Preparation method of nitrogen-sulfur co-doped three-dimensional graphene, prepared product and product application thereof

A nitrogen-sulfur co-doping, graphene technology, applied in nanotechnology for materials and surface science, electrical components, electrochemical generators, etc., can solve the problems of harsh experimental conditions, difficult to achieve large-scale preparation, and high cost , to achieve the effect of simple operation, low cost and large specific surface area

Inactive Publication Date: 2018-08-31
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, methods such as CVD and epitaxial growth have high costs and harsh e

Method used

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  • Preparation method of nitrogen-sulfur co-doped three-dimensional graphene, prepared product and product application thereof
  • Preparation method of nitrogen-sulfur co-doped three-dimensional graphene, prepared product and product application thereof
  • Preparation method of nitrogen-sulfur co-doped three-dimensional graphene, prepared product and product application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of precursor by hydrothermal reaction: First, 100 mg of graphene oxide was dispersed in 10 ml of deionized water to obtain a graphene oxide dispersion, then 0.03 g of melamine was added, stirred at 80°C until completely dissolved, and A liquid was obtained; another 0.04 1 g of thiocyanuric acid was dissolved in 25ml of ethanol to obtain liquid B; slowly add liquid B to liquid A, stir at 70°C for 10 minutes and then put it into a hydrothermal kettle with a filling ratio of 35% and a hydrothermal reaction temperature of 120°C / 4h. After the hydrothermal reaction is completed, freeze-dry to obtain the precursor.

[0023] (2) Preparation of three-dimensional doped graphene by heat treatment: the precursor was placed in a tube furnace, protected by argon, and heated to 600°C at a heating rate of 2°C / min for 5 hours.

Embodiment 2

[0025] (1) Preparation of precursor by hydrothermal reaction: First, disperse 100 mg of graphene oxide in 25 ml of deionized water to obtain a graphene oxide dispersion, then add 0.13 g of melamine, stir at 80°C until completely dissolved, and obtain liquid A; another 0.18 1 g of thiocyanuric acid was dissolved in 25ml of ethanol to obtain liquid B; slowly add liquid B to liquid A, stir at 80°C for 60 minutes, then put it into a hydrothermal kettle, the filling ratio is 50%, and the hydrothermal reaction is 200°C / 12h. After the hydrothermal reaction is completed, freeze-dry to obtain the precursor.

[0026] (2) Preparation of three-dimensional doped graphene by heat treatment: the precursor was placed in a tube furnace, protected by argon, and heated to 700 °C at a heating rate of 5 °C / min for 2 h.

[0027] refer to figure 1 , figure 1 SEM photographs of samples prepared for this example. Using the S-4800 scanning electron microscope (SEM) of Japan Electronics Co., Ltd. t...

Embodiment 3

[0031] (1) Preparation of precursor by hydrothermal reaction: First, disperse 100 mg of graphene oxide in 20 ml of deionized water to obtain a graphene oxide dispersion, then add 0.252 g of melamine, stir at 120 °C until completely dissolved, and obtain liquid A; another 0.354 Dissolve thiocyanic acid in 25ml of ethanol to obtain liquid B; slowly add liquid B to liquid A, stir at 120°C for 10 minutes, then put it into a hydrothermal kettle, the filling ratio is 55%, and the hydrothermal reaction is 150°C / 36h . After the hydrothermal reaction is completed, freeze-dry to obtain the precursor.

[0032] (2) Preparation of three-dimensional doped graphene by heat treatment: the precursor was placed in a tube furnace, protected by argon, and heated to 1000 °C at a heating rate of 10 °C / min for 1 h.

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Abstract

The invention provides a preparation method of nitrogen-sulfur co-doped three-dimensional graphene. Graphene oxide is dispersed in deionized water to obtain graphene oxide dispersion liquid, and melamine powder and an ethanol solution of trithiocyanuric acid are added, uniformly dispersed and then placed into a hydrothermal reactor for hydrothermal reaction; hydrothermal products are dried, and finally heat treatment is conducted. The invention further provides the nitrogen-sulfur co-doped three-dimensional graphene and application of the graphene as an electrode material. The prepared producthas nitrogen element content of 3-10% and sulfur element content of 0.5-3%. The preparation method has the advantages that an experimental method is safe, non-toxic, low in cost and simple to operate. A hydrothermal method is adopted to achieve doping, three-dimensional construction and graphene oxide reduction. The prepared three-dimensional graphene has a large specific surface area and can beapplied in the fields of lithium ion batteries, supercapacitors, electrocatalysis and the like.

Description

technical field [0001] The invention relates to the field of carbon nanomaterials, in particular to a preparation method of nitrogen-sulfur co-doped three-dimensional graphene, a product prepared by the same and an application of the product. Background technique [0002] Graphene is a two-dimensional crystal with a single atomic layer thickness composed of carbon atoms. It is known as a material with a perfect structure. It is considered to be a high-storage lithium material because of its large specific surface area, high electrical conductivity, and high strength. . However, experiments and theory have proved that pure graphene has insufficient active sites, is not selective, and does not have a good match for practical applications. Studies have shown (Electrochimica Acta, 2016, 205:188-197.) Heteroatom doping can effectively solve the application problems of graphene, introducing defects to provide active sites. Heteroatom doping methods include CVD, epitaxial growth,...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/587H01M4/62H01M10/0525B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00H01M4/364H01M4/587H01M4/628H01M10/0525Y02E60/10
Inventor 黄剑锋席乔李嘉胤曹丽云程娅伊齐慧郭玲党欢
Owner SHAANXI UNIV OF SCI & TECH
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