Preparation method of nickel-iron hydrotalcite water-oxidation electrode loaded on nitrogen-doped graphite foam

A graphite foam, nickel molten iron technology, applied in electrodes, electrode shape/type, electrolysis process, etc., can solve the problems of poor controllability of oxygen evolution reaction, inability to prepare large-area working electrodes, etc., to achieve mass production and save reactions Preparation cost, good flexibility

Active Publication Date: 2018-10-16
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing nickel-iron hydrotalcite water oxidation electrode supported on azagraphite foam, which mainly solves the poor controllability of the oxygen evolution reaction existing in the prior art, and the prepared compound is usually a powder, It can only be loaded on glassy carbon electrodes, and cannot prepare large-area working electrodes

Method used

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  • Preparation method of nickel-iron hydrotalcite water-oxidation electrode loaded on nitrogen-doped graphite foam
  • Preparation method of nickel-iron hydrotalcite water-oxidation electrode loaded on nitrogen-doped graphite foam
  • Preparation method of nickel-iron hydrotalcite water-oxidation electrode loaded on nitrogen-doped graphite foam

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preparation example Construction

[0021] A preparation method of nickel-iron hydrotalcite water oxidation electrode supported on nitrogen-assorted graphite foam, comprising the steps of:

[0022] (S1) placing the required graphite foil in a mixed solution of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1, and oxidizing at room temperature for 2-12 hours to obtain a loose and porous graphite oxide foil;

[0023] (S2) placing the graphite oxide foil in deionized water, and dialyzing to remove acidic substances and small molecular organics remaining on the graphite oxide foil;

[0024] (S3) Put the graphite oxide foil cleaned in (S2) in a hydrothermal kettle, add urea with a concentration of 0.1-2mol / L, and soluble divalent nickel salt nickel sulfate and nitric acid with a concentration of 10-200mmol / L Nickel or nickel chloride, a mixed solution of soluble ferric salt ferric sulfate, ferric nitrate or ferric chloride with a concentration of 2-100mmol / L, and hydrothermal reactio...

Embodiment 1

[0028] Cut the 200μm thick graphite foil into 4×2cm, and oxidize it in the mixed acid system of concentrated sulfuric acid:concentrated nitric acid=3:1 at room temperature for 6h to obtain graphite oxide foil, and dialyze the prepared graphite oxide foil in deionized water to remove the residual acidic substances and small molecular organic matter, put graphite oxide foil in a hydrothermal kettle, add 0.2mol / L urea, 20mmol / L soluble nickel salt, 5mmol / L soluble iron salt mixed solution, and react under 180°C for 12 hours. After washing with deionized water and dialysis, a nickel-iron hydrotalcite water oxidation electrode with the same size as graphite foil and uniformly loaded on azagraphite foam was obtained.

[0029] Depend on figure 2 In (a, b), it can be seen that the surface of the nitrogen graphite foam still maintains the wrinkled structure of the graphite surface after the hydrothermal reaction, and the size distribution of the nickel-iron hydrotalcite nanostructure ...

Embodiment 2

[0031] Cut the 500 μm thick graphite foil into 2×1cm, oxidize it in the mixed acid system of concentrated sulfuric acid:concentrated nitric acid=3:1 for 12h at room temperature to obtain graphite oxide foil, place the prepared graphite oxide foil in deionized water and dialyze to remove residual acidic substances and For small molecular organic matter, put the obtained graphite oxide foil in a hydrothermal kettle, add a mixed solution of 0.4mol / L urea, 40mmol / L soluble nickel salt, and 10mmol / L soluble iron salt, and conduct a hydrothermal reaction at 180°C for 12h , after cleaning and dialysis with deionized water, a nickel-iron hydrotalcite water oxidation electrode with the same size as graphite foil and uniformly loaded on azagraphite foam was obtained.

[0032] Depend on figure 2 (c, d) It can be seen that after increasing the concentration of nickel salt and iron salt, the surface wrinkle structure of azagraphite foam remains unchanged, and the nanostructure size of nic...

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Abstract

The invention discloses a preparation method of a nickel-iron hydrotalcite water-oxidation electrode loaded on nitrogen-doped graphite foam. The method comprises the following steps that needed graphite foil is placed into a mixed solution, wherein the volume ratio of concentrated sulfuric acid to concentrated nitric acid in the mixed solution is 3:1, oxidizing is carried out at room temperature for 2-12 hours, obtained graphite oxide foil is taken out and is placed in deionized water, and dialysis is carried out to remove acidic substances and small-molecule organic matter remaining on the graphite oxide foil; and then the graphite oxide foil is placed in a hydrothermal kettle, a mixed solution of urea, soluble bivalent nickel salt and trivalent ferric salt is added into the kettle, furthermore, hydrothermal reaction is carried out under the condition of 120-180 DEG C for 6-12 hours, an obtained composite material is washed by using the deionized water, residual salt is removed through dialysis, and then the nickel-iron hydrotalcite water-oxidation electrode loaded on the nitrogen-doped graphite foam is obtained. According to the scheme, the purpose of obtaining the self-supporting electrode with the uniformly-dispersed hydrotalcite structure is achieved, and high practical value and popularization value are achieved.

Description

technical field [0001] The invention belongs to the technical field of nanocomposite materials, and in particular relates to a method for preparing a nickel-iron hydrotalcite water oxidation electrode loaded on nitrogen-assorted graphite foam. Background technique [0002] Oxygen evolution reaction catalysis is the bottleneck that restricts water electrolysis to obtain hydrogen energy and related energy systems. Studies have shown that noble metal catalysts such as IrO2 and RuO2 have excellent catalytic activity, but their practical application is limited by expensive price and low catalytic stability. Transition metal catalysts, especially nickel-iron hydrotalcite (NiFe LDH) have attracted extensive attention of researchers due to their high catalytic activity, high stability and low cost. Just like the Chinese patent, the application number is 201610565736.2, which is an iron oxyhydroxide-nickel-iron hydrotalcite integrated oxygen evolution electrode and its preparation a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/04C25B11/06C25B11/12C25B11/03
CPCC25B1/04C25B11/031C25B11/051C25B11/069C25B11/075Y02E60/36
Inventor 李瑞徐劲松把静文闫霞艳巫泉文唐涛
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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