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A kind of thin film electrocatalyst with transition metal core-shell structure and preparation method thereof

A transition metal, core-shell structure technology, applied in structural parts, electrochemical generators, circuits, etc., can solve the problems of multiple by-products, high preparation temperature, unsuitable for large-scale industrial production, etc., to achieve increased surface area, high catalysis Performance, low cost effect

Active Publication Date: 2020-01-07
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method usually requires a higher preparation temperature (>900°C), and introduces more by-products at the same time, and is not suitable for mass industrial production

Method used

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  • A kind of thin film electrocatalyst with transition metal core-shell structure and preparation method thereof
  • A kind of thin film electrocatalyst with transition metal core-shell structure and preparation method thereof
  • A kind of thin film electrocatalyst with transition metal core-shell structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0034] 1) Clean and dry the substrate; specifically, soak the substrate in HF acid solution (concentration 1%) for 5-15 minutes to remove surface oxides; then place the substrate in acetone solution for ultrasonic cleaning for 10-30 minutes , remove the oil on the surface of the substrate; then put the substrate in alcohol and ultrasonically clean it for 10-30 minutes to remove the organic matter on the surface of the substrate; finally, ultrasonically clean the substrate in deionized water for 10-30 minutes, take it out and put it in a drying box Dry at 30-50°C for 1-2 hours.

[0035] 2) Using magnetron sputtering equipment, put the cleaned and dried substrate into the vacuum chamber of the magnetron sputtering device, adjust the deposition angle to 45°, and the distance between the target and the substrate to be 100mm. The body is evacuated to 5×10 -4 Below Pa.

[0036] 3) Preset the substrate temperature to 250°C; after the substrate temperature rises to the preset temper...

Embodiment example 2

[0040] The substrate temperature in step 3) of Embodiment 1 is preset to 450° C., and the rest of the steps are the same as Embodiment 1. Under this condition, no core-shell structure was formed, and the Figure 6 It can be seen that the half-wave potential and initial potential obtained by the test are respectively -0.5V and -0.18V, and the electron transfer number is 3.59.

[0041] The above examples 1-2 are negative examples, because the pre-set temperature of the substrate is unreasonable, finally no sample with core-shell structure was obtained. The oxygen reduction catalytic performance of the product is poor

Embodiment example 3

[0043] The substrate temperature in step 3) of Embodiment 1 is preset as 650° C., and the rest of the steps are the same as Embodiment 1. Transmission electron microscopy of the resulting product was as image 3 shown by image 3It can be seen that the Cu@N-C core-shell structure film catalyst was prepared under the conditions of this example, the size of the metal core was 5-15 nm, the number of graphite shell layers was 3-5 layers, and the atomic percentage contents of Cu, C, and N elements were respectively: 22.81at%, 71.21at%, 5.98at%, and the film thickness of the thin film catalyst is 600nm.

[0044] The linear sweep voltammogram of the sample prepared in this embodiment to the oxygen reduction reaction is as follows Figure 6 shown by Figure 6 It can be seen that the half-wave potential and initial potential obtained by the test are -0.24V and -0.06V, respectively, which are close to -0.17V and -0.06V of the commercial Pt / C catalyst. The electron transfer number is...

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Abstract

The invention relates to an electrocatalyst for a transition metal core-shell structure film and preparation method thereof, and belongs to the field of the preparation of catalyst materials. The filmtakes a metal nanometer particle as a core, and nitrogen-doped onion-shaped graphite as a shell, and the thickness of the film formed by the nanometer particle adopting a core-shell structure on a substrate is 200 to 1200nm. According to the method, a magnetron sputtering small angle deposition technology is adopted, a metal target is taken as a metal nanometer particle source, a graphite targetor methane gas is taken as a carbon source, nitrogen is taken as nitrogen source gas, and meanwhile argon is led, so as be taken as sputtering gas, so that the fact that metal catalyzes the graphitization growth and in-situ self-assembly of carbon to form a nitrogen-doped onion-shaped graphite packed metal nanometer particle film is realized. The electrocatalyst has the advantages of simple technology, low cost, high repeatability, high yield and capability of realizing mass industrial production; no by-products exist during the preparation, and a formed sample presents stability and methanoltolerant property superior to that of commercial Pt / C catalysts.

Description

technical field [0001] The invention belongs to the field of preparation of catalyst materials, in particular to a thin film electrocatalyst with a transition metal core-shell structure, and a low-cost, simple process, high yield and repeatable magnetron sputtering method for preparing the transition metal core-shell structure thin film electrocatalyst Methods. Background technique [0002] At present, due to the increasingly serious energy and environmental problems, fuel cells with advantages such as high energy conversion efficiency and low environmental pollution have received extensive attention. However, the oxygen reduction reaction process at the cathode is complex and the reaction kinetics are slow, requiring catalysts to catalyze the reaction. Platinum-based catalysts have long been considered as catalysts with good performance, but their limited resources and high prices severely limit the commercialization of fuel cells. Therefore, it is urgent to find non-prec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/86H01M4/88H01M4/90H01M8/1011
CPCY02E60/50Y02P70/50
Inventor 文懋邵洪洋张侃郑伟涛任萍
Owner JILIN UNIV
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