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Preparation method of transition metal/nitrogen-doped carbon fiber electrocatalyst

A nitrogen-doped carbon fiber and electrocatalyst technology, applied in circuits, electrical components, battery electrodes, etc., can solve problems affecting oxygen reduction performance, unfavorable exposure of electrocatalytic active sites, etc., achieve excellent electrocatalytic performance and inhibit agglomeration Effect

Active Publication Date: 2019-07-30
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, after heat treatment, the size of transition metal nanoparticles is generally as high as 10–50 nm, or even larger, which is not conducive to the exposure of electrocatalytic active sites, thereby affecting its oxygen reduction performance.

Method used

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  • Preparation method of transition metal/nitrogen-doped carbon fiber electrocatalyst
  • Preparation method of transition metal/nitrogen-doped carbon fiber electrocatalyst
  • Preparation method of transition metal/nitrogen-doped carbon fiber electrocatalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 20mL of hydrochloric acid (HCl) to 220mL of ultrapure water, and add 0.8g of cetyltrimethylammonium bromide ((C 16 -H 33 )-N(CH 3 ) 3 Br), evenly and continuously stirred for a period of time to obtain a milky white liquid; 1.2g ammonium persulfate ((NH 4 ) 2 S 2 o 8 ) and 1.6mL pyrrole (C 4 h 5 N) Add the milky white solution, continue to stir for 3 hours, filter, wash and dry to obtain the carbon-based precursor black powder polypyrrole; put a certain amount of polypyrrole into the corundum boat 1 and place it in the center of the tube furnace. Cobalt chloride hexahydrate (CoCl 2 ·6H 2 O) Placed in corundum boat 2, placed 1cm away from No. 1 corundum boat, and then placed in a high-purity Ar atmosphere furnace 900 o C lower tube furnace heating rate 10 o C / min, annealing treatment for 2.5h, black powder Co / N-CF electrocatalyst was obtained.

[0026] figure 1 (a) is the SEM picture of the polypyrrole prepared in this example. It can be seen from the pi...

Embodiment 2

[0028] Add 80mL of hydrochloric acid (HCl) to 220mL of ultrapure water, and add 0.8g of hexadecyltrimethylammonium bromide ((C 16 -H 33 )-N(CH 3 ) 3 Br), evenly and continuously stirred for a period of time to obtain a milky white liquid; 1.2g ammonium persulfate ((NH 4 ) 2 S 2 o 8 ) and 1.6mL pyrrole (C 4 h 5 N) Add the milky white solution, continue to stir for 3 hours, filter, wash and dry to obtain the carbon-based precursor black powder polypyrrole; put a certain amount of polypyrrole into the corundum boat 1 and place it in the center of the tube furnace. Cobalt chloride hexahydrate (CoCl 2 ·6H 2 O) placed in corundum boat 2, placed 1cm away from No. 1 corundum boat, and then placed in a high-purity Ar atmosphere furnace at 800 o C lower tube furnace heating rate 10 o C / min, annealing treatment for 2.5h, black powder Co / N-CF electrocatalyst was obtained.

[0029] Figure 1(b) is the SEM image of polypyrrole prepared in this example, it can be seen from the fig...

Embodiment 3

[0034] Add 80mL of hydrochloric acid (HCl) to 220mL of ultrapure water, and add 0.8g of hexadecyltrimethylammonium bromide ((C 16 -H 33 )-N(CH 3 ) 3 Br), evenly and continuously stirred for a period of time to obtain a milky white liquid; 1.2g ammonium persulfate ((NH 4 ) 2 S 2 o 8 ) and 1.6mL pyrrole (C 4 h 5 N) Add the milky white solution, continue to stir for 3 hours, filter, wash and dry to obtain the carbon-based precursor black powder polypyrrole; put a certain amount of polypyrrole into the corundum boat 1 and place it in the center of the tube furnace. Cobalt chloride hexahydrate (CoCl 2 ·6H 2 O) placed in corundum boat 2, placed 1cm away from No. 1 corundum boat, and then placed in a high-purity Ar atmosphere furnace at 900 o C lower tube furnace heating rate 10 o C / min, annealing treatment for 2.5h, black powder Co / N-CF electrocatalyst was obtained.

[0035] image 3It is the TEM image of the Co / N-CF electrocatalyst prepared under this example, as can b...

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Abstract

The invention provides a preparation method of a transition metal / nitrogen-doped carbon fiber electrocatalyst. The preparation method comprises the following steps: adding hydrochloric acid into ultrapure water, adding cetyl trimethyl ammonium bromide under the condition of ice-water bath, and stirring to obtain milky white liquid; adding ammonium persulfate and pyrrole into the milky white liquid, continuously stirring, and performing suction filtration, washing and drying to obtain carbon-based precursor black powder polypyrrole; putting polypyrrole into a corundum boat, spreading, and thenputting in the center of a tubular furnace; and respectively placing cobalt chloride hexahydrate, copper chloride dihydrate, manganese chloride tetrahydrate, nickel chloride hexahydrate and ferric chloride hexahydrate in another corundum boat, placing the corundum boat in the upstream of a tubular furnace, and obtaining the transition metal / nitrogen-doped carbon fiber electrocatalyst in an inert atmosphere by a high-temperature gas-phase carbothermal reduction method. The catalyst has excellent oxygen reduction electrocatalytic activity. Compared with the prior art, the preparation method of the transition metal / nitrogen-doped carbon fiber electrocatalyst has the advantages of simple preparation process, good repeatability, good conductivity, high electrocatalytic activity and stability and the like.

Description

technical field [0001] The invention relates to a preparation method of a transition metal / nitrogen-doped carbon fiber electrocatalyst, belonging to the field of oxygen reduction applications. Background technique [0002] The development of cheap and efficient oxygen reduction reaction (ORR) catalysts is a key factor in solving next-generation energy conversion and storage devices (such as fuel cells, metal-air batteries, etc.). Zn-air batteries, which convert chemical energy in fuels into electrical energy through electrochemical reactions, have broad application prospects in stable power generation and transmission, and are expected to solve global energy supply and clean environment problems. At present, Pt-based materials are the most effective catalysts for oxygen reduction, but the high cost and scarcity of noble metal Pt, as well as the problem of methanol crossover, have prompted people to explore inexpensive, efficient, and durable non-noble metal catalysts and ach...

Claims

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Application Information

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IPC IPC(8): H01M4/90
CPCH01M4/9041H01M4/9083Y02E60/50
Inventor 孙盼盼张丹左壮田良愉孙小华黄妞
Owner CHINA THREE GORGES UNIV
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