Three-dimensional porous Fe-N-C catalyst based on cetyl trimethyl ammonium bromide as carbon material pore-forming agent and preparation method

A hexadecyl trimethyl ammonium bromide, three-dimensional porous technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problem of high price, achieve increased contact area, good ORR catalytic performance, convenient and flexible adjustment Effect

Inactive Publication Date: 2017-04-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although soft template pore-making technology has been studied, the price of the template used for carbon material pore-making is too high, and the performance needs to be further improved. CTAB soft template is flexible and cheap, but it is used for carbon material pore-making Catalysts used in oxygen reduction reactions have not been reported yet

Method used

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  • Three-dimensional porous Fe-N-C catalyst based on cetyl trimethyl ammonium bromide as carbon material pore-forming agent and preparation method
  • Three-dimensional porous Fe-N-C catalyst based on cetyl trimethyl ammonium bromide as carbon material pore-forming agent and preparation method
  • Three-dimensional porous Fe-N-C catalyst based on cetyl trimethyl ammonium bromide as carbon material pore-forming agent and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1: Fe-N-O-CTAB-SiO 2 -1:1:4-900°C (Fe: FeCl 3 ·6H 2 O, Fe-N-O-CTAB-SiO 2 -1:1:4-900℃ refers to o-methylaniline, CTAB, SiO in raw materials 2 The mass ratio is 1:1:4, and the calcination temperature is 900°C)

[0046] 2g SiO 2 Disperse in 10mL of phosphoric acid aqueous solution and place in an ice-water bath, add 500μL o-methylaniline and stir evenly, then add dropwise 2.5mL of 3.7mol L -1 FeCl 3 ·6H 2 O solution and 500 μL H 2 o 2 , add CTAB (concentration of CTAB reaches 80mmol L in the solution) after dropping -1 ) and stir evenly; after the solution turns dark green, transfer the solution to an autoclave for 10 hours of reaction, then move it into an air drying oven and dry it in an air atmosphere at 100°C for 12 hours to obtain a catalyst precursor; grind the precursor evenly and place it in a quartz In the boat, under the protection of nitrogen, at 3°C ​​min -1 After heating up to 550°C, keep the temperature for 4 hours, and then at 5°C min -1 ...

Embodiment 2

[0047] Example 2: Fe-N-O-CTAB-SiO 2 -2:1:8-900°C (Fe: FeCl 3 ·6H 2 O, Fe-N-O-CTAB-SiO 2 -2:1:8-900℃ refers to o-methylaniline, CTAB, SiO in raw materials 2 The mass ratio is 2:1:8, and the calcination temperature is 900°C)

[0048] 2g SiO 2 Disperse in 10mL of phosphoric acid aqueous solution and place in an ice-water bath, add 500μL o-methylaniline and stir evenly, then add dropwise 2.5mL of 3.7mol L -1 FeCl 3 ·6H 2 O solution and 500 μL H 2 o 2 , add CTAB (concentration of CTAB reaches 40mmol L in the solution) after dropping -1 ) and stir evenly; after the solution turns dark green, transfer the solution to an autoclave for 10 hours of reaction, then move it into an air drying oven and dry it in an air atmosphere at 100°C for 12 hours to obtain a catalyst precursor; grind the precursor evenly and place it in a quartz In the boat, under the protection of nitrogen, at 3°C ​​min -1 After heating up to 550°C, keep the temperature for 4 hours, and then at 5°C min -1 ...

Embodiment 3

[0049] Example 3: Fe-N-O-CTAB-SiO 2 -5:1:20-900°C (Fe: FeCl 3 ·6H 2 O, Fe-N-O-CTAB-SiO 2 -5:1:20-900℃ refers to o-methylaniline, CTAB, SiO in raw materials 2 The mass ratio is 5:1:20, and the calcination temperature is 900°C)

[0050] 2g SiO 2 Disperse in 10mL phosphoric acid aqueous solution and place it in an ice-water bath, then add 500μL o-toluidine to the solution and stir evenly, then add 2.5mL 3.7mol L -1 FeCl 3 ·6H 2 O solution and 500 μL H 2 o 2 , add CTAB (CTAB concentration reaches 16mmol L in the solution) after dropping -1) and stir evenly; after the solution turns dark green, transfer the solution to an autoclave for 10 hours of reaction, then move it into an air drying oven and dry it in an air atmosphere at 100°C for 12 hours to obtain a catalyst precursor; grind the precursor evenly and place it in a quartz In the boat, under the protection of nitrogen, at 3°C ​​min -1 After heating up to 550°C, keep the temperature for 4 hours, and then at 5°C min ...

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Abstract

The invention belongs to the field of fuel-cell catalysts, and relates to a three-dimensional porous Fe-N-C catalyst based on cetyl trimethyl ammonium bromide as a carbon material pore-forming agent and a preparation method. The three-dimensional porous Fe-N-C electrocatalyst is obtained through high-temperature calcination of o-toluidine as a C source and an N source, FeCl3.6H2O as a metal source, CTAB as a soft template and SiO2 as a hard template under an N2 atmosphere. In the preparation process, the size and the shape of a micelle can be accurately controlled through changing the concentration of the CTAB, a three-dimensional interconnected porous structure with a lot of active sites exposed on the surface can be finally formed after the templates are removed due to CTAB micelle decomposition after high-temperature calcination, the quantity of the active sites for catalytic oxygen reduction reaction is ensured, the mass transfer requirements can be met and improvement of the ORR activity of the catalyst is facilitated. Compared with a traditional Fe-N-C electrocatalyst, the three-dimensional porous Fe-N-C catalyst has the advantages that the three-dimensional porous structure of the catalyst is more beneficial to oxygen transfer and adsorption, the preparation process is flexible and controllable, the raw materials are cheap and available, massive production is facilitated and the three-dimensional porous Fe-N-C catalyst has relatively high practical value.

Description

technical field [0001] The invention belongs to the field of fuel cell catalysts, and relates to a method for preparing an electrocatalyst for oxygen reduction reaction at the cathode of a fuel cell, in particular to a three-dimensional porous material Fe-N-C electrocatalyst and a preparation method thereof. Background technique [0002] Fuel cells have attracted extensive attention from researchers due to their high energy conversion efficiency, environmental friendliness, abundant and easy-to-obtain fuels, and not being limited by the Carnot cycle. However, the current application of fuel cells still faces severe challenges, especially the slow kinetics of the cathode oxygen reduction reaction (ORR), which greatly limits the commercial application of fuel cells. At present, the catalyst with the best catalytic ORR performance is Pt-based catalysts, but Pt reserves are small, expensive, poor in stability and insufficient in methanol resistance. Therefore, it is necessary to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/88H01M4/90
CPCH01M4/88H01M4/90Y02E60/50
Inventor 李光兰袁丽芳陈雯雯刘彩娣程光春杨贝贝
Owner DALIAN UNIV OF TECH
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