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Preparation method and application of graphene-supported non-noble metal electrocatalyst

A non-precious metal, electrocatalyst technology, applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of performance gap and large particle size of electrocatalysts, etc. Achieve the effect of small size, high density and mild reaction conditions

Inactive Publication Date: 2014-08-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above methods only use a nitrogen-containing ligand, and the prepared electrocatalyst has a large particle size, and its performance is far behind that of platinum-based electrocatalysts.

Method used

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  • Preparation method and application of graphene-supported non-noble metal electrocatalyst
  • Preparation method and application of graphene-supported non-noble metal electrocatalyst

Examples

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Embodiment 1

[0040] Place 105mg of o-phenanthroline and 66mg of melamine in 100mL of deionized water, heat in a water bath at 80°C until dissolved, and dissolve 31mg of CoCl 2 ·H 2 O and 66 mg FeCl 3 Dissolve in 10 mL of deionized water respectively, and preheat in a water bath at 80°C after mixing, mix the above two preheated solutions, and reflux and stir in a water bath at 80°C for 30 minutes. Graphene oxide with a mass of 200 mg was weighed in 100 mL of deionized water for 40 min, dispersed evenly, placed in a water bath at 80 ° C for preheating, then added to the above reaction solution, refluxed and stirred for 30 min and then cooled to room temperature. Weigh 400mg of NaBH 4 Dissolve in 50mL deionized water, add dropwise to the reaction system, react for 30min, filter with suction, and dry under vacuum at 65°C. Under the protection of argon atmosphere, the temperature was programmed to 800 °C, stabilized for 2 h, and then naturally cooled to room temperature. 0.5M H 2 SO 4 The...

Embodiment 2

[0055] Different heat treatment temperatures: 105mg of o-phenanthroline and 66mg of melamine were placed in 100mL of deionized water, heated in a water bath at 80°C until dissolved, and 31mg of CoCl 2 ·H 2 O and 66 mg FeCl 3 Dissolve in 10mL deionized water respectively, and preheat in a water bath at 80°C after mixing, mix the above two preheated solutions, and reflux and stir in a water bath at 80°C for 30min. Graphene oxide with a mass of 200 mg was weighed in 100 mL of deionized water for 40 min, dispersed evenly, placed in a water bath at 80 ° C for preheating, then added to the above reaction solution, refluxed and stirred for 30 min and then cooled to room temperature. Weigh 400mg of NaBH 4 Dissolve in 50mL deionized water, add dropwise to the reaction system, react for 30min, filter with suction, and dry under vacuum at 65°C. Under the protection of argon atmosphere, the temperature was programmed to 450°C or 900°C, stabilized for 2 hours, and then naturally cooled ...

Embodiment 3

[0058] Three kinds of nitrogen-containing ligands: 35 mg of phenanthroline, 22 mg of melamine and 27 mg of 4,4’-bipyridine were placed in 100 mL of deionized water and heated in a water bath at 80 °C until dissolved, and 31 mg of CoCl 2 ·H 2 O and 66 mg FeCl 3 Dissolve in 10mL deionized water respectively, preheat in a water bath at 80°C after mixing, mix the above two preheated solutions, reflux and stir in a water bath at 80°C for 30min. Weigh 200 mg of graphene oxide in 100 mL of deionized water for 40 min, disperse evenly, place it in a water bath at 80 ° C for preheating, then add it to the above reaction solution, reflux and stir for 30 min, then cool to room temperature. Weigh 400mg of NaBH 4 Dissolve in 50mL deionized water, add dropwise to the reaction system, react for 30min, filter with suction, and dry under vacuum at 65°C. Under the protection of argon atmosphere, the temperature was programmed to 800 °C, stabilized for 2 h, and then naturally cooled to room te...

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Abstract

The invention provides a preparation method and application of a graphene-supported non-noble metal electrocatalyst. The method comprises the following concrete steps: under a heating condition, mixing a nitrogen-containing ligand with a metal salt to form a complex; depositing the complex on a graphene supporter through cooling; adding a reducing agent to reduce oxidized graphene; and carrying out washing, drying, heat treatment and pickling so as to obtain the graphene-supported non-noble metal electrocatalyst. The graphene-supported non-noble metal electrocatalyst prepared in the invention is such structured that particles with a size of 2 to 200 nm supports or coats reduced oxidized graphene. Under an alkaline condition, the onset potential of the non-noble metal electrocatalyst in an oxygen reduction reaction is positively shifted by 35 mV compared with that of a 20 wt% commercial platinum / carbon electrocatalyst, and durability and methanol poisoning resistance of the non-noble metal electrocatalyst are better than those of the 20 wt% commercial platinum / carbon electrocatalyst. The graphene-supported non-noble metal electrocatalyst can be applied to proton exchange membrane fuel cells.

Description

technical field [0001] The invention belongs to the field of proton exchange membrane fuel cell electrocatalysts, and in particular relates to a preparation method and application of a graphene-supported non-noble metal electrocatalyst. Background technique [0002] The electrocatalysts of proton exchange membrane fuel cells (PEMFC) are mainly noble metal platinum and its alloys. However, due to the disadvantages of platinum, such as high price, scarce resources, poor durability, and easy to be poisoned, the commercialization process of fuel cells has been seriously hindered. One possible solution is to develop non-precious metal electrocatalysts that can replace platinum and reduce the cost of fuel cells. [0003] Chinese patent (CN102324531A) reported a preparation method and application of a carbon-supported CoN fuel cell catalyst. Under the protection of an inert atmosphere, a carbon-supported CoN electrocatalyst was prepared by heat-treating a mixture of Co salt, nitrog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75B01J23/755H01M4/90
CPCY02E60/50
Inventor 宋玉江谢妍
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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