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Self-doped fullerene immobilized palladium nan-electrocatalyst, preparation method and application

An electrocatalyst and self-doping technology, applied in the direction of circuits, electrical components, battery electrodes, etc., can solve the problems of poor repeatability and complicated operation, and achieve the effect of simple operation, good repeatability and high conductivity

Active Publication Date: 2018-06-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing methods for preparing electrocatalysts with fullerene carriers such as: acoustic preparation, electrophoresis, high-temperature template synthesis, chemical vapor deposition, etc., are complex in operation and poor in repeatability. Key to low-cost, high-performance catalysts

Method used

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  • Self-doped fullerene immobilized palladium nan-electrocatalyst, preparation method and application
  • Self-doped fullerene immobilized palladium nan-electrocatalyst, preparation method and application
  • Self-doped fullerene immobilized palladium nan-electrocatalyst, preparation method and application

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Embodiment 1

[0038] Mix 1.1 mg (1 μmol) PCBANI with 50 μL acetic acid and sonicate for 5 minutes, then add 1.95 mL methanol and sonicate for 15 minutes. Electrodes were ultrasonically cleaned with acetone, deionized water and ethanol for 5 min, respectively. Then the PCBANI dispersion was added dropwise on the electrode, and spin-coated at a speed of 300 rpm for 1.5 hours to obtain a PCBANI film. Subsequently, the electrode coated with PCBANI film was exposed to 1 mg / mL K 2 PdCl 4 Soak in aqueous solution for 30 minutes, soak in pure water for 10 minutes. It was then treated with hydrazine hydrate solution for 5 minutes and rinsed with deionized water. The Pd loading was determined by ICP-MS, and the obtained working electrode can be used for electrocatalytic activity test.

[0039] The electrocatalytic oxidation of ethanol was tested by cyclic voltammetry (CV) using a three-electrode system at room temperature. Pt electrode and Hg / HgO electrode were used as counter and reference elec...

Embodiment 2

[0043] Mix 2.2 mg (2 μmol) PCBANI with 50 μL acetic acid and sonicate for 5 minutes, then add 1.95 mL methanol and sonicate for 15 minutes. Then the PCBANI dispersion was added dropwise on the cleaned electrode, and spin-coated at a speed of 300 rpm for 1.5 hours to obtain a PCBANI film. Subsequently, the electrode coated with PCBANI film was exposed to 1 mg / mL K 2 PdCl 4 Soak in aqueous solution for 30 minutes, soak in pure water for 10 minutes. It was then treated with hydrazine hydrate solution for 5 minutes and rinsed with deionized water. The mass current density of the obtained working electrode for the electrocatalytic oxidation of ethanol is 969.9 A g -1 .

Embodiment 3

[0045] Mix 0.22 mg (0.1 μmol) PCBANI with 50 μL acetic acid and sonicate for 5 minutes, then add 1.95 mL methanol and sonicate for 15 minutes. Then the PCBANI dispersion was added dropwise on the cleaned electrode, and spin-coated at a speed of 300 rpm for 1.5 hours to obtain a PCBANI film. Subsequently, the electrode coated with PCBANI film was treated at 1mg / mLK 2 PdCl 4 Soak in aqueous solution for 30 minutes, soak in pure water for 10 minutes. It was then treated with hydrazine hydrate solution for 5 minutes and rinsed with deionized water. The obtained working electrode has a mass current density of 150 A g for the electrocatalytic oxidation of ethanol -1 .

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Abstract

The invention discloses a self-doped fullerene immobilized palladium nan-electrocatalyst, a preparation method and application. The preparation method comprises the following steps: mixing self-dopedfullerene ammonium iodine salt and a solvent, dispersing a mixture, then dropwise adding a dispersion liquid on an electrode, and performing spin-coating to form a film; soaking the electrode in a K2PdCl4 aqueous solution and a hydrazine hydrate solution in sequence, and flushing the electrode with deionized water, wherein the obtained working electrode can be used for electrocatalysis of oxidation of alcohols. Because of weak interaction between the self-doped fullerene ammonium iodine salt with high electrical conductivity and palladium, and a porous morphology and structure of a thin film of the self-doped fullerene ammonium iodine salt, scattered palladium immobilization and mass transfer are benefited. Compared with commoditized Pd / C, the obtained catalyst shows high catalytic activity and good stability. Therefore, a simple method for preparing a high-efficiency electrocatalyst which is directly used for an alcohol fuel battery in situ is provided.

Description

technical field [0001] The invention relates to a preparation method and application of a palladium nano electrocatalyst. Background technique [0002] Fuel cells are emerging as one of the most promising power source alternatives for stable, portable and mobile systems. Noble metal (such as Pd and Pt) nanocatalysts (NCs) have played an important role in fuel cells (FCs). For the anode catalysts of direct alcohol fuel cells (DAFCs), Pd is cheaper than Pt and has higher resistance to CO poisoning. Therefore, in recent years, researchers have devoted themselves to the development of Pd-based nanoparticle (NP) catalysts loaded on various supports. [0003] Carbon-based materials are an important class of electrocatalyst supports. These carbon supports have a great influence on the performance of noble metal catalysts, such as the dispersion, particle size distribution, and morphology of nanoparticles. Meanwhile, the microstructure and surface morphology of supports also syn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/88H01M4/90
CPCH01M4/8825H01M4/8828H01M4/921H01M4/925Y02E60/50
Inventor 雷鸣林周晨王欢欢
Owner ZHEJIANG UNIV
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