Preparation method of few-layer transition metal oxyhydroxide electro-catalysis electrode with step/crack structure

A technology of transition metal and oxide electrolysis, which is applied in the direction of electrodes, electrolytic processes, electrolytic components, etc., can solve the problems of complex preparation methods, high costs, and long processes, and achieve simple processes, low cost, and small contact resistance.

Pending Publication Date: 2022-03-22
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of a few-layer transition metal oxyhydroxide electrocatalytic electrode with a step / crack structure. The preparation method is simple, easy to operate, suitable for large-scale industrial production, and can solve the existing preparation problems. The method has problems such as complex process, high cost, and long process, and can obtain an ultra-thin metal oxyhydroxide integrated electrode with abundant and high active sites and high stability

Method used

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  • Preparation method of few-layer transition metal oxyhydroxide electro-catalysis electrode with step/crack structure
  • Preparation method of few-layer transition metal oxyhydroxide electro-catalysis electrode with step/crack structure
  • Preparation method of few-layer transition metal oxyhydroxide electro-catalysis electrode with step/crack structure

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Embodiment 1

[0057] In this embodiment, the preparation of the Fe / Ni-based oxyhydroxide electrocatalyst of ultra-thin structure:

[0058] 1.11g ferrous sulfate heptahydrate and 2.1g nickel sulfate hexahydrate were dissolved in 50mL deionized water to configure mixed metal salt solution A, and 1.26g oxalic acid was dissolved in a mixed solution of 50mL absolute ethanol and deionized water (1 : 4), adjust the pH value to 5 with ammonia water, configure it as oxalic acid solution B, heat the oxalic acid solution B to the reaction temperature of 50 ° C, and ultrasonically clean the foamed nickel substrate (2 × 6cm 2 ) is fixed with clips, immersed in oxalic acid solution B, preheated for 5 to 10 minutes, poured in mixed metal salt solution A, reacted for 30 minutes, cooled naturally, taken out, rinsed and dried to obtain iron / nickel loaded with nickel foam Oxalate intermediate.

[0059] Electrochemical in situ conversion by cyclic voltammetry: using a three-electrode system, the iron / nickel o...

Embodiment 2

[0062] In this example, the preparation of the Co / Ni-based oxyhydroxide electrocatalyst electrode with ultra-thin structure:

[0063] Dissolve 1.4g of cobalt sulfate heptahydrate and 1.31g of nickel sulfate hexahydrate in 50mL of deionized water to configure mixed metal salt solution A. Dissolve 1.26g of oxalic acid in a mixed solution of 50mL of absolute ethanol and deionized water (1: 4), adjust the pH value to 6 with ammonia water, configure it as oxalic acid solution B, heat the oxalic acid solution B to the reaction temperature of 50 ° C, and ultrasonically clean the foamed nickel substrate (2 × 6cm 2 ) fixed with clips, immersed in oxalic acid solution B, preheated for 5 to 10 minutes, poured mixed metal salt solution A into oxalic acid solution B, reacted for 30 minutes, cooled naturally, took out the substrate, rinsed and dried, and obtained foam Nickel supported cobalt / nickel oxalate intermediate.

[0064] Electrochemical in situ conversion by cyclic voltammetry: usi...

Embodiment 3

[0067] In this example, the preparation of the Co / Fe-based oxyhydroxide electrocatalyst with ultra-thin structure:

[0068]1.4g cobalt sulfate heptahydrate and 1.36g ferrous sulfate heptahydrate were dissolved in 50mL deionized water to configure mixed metal salt solution A, and 1.26g oxalic acid was dissolved in a mixed solution of 50mL absolute ethanol and deionized water (1 : 4), adjust the pH value to 5 with ammonia water, configure it as oxalic acid solution B, heat the oxalic acid solution B to the reaction temperature of 50 ° C, and ultrasonically clean the foamed nickel substrate (2 × 6cm 2 ) is fixed with clips, immersed in oxalic acid solution B, preheated for 5 to 10 minutes, poured in mixed metal salt solution A, reacted for 30 minutes, cooled naturally, taken out, rinsed and dried to obtain foamed nickel-supported cobalt / iron Oxalate intermediate.

[0069] Electrochemical in situ conversion by cyclic voltammetry: using a three-electrode system, the cobalt / iron ox...

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Abstract

The invention relates to the field of nanomaterial technology and electrochemical energy conversion and storage, in particular to a preparation method of a few-layer transition metal oxyhydroxide electro-catalysis electrode with a step/crack structure. The method comprises the following steps: firstly, dissolving transition metal salt in deionized water to prepare a transition metal salt solution with a certain concentration; then, the metal-based electrode is placed in an oxalic acid solution, in the stirring process, the prepared metal salt solution is mixed in the oxalic acid solution, after a reaction is conducted for a period of time, hydrated metal oxalate is generated on the surface of the metal electrode in situ, and an electrode of an integrated structure is formed; and then, in an alkali solution with a certain concentration, electrochemical activation treatment is carried out, and the transition metal oxyhydroxide nanosheets are converted into few layers of transition metal oxyhydroxide nanosheets with rich steps and crack microstructures in an in-situ topology manner, so that the integrated composite electrode based on the metal current collector is formed. The method can be used for preparing the metal oxyhydroxide integrated electrode with different components, and the metal oxyhydroxide integrated electrode has excellent electro-catalysis water decomposition oxygen production activity.

Description

technical field [0001] The invention relates to the fields of nanometer material technology and electrochemical energy conversion and storage, in particular to a preparation method of a few-layer transition metal oxyhydroxide electrocatalytic electrode with a step / crack structure. Background technique [0002] With the rapid development of human society, the demand for energy is increasing day by day, and the massive consumption of traditional fossil energy has caused serious environmental pollution problems. Therefore, people's demand for renewable energy is increasingly urgent. As a clean energy with high energy density, hydrogen has good compatibility with the existing energy system and has no pollution during use. It is a clean energy carrier with great application potential. Using renewable energy (wind energy, solar energy, tidal energy, etc.) to generate electricity and electrolyze water to produce hydrogen is an ideal way to produce hydrogen in a green way. Renewabl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/031C25B11/061C25B11/095C25B1/04
CPCC25B11/031C25B11/061C25B11/095C25B1/04
Inventor 刘岗甄超贾春旭成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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