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Preparation method of three-dimensional graphene-based iron vanadate

A technology of alkenyl vanadic acid and graphene, which is applied in the field of materials, can solve the problems of large sheet surface energy, easy folding and agglomeration of graphene sheets, and reduced specific surface area and electrical conductivity, so as to achieve large specific surface area and improve Effects of surface area utilization and electrical conductivity, capacity improvement and lifespan improvement

Inactive Publication Date: 2018-01-12
ANHUI XUANTONG IND DESIGN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method only uses original graphene to coat modified ferric vanadate, and the few layers of graphene have high activity and large surface energy, which makes the exfoliated graphene sheets easy to fold back and agglomerate, resulting in its ratio The surface area and electrical conductivity are greatly reduced, which inevitably affects the electrochemical performance of the material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Add 10g of deionized water to 0.5g of dispersant and mix, then add 5g of graphene oxide, ultrasonically disperse for 2h at a power of 300W and a temperature of 25°C, then add 1.3g of cross-linking agent, at a temperature of 150°C Under the hydrothermal reaction for 9h, a mixed solution was obtained;

[0020] 2) in 0.25L n-amyl alcohol, add 0.1L sodium dodecyl sulfate solution (0.1M, that is, the substance concentration of sodium dodecyl sulfate solution is 0.1M, the same below) to mix, then add metavanadic acid Aqueous ammonium solution (0.1M) and ferrous sulfate solution (0.1M) were 1L each, heated and stirred at 150°C for 3h, rinsed with ethanol 3 times, and the upper suspension was taken;

[0021] 3) Under the temperature condition of 20 ℃, add 6g of dodecyl dimethyl amine oxide to the mixed solution, fully stir until uniform, then add the suspension and mix well, then add 4g each of ammonium bicarbonate and ammonium nitrate, slowly Stir for 1h, freeze-dry for 12...

Embodiment 2

[0025] 1) Add 10g of deionized water to 0.5g of dispersant and mix, then add 5g of graphene oxide, ultrasonically disperse for 2h at a power of 300W and a temperature of 25°C, then add 1.3g of cross-linking agent, at a temperature of 170°C Under the hydrothermal reaction for 8h, a mixed solution was obtained;

[0026] 2) Add 0.1L sodium dodecyl sulfate solution (0.1M) to 0.3L n-amyl alcohol and mix, then add 0.8L ammonium metavanadate aqueous solution (0.1M) and 0.8L ferrous sulfate solution (0.1M) each. 1L, heated and stirred at 140°C for 4h, rinsed twice with ethanol, and took the upper suspension;

[0027] 3) Under the temperature condition of 20 ℃, add 7g of dodecyl dimethyl amine oxide to the mixed solution, fully stir until uniform, then add the suspension and mix well, then add 5g each of ammonium bicarbonate and ammonium nitrate, slowly Stir for 1h, freeze-dry for 13h, take out;

[0028] S4: quickly push the taken out dried material into a hydrogen atmosphere at 260°...

Embodiment 3

[0031] 1) Add 21g of deionized water to 0.7g of dispersant and mix, then add 5g of graphene oxide, ultrasonically disperse for 2h at a power of 300W and a temperature of 25°C, then add 1.4g of cross-linking agent, at a temperature of 170°C Under the hydrothermal reaction for 8h, a mixed solution was obtained;

[0032] 2) Add 0.1L sodium dodecyl sulfate solution (0.1M) to 0.2L n-amyl alcohol and mix, then add 1L ammonium metavanadate aqueous solution (0.1M) and 0.8L ferrous sulfate solution (0.1M), in Heating and stirring at 140°C for 3 hours, rinsed with ethanol for 3 times, and the upper suspension was taken;

[0033] 3) Under the temperature condition of 25 ℃, add 5g of dodecyl dimethyl amine oxide to the mixed solution, fully stir until uniform, then add the suspension and mix well, then add 5g of ammonium bicarbonate and 4g of ammonium nitrate, slowly Stir for 0.5h, freeze-dry for 15h, take out;

[0034] S4: quickly push the taken-out dried material into a hydrogen atmos...

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PUM

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Abstract

The invention relates to the field of battery materials, and particularly discloses a preparation method of three-dimensional graphene-based iron vanadate. The preparation method comprises the following steps: S1, adding a cross-linking agent into a graphene oxide dispersion, and performing a hydrothermal reaction to obtain a mixed solution; S2, adding a sodium lauryl sulfate solution into n-amylalcohol, mixing, and then adding an aqueous ammonium metavanadate solution and a ferrous sulfate solution, heating while stirring, rinsing by using ethanol, and taking an upper suspension; S3, addingdodecyldimethylamine oxide into the mixed solution, sufficiently stirring until a uniform state, then adding the suspension, sufficiently mixing, then adding ammonium hydrogen carbonate and ammonium nitrate, slowly stirring for 0.5-1h, performing freeze drying for 10-20h, and taking out; S4, calcinating a taken dried product at gradient temperatures, and cooling to obtain the three-dimensional graphene-based iron vanadate.

Description

technical field [0001] The invention relates to the technical field of materials, in particular to a preparation method of three-dimensional graphene-based iron vanadate. Background technique [0002] Metal vanadates are a class of excellent functional materials. In addition to being widely used as good host materials in the fields of fluorescence and laser materials, they can also be used as anode materials for lithium-ion batteries. The material has huge application potential. From the analysis of the mechanism of the electrochemical reaction, the iron vanadate electrode material has a high theoretical capacity. However, in the process of charging after the discharge, the iron vanadate is a non-spontaneous reaction. The reversibility of the material is poor, and the capacity decay is severe. These poor reversibility are related to the particle size of the material, the surface morphology and the electrical conductivity of the material. [0003] As a new type of carbon nan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525
CPCY02E60/10
Inventor 王丽李彦
Owner ANHUI XUANTONG IND DESIGN CO LTD