High-specific-surface-area nitrogen doped grapheme and preparation method thereof

A nitrogen-doped graphene, large specific surface area technology, applied in graphene, chemical instruments and methods, inorganic chemistry and other directions, to achieve the effect of time and energy cost reduction, high specific surface area

Active Publication Date: 2016-11-23
BEIJING GUANGKEBOYE SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, at this stage, these energy alternatives still have their own shortcomings

Method used

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  • High-specific-surface-area nitrogen doped grapheme and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A.Hummers method prepares graphene oxide:

[0037] (1) Oxidation: take by weighing natural flake graphite 3g, potassium permanganate 7g, wherein the diameter of natural flake graphite particle is 1-200 micron, slowly add 60ml mass concentration after two kinds of raw materials are mixed and be the vitriol oil of 98%, concentrated The sulfuric acid temperature is 2°C. After the mixture was kept at 0-2°C and stirred for 60 minutes, the temperature was adjusted to 30°C, and then kept stirring for 60 minutes. Slowly add 150ml of deionized water at a temperature of 2°C for the first time, while increasing the stirring speed. Raise the temperature to 95°C, keep warm for 15 minutes, then add 6ml of hydrogen peroxide with a mass fraction of 30%, and then add 250ml of deionized water for dilution. The concentration of graphite oxide is about 6mg / ml to obtain a graphite oxide dilution.

[0038] (2) Ultrasonic: The obtained graphite oxide solution is subjected to ultrasonic trea...

Embodiment 2

[0046] A.Hummers method prepares graphene oxide:

[0047] (1) Oxidation: take artificial graphite powder 3.5g, potassium permanganate 6.5g, wherein the diameter of artificial graphite powder particle is 1-200 micron, after two kinds of raw materials mix, slowly add 105ml concentration and be the concentrated sulfuric acid of 98%, The temperature of concentrated sulfuric acid is 2°C. After the mixture was kept at 0-2°C and stirred for 120 minutes, the temperature was adjusted to 40°C, and then kept stirring for 120 minutes. Slowly add 230ml of deionized water at a temperature of 2°C for the first time, while increasing the stirring speed. Raise the temperature to 90°C, keep warm and heat for 15 minutes, then add 11ml of hydrogen peroxide with a mass fraction of 30%, and then add 200ml of deionized water to dilute the acid solution. The graphite oxide concentration is about 10mg / ml to obtain a graphite oxide dilution.

[0048] (2) Ultrasonic: Ultrasonic treatment is performed ...

Embodiment 3

[0056] A.Hummers method prepares graphene oxide:

[0057] (1) Oxidation: take expanded graphite 10g, potassium permanganate 20g, wherein the diameter of expanded graphite particle is 1-200 micron, slowly add 250ml concentration after two kinds of raw materials mix and be the vitriol oil of 98%, the vitriol oil temperature is 2°C. After the mixture was kept at 0-2°C and stirred for 90 minutes, the temperature was adjusted to 35°C, and then kept stirring for 90 minutes. Slowly add 500ml of deionized water at a temperature of 2°C for the first time, while increasing the stirring speed. Raise the temperature to 93°C, keep warm for 10 minutes, then add 25ml of hydrogen peroxide with a mass fraction of 30%, and then add 700ml of deionized water to dilute the acid solution. The graphite oxide concentration is about 8mg / ml to obtain a graphite oxide dilution.

[0058] (2) Ultrasound: The obtained graphite oxide solution was subjected to ultrasonic treatment, the power of the ultraso...

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Abstract

The invention provides a preparation method of high-specific-surface-area nitrogen doped grapheme by adopting a microwave vacuum high-temperature heating furnace. The preparation method includes the steps of 1), preparing grapheme oxide (2) by a Hummers method and performing in-situ microwave treatment, thermal reduction and chemical vapor deposition (CVD) doping of the grapheme oxide. In-situ operations of microwave prestripping and thermal reduction before thermal reduction and chemical vapor deposition doping after thermal reduction of the grapheme oxide are realized on the premise of self-improvement of equipment, synthetic efficiency is increased, energy consumption of synthesis is lowered, and the preparation method is suitable for industrial mass production. The doped grapheme obtained in synthesis can be used in fields of electrochemical catalysis, supercapacitor and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and specifically relates to nitrogen-doped graphene with a large specific surface area and a preparation method thereof. Background technique [0002] With the continuous depletion of non-renewable resources such as coal, oil, and natural gas and the increasingly serious environmental pollution, it is particularly urgent and important to research and develop new energy storage devices that can provide renewable, green, and clean energy for human beings. Among many energy alternatives, supercapacitors and new batteries have huge potential and market. [0003] However, at this stage, these energy alternatives still have their own shortcomings. The capacity of lithium-ion battery cathode materials and supercapacitor electrode materials is not high, fuel cells rely on expensive noble metal electrode catalysts, and the cathode oxygen reduction reaction rate is much lower than the anode hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04H01M4/583H01M4/96H01G11/36
CPCC01B2204/20C01B2204/32C01P2004/03H01G11/36H01M4/583H01M4/96Y02E60/10Y02E60/13Y02E60/50
Inventor 田陆黄郁君
Owner BEIJING GUANGKEBOYE SCI & TECH
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