Palladium/nitrogen-doped graphene composite electrode catalyst and preparation method thereof

A nitrogen-doped graphene and composite electrode technology, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems that are not suitable for large-scale industrial production and preparation High cost, complex process and other issues, to achieve excellent electrochemical performance, long cycle life and good repeatability

Inactive Publication Date: 2015-11-04
NANJING UNIV OF SCI & TECH +1
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  • Abstract
  • Description
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Problems solved by technology

However, these preparation methods are complex in process, high in preparation cost and low in yield, and are not suitable for large-scale industrial production, such as the literature Sheng Z H, Shao L, Chen J J, et al.Catalyst-free synthesis of nitrogen-doped graphene via thermal The preparation method disclosed in annealing graphite oxide with melamine and its excellent electrocatalysis.ACS Nano, 2011,5:4350-4358

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  • Palladium/nitrogen-doped graphene composite electrode catalyst and preparation method thereof
  • Palladium/nitrogen-doped graphene composite electrode catalyst and preparation method thereof
  • Palladium/nitrogen-doped graphene composite electrode catalyst and preparation method thereof

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Embodiment 1

[0037] Step 1: Disperse 200 mg of graphite oxide ultrasonically in 50 mL of deionized water for 2 hours to obtain a graphene oxide solution;

[0038] In the second step, 200mg of melamine was added to the system of the first step, and heated to reflux at 80°C for 2 hours, and stirred to reduce to room temperature;

[0039] The third step is to freeze-dry the reaction system of the second step;

[0040] In the fourth step, the powder obtained after the third step freeze-drying is heat-treated at 500°C for 1 hour under a nitrogen atmosphere, and then the temperature is raised to 700°C for 2 hours to obtain nitrogen-doped graphene;

[0041] In the fifth step, 10 mg of the nitrogen-doped graphene obtained in the fourth step is ultrasonically dispersed in 80 mL of ethylene glycol solution for 2 hours to obtain a dispersion solution of the nitrogen-doped graphene;

[0042] In the sixth step, add 0.025mL of 0.73mol / L palladium nitrate solution to the system of the fifth step and mix and stir f...

Embodiment 2

[0046] The first step: ultrasonically disperse 100 mg of graphite oxide in 100 mL of deionized water for 2 hours to obtain a graphene oxide solution;

[0047] In the second step, 300mg of melamine was added to the system of the first step, and heated to reflux at 80°C for 2 hours, and stirred to reduce to room temperature;

[0048] The third step is to freeze-dry the reaction system of the second step;

[0049] In the fourth step, the powder obtained after the third step freeze-drying is heat-treated at 700°C for 4 hours in a nitrogen atmosphere to obtain nitrogen-doped graphene;

[0050] In the fifth step, 10 mg of the nitrogen-doped graphene obtained in the fourth step is ultrasonically dispersed in 50 mL of ethylene glycol solution for 2 hours to obtain a dispersion solution of the nitrogen-doped graphene;

[0051] In the sixth step, 0.012 mL of 0.73 mol / L palladium nitrate solution was added to the system in the fifth step and mixed and stirred for 20 minutes;

[0052] In the seventh...

Embodiment 3

[0055] Step 1: Disperse 200 mg of graphite oxide ultrasonically in 100 mL of deionized water for 2 hours to obtain a graphene oxide solution;

[0056] In the second step, 400mg of melamine was added to the system of the first step, and heated to reflux at 80°C for 2 hours, and stirred to reduce to room temperature;

[0057] The third step is to freeze-dry the reaction system of the second step;

[0058] In the fourth step, the powder obtained after the third step freeze-drying is heat-treated at 550°C for 2 hours under a nitrogen atmosphere, and then the temperature is increased to 800°C for 2 hours to obtain nitrogen-doped graphene;

[0059] In the fifth step, 10 mg of the nitrogen-doped graphene obtained in the fourth step was ultrasonically dispersed in a 100 mL ethylene glycol solution for 2 hours to obtain a dispersion solution of the nitrogen-doped graphene;

[0060] In the sixth step, add 0.025mL of 0.73mol / L palladium nitrate solution to the system of the fifth step and mix and ...

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Abstract

The invention discloses a palladium/nitrogen-doped graphene composite electrode catalyst and a preparation method thereof. The preparation method comprises the following steps: carrying out ultrasonic dispersion on oxidized graphene in water, adding tripolycyanamide, heating and stirring the mixture, freezing and drying the mixed system and carrying out high-temperature heat treatment, so as to obtain nitrogen-doped graphene; carrying out ultrasonic dispersion again on the nitrogen-doped graphene in an ethylene glycol solution, adding a palladium nitrate solution to the ethylene glycol solution and mixing the mixture evenly; reducing palladium nitrate by virtue of a mild reduction method, and depositing palladium nanoparticles in-situ on the surface of the nitrogen-doped graphene; and after reaction is ended, carrying out centrifugal separation to obtain a solid product, and washing and drying the product to obtain the catalyst. By virtue of the mild reduction method, the palladium nanoparticles are deposited in-situ on the surface of the nitrogen-doped graphene; and high temperature or high pressure is not needed, so that the preparation method is simple and controllable, and the repeatability is relatively good. The prepared palladium/nitrogen-doped graphene composite electrode catalyst has excellent electrochemical properties as a direct methanol/formic acid fuel cell cathode material.

Description

Technical field [0001] The invention relates to a palladium / nitrogen doped graphene composite electrode catalyst and a preparation method thereof, and belongs to the field of nano material preparation. Background technique [0002] Direct methanol / formic acid fuel cell, as a new generation of proton membrane fuel cell, has the advantages of low operating temperature, high energy efficiency, no electrolyte corrosion, low pollution emissions and easy fuel transportation. It has broad application prospects in the field of portable electronic equipment. At present, the main obstacles restricting the commercialization of direct methanol / formic acid fuel cells are the high production cost and the slow oxidation kinetic reaction rate of liquid fuels (methanol and formic acid). The key to solving these problems is to find suitable anode catalyst materials. [0003] In recent years, the rise of nano-carbon materials (such as fullerenes, carbon nanotubes, graphene, etc.) has provided new ide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/92B01J23/44
CPCB01J23/44H01M4/926Y02E60/50
Inventor 汪信张文耀付永胜朱俊武钱华玉胡辰尧孙敬文范晔查道松夏佳伟
Owner NANJING UNIV OF SCI & TECH
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