citric acid (CA) is 1:15, respectively weigh ferrous ammonium sulfate hexahydrate 2.352g, selenium dioxide 1.332g, citric acid (CA) ) 18g, and successively added to 100ml deionized water, after ultrasonic 0.5h dispersed uniformly, slowly added the mixed solution into the above-mentioned sulfur-containing graphene oxid...

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Abstract

The invention discloses an iron diselenide / sulfur-doped graphene anode composite material for a sodium-ion battery and a preparation method of the iron diselenide / sulfur-doped graphene anode composite material. The preparation method comprises the following steps: dissolving a sulfur source, a selenium-containing inorganic matter, an iron-containing inorganic salt and citric acid or sodium citrate into a graphene oxide solution; dropwise adding hydrazine hydrate to form a light black solution, adding the light black solution to a hydrothermal reaction kettle for reaction, and naturally cooling the product after the reaction is ended; and carrying out repeated washing, suction filtration and drying on a reaction sediment with distilled water and absolute ethyl alcohol, so as to obtain the iron diselenide / sulfur-doped graphene composite material. According to the iron diselenide / sulfur-doped graphene composite material prepared by the method, iron diselenide nano-particles are evenly distributed on the surface of the sulfur-doped graphene and the iron diselenide / sulfur-doped graphene composite material has excellent electrochemical properties as a sodium-ion battery anode material. The iron diselenide / sulfur-doped graphene anode composite material is prepared by a simple hydrothermal process; synchronous sulfur doping, graphene oxide reduction and graphene oxide and iron diselenide recombination can be achieved; and the iron diselenide / sulfur-doped graphene anode composite material is simple in preparation technology and low in cost, and has a wide industrial application prospect.

Description

technical field [0001] The invention relates to a negative electrode material of a sodium ion battery and a preparation method thereof, belonging to the field of sodium ion batteries. Background technique [0002] As a socially dominant electrochemical energy storage device, lithium-ion batteries have achieved good results in portable electronics (laptops, smart mobile devices, tablets, etc.), electric vehicles, and plug-in hybrid electric vehicles. Application prospects. However, due to the lack of metal lithium resources and the high cost of lithium-ion batteries and other limiting factors, the large-scale commercial application of lithium-ion batteries is facing severe challenges. This means that it is imperative to research and develop a battery system that can be commercialized on a large scale and applied industrially. Metal sodium and lithium are in the same main group in the periodic table of elements, and it has similar physical and chemical properties to metal li...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/38H01M4/58H01M4/62H01M10/054
CPCH01M4/364H01M4/38H01M4/581H01M4/625H01M4/628H01M10/054Y02E60/10
Inventor 张治安史晓东
Owner CENT SOUTH UNIV
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