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Heteroatom-doped porous graphite electro-catalyst and preparation and application thereof as well as device

A technology of porous graphene and electrocatalyst, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical/physicochemical processes of energy application, etc. Long reaction time and other problems, to achieve the effect of reducing van der Waals interaction, improving electrocatalytic performance, and good solubility

Active Publication Date: 2015-10-07
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of using these two methods are: 1) the operating conditions are relatively harsh, the reaction temperature is high (usually >800 ° C), and the reaction time is long; 2) the degree of reduction is not high, and the C / O atomic ratio is only 10, which affects the The conductivity of heteroatom-doped graphene; 3) the degree of doping is not high, the amount of heteroatom doping is less than 10%, and it is not easy to control; 4) the preparation cost is high; 5) the prepared graphene sheets are easy to aggregate, due to High specific surface area, graphene is easy to aggregate due to strong van der Waals forces between planes
Oxygen reduction mainly occurs at the edge of the graphene sheet, and the practical utilization rate of the catalyst is low, which greatly hinders the application in batteries

Method used

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  • Heteroatom-doped porous graphite electro-catalyst and preparation and application thereof as well as device
  • Heteroatom-doped porous graphite electro-catalyst and preparation and application thereof as well as device
  • Heteroatom-doped porous graphite electro-catalyst and preparation and application thereof as well as device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] A preparation method of heteroatom-doped porous graphene electrocatalyst, specifically comprising the following steps:

[0054] (1) Synthesis of graphene oxide

[0055] Adopt improved Hummers method to prepare graphene oxide, its technological process is as follows:

[0056] (1-1) Assemble the reaction flask in an ice-water bath, add a solid mixture of 1g of expanded graphite powder and 2.5g of sodium nitrate to the reaction flask under stirring (the stirring speed is 500r / min), and then add 150mL of mass percentage 95% concentrated sulfuric acid, reacted in an ice-water bath for 30 minutes; then, added 15 g of potassium permanganate 60 times (1 min each time), controlled the reaction temperature at 0 ° C, and continued to react for 12 h; then added 150 mL of deionized water to dilute After stirring and reacting for 30 minutes (the rotating speed of stirring is 500r / min), the temperature was raised to 98° C. at a heating rate of 10° C. / min, and the heat preservation re...

Embodiment 2

[0071] Preparation of the nitrogen-doped porous graphene-modified glassy carbon electrode prepared in Example 2: The nitrogen-doped porous graphene electrocatalyst prepared in Example 2 was replaced by the nitrogen-doped porous graphene electrocatalyst prepared in Example 1, using the method of implementing The preparation method of the glassy carbon electrode modified by the nitrogen-doped porous graphene electrocatalyst prepared in Example 1 can obtain the desired electrode.

[0072] Preparation of commercial Pt / C modified glassy carbon electrode: Weigh 4 mg of commercial Pt / C (purchased from Johnson-Matthey, UK, with a mass ratio of 40%), drop 35 μL of 5wt% Nafion solution, and then disperse it in In ethanol with a volume of 1mL, ultrasonically disperse for 60min in an ultrasonic instrument with a frequency of 50KHz and a power of 150W to obtain a uniformly dispersed ink. Take 5μL of ink and drop-coat it on the surface of a glassy carbon electrode with a diameter of 5mm, and...

Embodiment 3

[0080] A heteroatom-doped porous graphene electrocatalyst, the specific preparation method is:

[0081] (1) synthesis of graphene oxide: same as embodiment 1;

[0082] (2) synthesis of graphene oxide with holes on the surface: same as embodiment 1;

[0083] (3) Graphene oxide with holes on the surface mixed with dibenzyl disulfide

[0084] 20mg of graphene oxide with holes on the surface prepared in step (2), 100mg of dibenzyl disulfide and ethanol were first ultrasonically mixed for 60min (frequency is 50KHz, power is 150W), and then stirred and mixed for 12h (stirring speed is 500r / min) , to obtain a coating solution with a concentration of 30% by mass, and then apply the coating solution to the surface of copper foil by scraping method, and freeze-dry (the temperature is -48°C, the drying time is 24h), and the obtained solution loaded on the substrate is Solid films of graphene oxide dibenzyl disulfide with pores on the surface;

[0085] (4) Plasma preparation of heteroa...

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Abstract

The invention belongs to the field of carbon materials and electrochemistry, and discloses a heteroatom-doped porous graphite electro-catalyst and preparation and application thereof as well as a device. The method comprises the following steps: firstly adding concentrated HNO3 into a graphite oxide aqueous solution, performing sealing, ultrasonic reaction and stewing, and pouring the solution into deionized water for centrifugation, filtering and drying to obtain graphite oxide with holes in the surface; uniformly mixing the graphite oxide with holes in the surface, a heteroatom-doped source compound and a solvent to obtain a mixture, coating the surface of a substrate with the mixture, and performing freeze drying to obtain a solid thin film; putting the substrate loaded with the solid thin film into a plasma high-temperature tubular reactor for reaction to obtain the heteroatom-doped porous graphite electro-catalyst. The prepared electro-catalyst is higher in oxygen reduction electro-catalytic performance and is higher in electrochemical performance when applied in an electrode material; the electro-catalyst can be applied to the field of proton exchange membrane fuel batteries, direct alcohol fuel batteries and metal-air battery anode materials.

Description

technical field [0001] The invention relates to the fields of carbon materials and electrochemistry, in particular to a heteroatom-doped porous graphene electrocatalyst and its preparation method, application and device. Background technique [0002] Fuel Cells is a new energy technology that directly converts the chemical energy of fuel into electrical energy in an efficient and environmentally friendly manner, because of its high energy conversion efficiency, low impact on the environment (zero or low emission), and fuel diversification. They have received widespread attention due to their many advantages; they are known as the fourth generation of power generation technology after water power, fire power and nuclear power. Among them, the proton exchange membrane fuel cell has the advantages of low operating temperature and fast start-up speed, and is considered to be the most promising alternative to the internal combustion engine as the future automotive power plant. A...

Claims

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Application Information

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IPC IPC(8): B01J21/18B01J27/14B01J27/04B01J19/08H01M4/90
CPCY02E60/50
Inventor 蒋仲杰
Owner SOUTH CHINA UNIV OF TECH
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