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Method for preparing nitrogen-doped graphene aerogel by simultaneously using SiO2-NH2 as template and nitrogen doping agent

A graphene airgel and graphene technology, applied in the direction of graphene, nano-carbon, hybrid capacitor electrodes, etc., can solve the problems of limiting the performance of graphene, and achieve the effects of easy promotion, strong practicability, and high adsorption efficiency

Active Publication Date: 2017-10-20
山东济清科技服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, non-conductive perfluorinated moieties may limit the performance of graphene in energy storage applications
Therefore, it remains a challenge to design and prepare porous 3D graphene materials with highly usable surface area and without complex fabrication processes by suppressing graphene sheet restacking.

Method used

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  • Method for preparing nitrogen-doped graphene aerogel by simultaneously using SiO2-NH2 as template and nitrogen doping agent
  • Method for preparing nitrogen-doped graphene aerogel by simultaneously using SiO2-NH2 as template and nitrogen doping agent
  • Method for preparing nitrogen-doped graphene aerogel by simultaneously using SiO2-NH2 as template and nitrogen doping agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1 Experimental part

[0044] 1.1 Materials

[0045] Natural graphite flakes (8000 mesh, 99.95% purity), tetraethylsilicate (TEOS) and (3-aminopropyl)triethoxysilane (APTES) were purchased from Aladdin. Concentrated sulfuric acid (95-98%), concentrated hydrochloric acid (36-38%), hydrofluoric acid (40%) and potassium permanganate of analytical grade were purchased from Beijing Chemical Plant (China). Hydrogen peroxide (H 2 o 2 ) and sodium nitrate were provided by Laiyang Shikang Chemical Company. The above-mentioned concentrations are all mass concentrations.

[0046] 1.2 Amino-functionalized silica particles

[0047] Silica was prepared by a modified Stober method. 1 g of silica particles was dispersed in ethanol (100 mL) and sonicated for 15 minutes to ensure uniform dispersion of the dispersion. Then 0.1430 g of APTES was dispersed in ethanol, and then slowly added into the silica suspension, and then stirred at 50° C. for about 24 hours under a nitrogen atmos...

Embodiment 2

[0087] SiO 2 -NH 2 The preparation method is with embodiment 1. Graphene oxide (GO) was prepared from natural graphite using a modified Hummers method. In the synthesis of N-doped airgel, 1 mL of SiO 2 -NH 2 The ethanol dispersions were respectively dispersed in 3 mg / mL GO aqueous solution. The suspension was then sealed in a Teflon-lined stainless steel autoclave for hydrothermal reaction at 160 °C for 14 h. The product was repeatedly washed with distilled water three times, and then freeze-dried to prepare an airgel. The prepared airgel was placed in a tube furnace with two temperature zones, and argon gas was passed through for 15 minutes to exhaust the air. and at 5°C min under argon -1 at a rate of 800 °C, followed by calcination at 800 °C for 1.5 h, and then cooled to room temperature. The resulting N-doped graphene gel was etched with hydrofluoric acid (3-5% molar concentration) and washed again with distilled water.

Embodiment 3

[0089] SiO 2 -NH 2 The preparation method is with embodiment 1. Graphene oxide (GO) was prepared from natural graphite using a modified Hummers method. In the synthesis of N-doped airgel, 1 mL of SiO 2 -NH 2The ethanol dispersions were respectively dispersed in 3 mg / mL GO aqueous solution. The suspension was then sealed in a Teflon-lined stainless steel autoclave for hydrothermal reaction at 172 °C for 13 h. The product was repeatedly washed with distilled water three times, and then freeze-dried to prepare an airgel. The prepared airgel was placed in a tube furnace with two temperature zones, and argon gas was passed through for 15 minutes to exhaust the air. and at 5°C min under argon -1 at a rate of 860 °C, followed by calcination at 860 °C for 1.4 h, and then cooled to room temperature. The resulting N-doped graphene gel was etched with hydrofluoric acid (3-5% molar concentration) and washed again with distilled water.

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Abstract

The invention provides a method for preparing nitrogen-doped graphene aerogel by simultaneously using SiO2-NH2 as a template and a nitrogen doping agent. Amino functionalized silica (SiO2-NH2) is used as the template to prevent the stacking of graphene sheets, and is also used as the doping agent. A result of analysis of the microstructure, the porousness and the chemical composition of graphene through SEM, TEM, XRD spectrum, Raman, XPS and BET technologies shows that the content of the SiO2-NH2 has a remarkable influence on the surface area and the carbon activity of the graphene sheets. A 3D layered porous graphene gel electrode has excellent electrochemical performances due to the large specific surface area of 481.8 m<2>g<-1> and high nitrogen doping content (4.4%), has an ultrahigh specific capacitance of 350 F g<-1> under a current density of 1 A g<-1>, and has good reversibility after 5000 cycles in aqueous and organic electrolytes, and the cycle efficiency is 92.8%. Additionally, the N-doped graphene aerogel has high oil absorbency and good recoverability. The method has the advantages of simple steps, convenience in operation, and high practicality.

Description

technical field [0001] The invention belongs to the field of graphene-based materials, in particular to a SiO 2 -NH 2 A method for preparing nitrogen-doped graphene aerogels simultaneously as a template and a nitrogen dopant. Background technique [0002] To reduce the power consumption of electronic devices and electric vehicles, the development of new energy storage devices with high power density and energy density is urgently needed. Supercapacitors are a promising energy storage device due to their outstanding properties, such as fast charge-discharge capability, long cycle life and wide operating temperature, and safety. Graphene, a typical two-dimensional planar monolayer of sp2 carbon atoms, has attracted extensive attention in this regard due to its excellent mechanical and electrical properties and extremely high surface. Theoretically, if fully utilized its entire surface area is 2630m 2 g -1 , the capacitance of single-layer graphene can reach 550F g -1 . ...

Claims

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Application Information

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IPC IPC(8): C01B32/184H01G11/24H01G11/36
CPCY02E60/13H01G11/24C01P2002/72C01P2002/80C01P2002/82C01P2002/85C01P2004/01C01P2004/03C01P2004/04C01P2006/12C01P2006/40H01G11/36
Inventor 刘利彬杜永旭张强郭改兰潘晨光
Owner 山东济清科技服务有限公司
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