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A method for preparing in situ oxygen-doped three-dimensional graphene by electrochemical exfoliation

A technology of oxygen doping and graphene, applied in the field of electrochemical materials, can solve the problems of reduced conductivity, low oxygen doping content, high production cost, etc.

Active Publication Date: 2021-05-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Other oxygen-doped graphene preparation technologies, including plasma method, high-temperature calcination method and electrolysis method (CN107601488A, CN107311165A), have problems such as low oxygen doping content, complex equipment, high production cost, etc., and it is difficult to realize industrialization
[0005] In addition, most of the oxygen-doped graphene materials reported so far are powder materials, which need to be prepared twice to become electrodes. The process is complicated, and the introduced binder material will reduce the conductivity and inhibit its catalytic performance.
[0006] How to overcome the problems of long preparation cycle, high cost and low oxygen doping amount in the existing oxygen-doped graphene technology has become an urgent problem in the industry

Method used

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  • A method for preparing in situ oxygen-doped three-dimensional graphene by electrochemical exfoliation
  • A method for preparing in situ oxygen-doped three-dimensional graphene by electrochemical exfoliation
  • A method for preparing in situ oxygen-doped three-dimensional graphene by electrochemical exfoliation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] a) Preparation of in-situ oxygen-doped three-dimensional electrochemically exfoliated graphene materials:

[0037] 1. Washing of natural graphite flakes:

[0038] (1) Cut the natural graphite sheet into a size of 3*4cm;

[0039] (2) Ultrasonic washing with acetone, deionized water and ethanol for 30 min respectively;

[0040] (3) After washing the surface of the natural graphite sheet again with deionized water, dry it overnight at 60°C in an oven;

[0041] 2. Liquid nitrogen freezing expansion:

[0042] (1) Put the above-mentioned cleaned natural graphite flakes into liquid nitrogen, and freeze for 10 seconds;

[0043] (2) Quickly take out the graphite flakes and put them into the water at room temperature;

[0044] (3) Take out the expanded graphite sheet, put it into deionized water for washing, and remove the graphite that has completely peeled off after the surface is frozen and expanded by liquid nitrogen;

[0045] (4) Place in an oven and dry overnight at 60...

Embodiment 2

[0103] a) Preparation of in-situ oxygen-doped three-dimensional graphene materials:

[0104] 1. Washing of natural graphite flakes:

[0105] (1) Cut the natural graphite sheet into a size of 3*4cm;

[0106] (2) Ultrasonic washing with acetone, deionized water and ethanol for 30 min respectively;

[0107] (3) After washing the surface of the natural graphite sheet again with deionized water, dry it overnight at 60°C in an oven;

[0108] 2. Liquid nitrogen freezing expansion:

[0109] (1) Put the above-mentioned cleaned natural graphite flakes into liquid nitrogen and freeze for 2 hours;

[0110] (2) Quickly take out the graphite flakes and put them into the water at room temperature;

[0111] (3) take out the graphite sheet after expansion, put into deionized water and wash, remove the graphite that the surface has completely peeled off through liquid nitrogen freezing expansion;

[0112] (4) Place in an oven and dry overnight at 60°C;

[0113] 3. Electrostripping:

[01...

Embodiment 3

[0129] a) Preparation of in-situ oxygen-doped three-dimensional graphene materials:

[0130] 1. Washing of natural graphite flakes:

[0131] (1) Cut the natural graphite sheet into a size of 3*4cm;

[0132] (2) Ultrasonic washing with acetone, deionized water and ethanol for 30 min respectively;

[0133] (3) After washing the surface of the natural graphite sheet again with deionized water, dry it overnight at 60°C in an oven;

[0134] 2. Liquid nitrogen freezing expansion:

[0135] (1) Put the above-mentioned cleaned natural graphite flakes into liquid nitrogen and freeze for 10 minutes;

[0136] (2) Quickly take out the graphite flakes and put them into the water at room temperature;

[0137] (3) take out the graphite sheet after expansion, put into deionized water and wash, remove the graphite that the surface has completely peeled off through liquid nitrogen freezing expansion;

[0138] (4) Place in an oven and dry overnight at 60°C;

[0139] 3. Electrostripping:

...

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PUM

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Abstract

The invention discloses a method for preparing in-situ oxygen-doped three-dimensional graphene through electrochemical exfoliation, comprising: after the graphite sheet is pretreated, subjected to liquid nitrogen freezing and physical expansion treatment to obtain an expanded graphite sheet; the expanded graphite sheet is passed through The electrochemical stripping method is transformed into an in-situ oxygen-doped three-dimensional graphene material; the electrolytic solution for electrostripping is an oxidizing acid electrolyte. The preparation process route of the method is short, the required equipment is simple, the raw material price is low, and the preparation cycle is short; the in-situ oxygen-doped three-dimensional graphene provided by the preparation method of the present invention can be directly grown on the surface of the graphene material, which is not a powder material and can be directly It is used as an electrode material without secondary electrode preparation; and in an acidic electrolyte, its anode overpotential is as low as 268mV, which has both high-efficiency catalytic activity and good stability. The preparation of in-situ oxygen-doped three-dimensional graphene materials also has obvious cost advantages and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of electrochemical materials, in particular to a method for preparing in-situ oxygen-doped three-dimensional graphene by electrochemical exfoliation. Background technique [0002] Water splitting to produce hydrogen and oxygen is recognized as the most potential energy conversion technology and an important means to solve the energy crisis and environmental pollution. Compared with other energy conversion technologies such as fossil fuel hydrogen production and wind energy hydrogen production, electrocatalytic water splitting hydrogen production has the characteristics of cleanness, continuity and high efficiency. However, the low energy conversion efficiency limits the development of its application. The root cause is that the anode material has a high overpotential. [0003] At present, the water splitting hydrogen production reaction is more efficient in acidic environment, but the acidic environment is not conduc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C25B1/04C25B11/075
CPCC25B1/04C25B11/04C01B32/19Y02E60/36
Inventor 侯阳雷超君杨彬杨建雷乐成
Owner ZHEJIANG UNIV
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