A preparation method of a nitrogen-sulfur co-doped three-dimensional graphene foam electrode active material

A graphene foam, nitrogen-sulfur co-doping technology, applied in graphene, battery electrodes, circuits, etc., to achieve the effects of simple operation, low cost, and broad application prospects

Active Publication Date: 2018-12-18
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although two-dimensional doped graphene can significantly increase the specific capacity of the material as an electrode material, there is still a lot of room for improvement in terms of kinetics.

Method used

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  • A preparation method of a nitrogen-sulfur co-doped three-dimensional graphene foam electrode active material
  • A preparation method of a nitrogen-sulfur co-doped three-dimensional graphene foam electrode active material
  • A preparation method of a nitrogen-sulfur co-doped three-dimensional graphene foam electrode active material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) First, disperse 50mg of graphene oxide in a mixed solvent of 70ml of deionized water and 10ml of ethanol to obtain a graphene oxide dispersion. After ultrasonic stripping of graphene oxide, add 0.03g of melamine and 0.04g of thiocyanate in sequence , Stir at 80°C until completely dissolved.

[0022] (2) Immerse 30*60*0.5mm nickel foam into the liquid of (1), and then put it into a 100ml polytetrafluoroethylene reactor for hydrothermal reaction. The hydrothermal reaction time is 4 hours, and the hydrothermal temperature is 100°C.

[0023] (3) After freeze-drying, the hydrothermal product was placed in a tube furnace, and the temperature was raised to 500°C at a rate of 2°C / min for 5 hours under an atmosphere protected by argon.

[0024] (4) Immerse the product in 5% dilute hydrochloric acid, stir magnetically at 80°C for 12 hours, and etch off the nickel foam. Then centrifuged and washed 6 times, dried to obtain the sample.

Embodiment 2

[0026] (1) First, disperse 100mg of graphene oxide in a mixed solvent of 25ml of deionized water and 25ml of ethanol to obtain a graphene oxide dispersion, then add 0.03g of melamine and 0.04g of thiocyanate in turn, and stir at 80°C until completely dissolve.

[0027] (2) Immerse 30*60*1mm nickel foam into the liquid of (1), and then put it into a 100ml polytetrafluoroethylene reactor for hydrothermal reaction. The hydrothermal reaction time is 24 hours, and the hydrothermal temperature is 150°C.

[0028] (3) After freeze-drying, the hydrothermal product was placed in a tube furnace, and the temperature was raised to 600°C at a rate of 5°C / min for 2 hours under an argon-protected atmosphere.

[0029] (4) Immerse the product in 5% dilute hydrochloric acid, stir magnetically at 80°C for 12 hours, and etch off the nickel foam. Then centrifuged and washed 6 times, dried to obtain the sample.

Embodiment 3

[0031] (1) First, disperse 100mg of graphene oxide in a mixed solvent of 50ml of deionized water and 10ml of ethanol to obtain a graphene oxide dispersion, then add 0.12g of melamine and 0.17g of thiocyanate in sequence, and stir at 80°C until completely dissolve.

[0032] (2) Immerse 30*60*2mm nickel foam into the liquid of (1), and then put it into a 100ml polytetrafluoroethylene reactor for hydrothermal reaction. The hydrothermal reaction time is 36 hours, and the hydrothermal temperature is 200°C.

[0033] (3) After freeze-drying, the hydrothermal product was placed in a tube furnace, and the temperature was raised to 800°C at a rate of 10°C / min under an argon-protected atmosphere for 1 hour.

[0034] (4) Immerse the product in 5% dilute hydrochloric acid, stir magnetically at 80°C for 12 hours, and etch off the nickel foam. Then centrifuged and washed 6 times, dried to obtain the sample.

[0035] Refer to attached Figure 1~3 , figure 1 Low magnification scanning ele...

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Abstract

The invention discloses a preparation method of a nitrogen-sulfur co-doped three-dimensional graphene foam electrode material, comprising the following steps: soaking foamed nickel in a dispersion liquid comprising graphene oxide, melamine, melamine thiocyanate and sufficient solvent; carrying out a solvothermal reaction; performing heat treatment on a solvothermal reaction product at 500 to 1200DEG C in inert atmosphere; and preparing nitrogen-sulfur co-doped three-dimensional graphene foam by strong acid etching of nickel foam in the heat-treated product. The nitrogen-sulfur co-doped three-dimensional graphene foam electrode material prepared by the method has three-dimensional doped graphene foam and doped nitrogen and sulfur elements. The content of nitrogen element, sulfur element and oxygen element is 3 - 7%, 1 - 3% and 4 - 12%, respectively. The doping amount is controllable. The experimental method is safe, non-toxic, low cost and easy to operate. The three-dimensional doped graphene foam electrode can be used in the fields of lithium ion batteries, supercapacitors and electrocatalysis, and has broad application prospects.

Description

technical field [0001] The invention relates to the technical field of graphene electrode materials, in particular to a preparation method of a nitrogen-sulfur co-doped three-dimensional graphene foam electrode material. Background technique [0002] As we all know, graphene is a two-dimensional crystal with a perfect structure of one atomic layer thickness composed of carbon atoms. However, graphene's lack of inherent band gap and its easy restacking in experiments limit its practical application in various fields. Studies have shown that heteroatom doping can effectively open the band gap of graphene, resulting in significantly improved physical, chemical and electrical properties. In addition, three-dimensional regulation of the graphene structure can solve the problem of its easy stacking. Common methods of doping graphene include CVD, ball milling, plasma, arc discharge, wet chemical and heat treatment. In contrast, the wet chemical method has been widely used due to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/583H01M4/62H01M10/0525H01M10/054C01B32/182
CPCH01M4/583H01M4/625H01M10/0525H01M10/054C01B32/182Y02E60/10
Inventor 李嘉胤席乔黄剑锋曹丽云何元元王彩薇罗晓敏郭鹏辉
Owner SHAANXI UNIV OF SCI & TECH
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