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Preparation method of ordered mesoporous non-noble metal-nitrogen-graphitized carbon material

A non-precious metal, graphitized carbon technology, used in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, chemical/physical processes, etc., can solve the problem of poor contact between active sites and conductive carriers, catalytic activity It can reduce the stability of the battery, hinder the output power of the battery, etc., and achieve the effect of increasing the density of catalytic active sites, improving the oxygen conversion rate, superior catalytic stability and methanol resistance.

Inactive Publication Date: 2013-09-25
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Secondly, the active species loaded on the surface of the carrier and the carbon carrier usually belong to two phases, which will re-accumulate or the carrier will peel off during use, resulting in the loss of effective active components, resulting in a decrease in the overall catalytic activity and stability of the material.
Moreover, in the iron-nitrogen-carbon catalytic material prepared by the carbon support-pyrolysis method, it is easy to occur the bad contact between the active site and the conductive aluminum support, especially when the cathode catalyst coating using the carbon support material is thick, it will be serious. hinder the output power of the battery
These factors have become obstacles that limit the use of existing methods to prepare highly active iron-nitrogen-carbon cathode catalytic materials that can replace Pt-based catalysts.

Method used

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  • Preparation method of ordered mesoporous non-noble metal-nitrogen-graphitized carbon material
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  • Preparation method of ordered mesoporous non-noble metal-nitrogen-graphitized carbon material

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Experimental program
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Effect test

Embodiment 1

[0035] a. Synthesis of filling materials

[0036] Dissolve 1 g of bipyridine in 20 mL of absolute ethanol, and after it is completely dissolved, add 0.2018 g of cobalt chloride to the solution to form a metal complex. Then add 0.2g of two-dimensional hard template mesoporous silica SBA-15, and continue to stir until dry; then, dry at a constant temperature at 60°C to obtain the filling material;

[0037] b. High temperature roasting of filling materials

[0038] Place the obtained filling material in a quartz tube, heat it at 500°C and 30ml / min pure nitrogen atmosphere, and keep it for 2 hours to carbonize the filling material to obtain a black powder;

[0039] c. Removal of hard template mesoporous silica

[0040] The black powder prepared above was stirred with 20% hydrofluoric acid solution for 8 hours, washed with deionized water at 60° C., and dried to obtain the ordered mesoporous non-noble metal-nitrogen-graphitized carbon material. The dosage ratio of black powder ...

Embodiment 2

[0042] a. Synthesis of filling materials

[0043] Dissolve 1 g of bipyridine in 20 mL of absolute ethanol, and after it is completely dissolved, add 0.2771 g of cobalt chloride to the solution to form a metal complex. Then add 0.4g of two-dimensional hard template mesoporous silica SBA-15, and continue to stir until dry; then, dry at a constant temperature at 60°C to obtain the filling material;

[0044] b. High temperature roasting of filling materials

[0045]Place the obtained filling material in a quartz tube, heat it at 600°C in a 30ml / min pure nitrogen atmosphere, and keep it for 3 hours to carbonize the filling material to obtain a black powder;

[0046] c. Removal of hard template mesoporous silica

[0047] The black powder prepared above was stirred with 20% hydrofluoric acid solution for 9 hours, washed with deionized water at 60° C., and dried to obtain the ordered mesoporous non-noble metal-nitrogen-graphitized carbon material. The dosage ratio of black powder ...

Embodiment 3

[0049] a. Synthesis of filling materials

[0050] Dissolve 1 g of bipyridine in 20 mL of absolute ethanol, and after it is completely dissolved, add 0.8313 g of cobalt chloride to the solution to form a metal complex. Then add 0.5g of three-dimensional hard template mesoporous silica KIT-6, and continue to stir until dry; then, dry at a constant temperature at 60°C to obtain the filling material;

[0051] b. High temperature roasting of filling materials

[0052] The obtained filling material was placed in a quartz tube, heated at 900°C and 30ml / min pure nitrogen atmosphere, and kept for 5 hours to carbonize the filling material to obtain a black powder;

[0053] c. Removal of hard template mesoporous silica

[0054] The black powder prepared above was stirred with 20% hydrofluoric acid solution for 10 h, washed with deionized water at 60° C., and dried to obtain the ordered mesoporous non-noble metal-nitrogen-graphitized carbon material. The dosage ratio of black powder to...

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Abstract

The invention discloses a preparation method of an ordered mesoporous non-noble metal-nitrogen-graphitized carbon material. According to the method, mesoporous silica is used as a hard template, nitrogen-containing organic small molecule is used as a precursor, and the ordered mesoporous non-noble metal-nitrogen-graphitized carbon material is prepared by nanometre pouring and high-temperature roasting on the hard template. The material obtained by the method disclosed by the invention keeps a large specific surface area and a good dispersibility while having a high nitrogen density; and moreover, the pore diameter is adjustable, and the regular pore channel structure is beneficial to material transmission in an electrode, and the catalytic active site density is greatly increased. Compared with the traditional fuel cell cathode material, the obtained material is good in catalytic performance, low in cost, good in stability, free from the cross effect of a direct methanol fuel cell, and good in commercial application prospect.

Description

technical field [0001] The invention relates to the synthesis technology of mesoporous materials prepared by a hard template method and the field of electrocatalysts for fuel cells; specifically, a method for preparing ordered mesoporous non-noble metal-nitrogen-graphitized carbon materials using nitrogen-containing organic small molecules as precursors ; The prepared material has high electrocatalytic activity for oxygen reduction reaction, and is mainly used in the cathode part of the fuel cell. Background technique [0002] In order to solve the growing contradiction between economic development, energy shortage and environmental pollution, it has become a very urgent task to develop clean, efficient and sustainable new energy power technology. Fuel cell is such a very competitive new energy power technology in the 21st century. Among them, the proton exchange membrane fuel cell has attracted special attention because of its wide application prospects in portable power s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75B01J23/06B01J23/34B01J23/745B01J23/26B01J23/72B01J23/755
Inventor 单永奎朱小方孔爱国
Owner EAST CHINA NORMAL UNIV
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