Preparation method of hierarchical pore high-entropy alloy water electrolysis catalyst

A high-entropy alloy, multi-level pore technology, applied in the electrolysis process, electrolysis components, non-precious metal oxide coating and other directions, to achieve a wide range, simple and convenient operation, improve the oxygen production performance and cycle stability of electrolyzed water.

Active Publication Date: 2021-07-02
UNIV OF SCI & TECH BEIJING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, high-entropy alloys with hierarchical porous structures appl

Method used

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  • Preparation method of hierarchical pore high-entropy alloy water electrolysis catalyst
  • Preparation method of hierarchical pore high-entropy alloy water electrolysis catalyst
  • Preparation method of hierarchical pore high-entropy alloy water electrolysis catalyst

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[0029] The invention discloses a method for preparing a multi-level porous high-entropy alloy electrolytic water catalyst. The preparation method uses the difference in mixing enthalpy between the molten metal and the pre-alloyed components to place the smelted high-entropy transition group pre-alloy in the molten melt In the metal M, the molten molten metal M selectively reacts with its phase containing elements whose mixing enthalpy is negative to form an alloy structure with M-rich and M-poor; finally remove the more active M-rich phase in the alloy, and the remaining The components form a homogeneous three-dimensional bicontinuous, hierarchical porous high-entropy alloy water electrolysis catalyst with the characteristic of hierarchical porous structure through diffusion. Specifically include the following steps:

[0030] S1) Select transition group metals according to the design composition, and obtain transition group high-entropy pre-alloyed ingots after smelting,

[0...

Embodiment 1

[0040] (1) FeCo 1.2 Cr 0.8 Ni 1.2 MnAl 0.8 As the nominal composition of pre-alloying, the pure elements required for pre-alloying (Fe>99.999wt%, Co>99.99wt%, Cr>99.999wt%, Ni>99.9wt%, Mn>99.99wt%, Al>99.99wt% ), converted into mass (10g) according to the percentage of alloy atoms and weighed respectively, and then placed in a high-vacuum electric arc furnace to vacuum the cavity to 10 -4 Below Mpa, and filled with high-purity argon (>99.9wt%).

[0041] (2) Use high vacuum arc melting equipment to match the FeCo 1.2 Cr 0.8 Ni 1.2 MnAl 0.8 The initial alloy constituent materials are melted. Such as figure 1 As shown, the precursor is composed of Al-Ni-rich bcc phase and Cr-Fe-Ni-rich fcc phase.

[0042] (3) Wire-cut the smelted pre-alloyed ingot to obtain thin slices of 10×10×1 mm, place the thin slices in molten magnesium, and cool to room temperature after fully reacting for 3 minutes. The Mg element combines with the rich Al-Ni phase to form the Mg-Al-Ni rich phas...

Embodiment 2

[0047] (1) with Fe 1.2 co 1.2 Cr 0.8 Ni 1.2 mn 0.8 Al 0.8 As the nominal composition of pre-alloying, the pure elements required for pre-alloying (Fe>99.999wt%, Co>99.99wt%, Cr>99.999wt%, Ni>99.9wt%, Mn>99.99wt%, Al>99.99wt% ), converted into mass (10g) according to the percentage of alloy atoms and weighed respectively, and then placed in a high-vacuum electric arc furnace to vacuum the cavity to 10 -4 Below Mpa, and filled with high-purity argon (>99.9wt%).

[0048] (2) Use high vacuum arc melting equipment to pair the prepared Fe 1.2 co 1.2 Cr 0.8 Ni 1.2 mn 0.8 Al 0.8 The initial alloy constituent materials are melted. Such as Figure 5 As shown, the precursor is composed of Al-Ni-rich bcc phase and Cr-Fe-Ni-rich fcc phase.

[0049] (3) Wire-cut the smelted pre-alloyed ingot to obtain thin slices of 10×10×1 mm, place the thin slices in molten magnesium, and cool to room temperature after fully reacting for 3 minutes. The Mg element combines with the rich Al-N...

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Abstract

The invention belongs to the technical field of electro-catalysis application, and relates to a preparation method of a hierarchical pore high-entropy alloy water electrolysis catalyst, which comprises the following steps of: by utilizing the difference of mixing enthalpy between melt metal and pre-alloy components, putting the smelted high-entropy pre-alloy into molten metal M, and selectively reacting the molten metal M with elements with negative mixing enthalpy in the pre-alloy to form M-rich and M-poor multi-phase structures; and selectively removing a relatively active M-rich phase in the alloy by utilizing an acidic solution, and diffusing the remaining components to form a three-dimensional bicontinuous high-entropy alloy with a hierarchical pore structure, wherein the size of macropores is 500 nanometers to 2 micrometers, and the size of micropores is 40-200 nanometers. According to the present invention, the cost is reduced, the water electrolysis oxygen production performance of the material can be substantially improved through the synergistic effect among the multi-principal element transition group metals and the hierarchical pore structure, the required overpotential at 10 mA cm <-2 > is 260-300 mV, and the potential industrial application value is great.

Description

Technical field: [0001] The invention belongs to the technical field of electrocatalytic application of multi-level porous high-entropy alloy electrode materials, and in particular relates to a preparation method of a multi-level high-entropy alloy electrolytic water catalyst. Background technique: [0002] With the development of industrial society, the social energy crisis and environmental problems are becoming more and more serious, and the acquisition technology of clean energy is becoming more and more important. As a recognized green and clean energy, hydrogen energy has the characteristics of high efficiency, no pollution, and easy storage and transportation. It is known as the most promising renewable energy in the 21st century and has attracted widespread attention from all over the world. Among various hydrogen production technologies, hydrogen production by electrolysis of water has the advantages of high product purity, simple process, green and recyclable, and ...

Claims

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Application Information

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IPC IPC(8): C25B11/046C25B11/031C22C30/00C22C30/06C22C30/02C22C1/02C23F1/44C25B1/04
CPCC25B11/04C22C30/00C22C30/06C22C30/02C22C1/02C23F1/44C25B1/04Y02E60/36
Inventor 刘雄军王晶李志斌高瑞樱王辉吴渊吕昭平
Owner UNIV OF SCI & TECH BEIJING
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