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Preparation method and application of carbon-based non-noble metal oxygen reduction catalyst

A non-precious metal and catalyst technology, applied in the field of electrocatalysis, carbon-based non-precious metal oxygen reduction catalyst and its preparation, can solve the problems of numerous experimental condition variables, rigid control of effective iron content, complex and time-consuming multi-factor process, etc. Accelerates kinetic processes, facilitates diffusion and fast transport, achieves uniform dispersion and stable loading

Active Publication Date: 2020-01-17
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are various synthesis methods for Fe / N-C catalysts, such as direct pyrolysis of macrocyclic iron compounds and organometallic framework complexes. This method has high synthesis efficiency and stable structure, but due to its precursor Fe / N coordination structure And the ratio has been fixed, the control of the content of effective iron is relatively rigid
It is also possible to use the one-pot pyrolysis method of small molecular iron compounds and nitrogen-containing compounds. This method has a wide range of sources of precursor materials, and the structure design is more flexible and diverse, which can increase the loading of effective iron. However, there are many variables in the experimental conditions and many adjustments. Factor process is complex and time-consuming

Method used

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  • Preparation method and application of carbon-based non-noble metal oxygen reduction catalyst
  • Preparation method and application of carbon-based non-noble metal oxygen reduction catalyst
  • Preparation method and application of carbon-based non-noble metal oxygen reduction catalyst

Examples

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Embodiment 1

[0021] Example 1: Preparation of polypyrrole doped with sodium ferrocyanide: 0.024mol (11.626g) sodium ferrocyanide decahydrate, 0.016mol (3.648g) ammonium persulfate and 200mL distilled water were added under nitrogen protection In a 500ml three-necked flask, keep the temperature of the system at 0°C and a fixed stirring speed in a refrigerator to dissolve for 10 minutes, dissolve 0.012mol (840μL) of pyrrole in 50mL of absolute ethanol, transfer to the separatory funnel and slowly drop into the three-necked flask , after continuous stirring for 6 hours, the black product was obtained for suction filtration, and washed with distilled water several times during the process, and dried in a vacuum oven at 60°C for 24 hours to obtain sodium ferrocyanide-doped polypyrrole. figure 1 Scanning electron micrographs of polypyrrole.

Embodiment 2

[0022] Example 2: Preparation of carbon-based oxygen reduction catalyst: Take 100 mg of sodium ferrocyanide-doped polypyrrole and 300 mg of sublimed sulfur, use an appropriate amount of absolute ethanol as a wetting agent, grind and mix them in a mortar until uniform. Then put the obtained product in a clean porcelain boat and put it into a high-temperature tube furnace. Under the protection of nitrogen, the temperature was first programmed to rise to 900 °C at 5 °C / min and maintained for 2 hours, and then the temperature was programmatically lowered to 25 °C at 10 °C / min. ℃, the doped carbon material was obtained, named as Fe / 3S / N-C, figure 2 Scanning electron micrographs of the corresponding carbon materials.

Embodiment 3

[0023] Example 3: Production of an oxygen reduction working electrode: Disperse 5 mg of the above-mentioned synthesized sample in 800 microliters of Nafion isopropanol solution with a volume fraction of 3%, and disperse the material evenly by ultrasonic waves, and take 10 microliters dropwise in the The dried rotating disc electrode (diameter 5mm), after natural drying, was used to test the electrochemical catalytic performance of the sample. image 3 It is the cyclic voltammetry curve of the oxygen reduction catalyst obtained in this embodiment, in saturated N 2 Under the 0.1M KOH electrolyte solution, the cyclic voltammogram in the voltage range of 0.2-1.0V is similar to a rectangle, and there is no obvious reduction peak. Relatively speaking, at saturation O 2 Under the 0.1M KOH electrolyte solution, there is an obvious characteristic peak of oxygen reduction reaction (ORR), indicating that this material has significant electrocatalytic activity for oxygen reduction reacti...

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Abstract

The invention belongs to the field of energy materials, particularly relates to a carbon-based non-noble metal oxygen reduction catalyst and a preparation method thereof, and further relates to an electrocatalytic application of the catalyst in a cathode oxygen reduction reaction of a fuel cell. The method has the following steps: forming Ferrous cyanide doped polypyrrole by adopting an anion doping method, adding sublimed sulfur in the pyrolysis process, further introducing heteroatomic sulfur, and forming the sulfur and nitrogen co-doped carbon-based non-noble metal oxygen reduction catalyst. The oxygen reduction catalyst shows efficient oxygen reduction electrochemical performance and stability, preferably, the half-wave potential of the oxygen reduction electrochemical reaction of theoxygen reduction catalyst is (0.89 V vs.RHE) and is superior to that of commercial platinum carbon (0.84 V vs.RHE), and the electrochemical stability of the oxygen reduction catalyst is greatly superior to that of the commercial platinum carbon; the maximum output power of the assembled zinc-air battery is 94 mW / cm < 2 > and is superior to 20 wt% of commercial platinum carbon (the maximum output power is 78 mW / cm < 2 >).

Description

technical field [0001] The invention belongs to the field of energy materials, and in particular relates to a carbon-based non-noble metal oxygen reduction catalyst and a preparation method thereof, and also relates to the electrocatalytic application of the catalyst in the oxygen reduction reaction of a fuel cell cathode. Background technique [0002] With the rapid consumption of traditional fossil fuels, it becomes more urgent to explore clean and renewable energy technologies to solve the problems of energy shortage and environmental pollution. Among all energy storage and conversion systems, fuel cells are known as "green energy for the 21st century" due to their advantages such as high energy density, light weight, abundant material sources, and no pollution. The anode of the fuel cell mainly undergoes the oxidation reaction of hydrogen (H 2 →2H + +2e － ,HOR), the reaction is relatively simple, is a fast kinetic process; the cathode mainly occurs the reduction react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M12/06H01M12/08
CPCH01M4/9041H01M4/9083H01M12/06H01M12/08Y02E60/10
Inventor 肖作旭陈艳丽游国强
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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