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Preparation method of nickel nanowire array electrode and application of nickel nanowire array electrode as electrochemical oxygen evolution active material

A silicon nanowire array and array electrode technology, which is applied in the field of electrochemical oxygen evolution, can solve the problems of low catalytic activity and insufficient durability, and achieve the effects of simple preparation and modification methods, good OER activity, and easy operation

Pending Publication Date: 2021-05-07
BEIJING UNIV OF TECH
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Problems solved by technology

[0005] Combining the above status quo, the present invention aims at the problems of low catalytic activity and insufficient durability of Ni-based catalysts in the electrocatalytic OER process, and aims to improve the electrocatalytic OER performance by optimizing the composition and structure of Ni-based catalysts.

Method used

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  • Preparation method of nickel nanowire array electrode and application of nickel nanowire array electrode as electrochemical oxygen evolution active material
  • Preparation method of nickel nanowire array electrode and application of nickel nanowire array electrode as electrochemical oxygen evolution active material
  • Preparation method of nickel nanowire array electrode and application of nickel nanowire array electrode as electrochemical oxygen evolution active material

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Embodiment 1

[0025] Embodiment 1: the preparation of silicon template

[0026] The silicon nanowire array structure prepared by deep reactive ion etching (DRIE) was used as a template. In this work, a silicon wafer was used as the original material, and its detailed parameters are listed in Table 1:

[0027] Table 1 Detailed parameters of silicon wafer

[0028]

[0029] The experiment used a high-density plasma etching machine (IPC-multiplex) produced by Surface Technology Systems (STS) in the UK. The silicon wafer will be transferred to a chamber that maintains highly anisotropic etching. This etching process Based on successive passivation and etch cycles. In this experiment, 75 continuous etching cycles were used to obtain a silicon nanowire array structure with a depth of 20 μm. In each cycle, octafluorocyclobutane (C 4 f 8 ) gas for passivation treatment, the passivation time is 11s, and the flow rate is 85sccm; subsequently, in sulfur hexafluoride (SF 6 ) and O 2 Etching in ...

Embodiment 2

[0030] Embodiment 2: the preparation of Ni-NG electrode

[0031] In order to obtain a nickel nanowire array structure with a high surface area, nickel was deposited on the silicon template by electroplating. First, put the prepared silicon template into the platform groove made of polymethyl methacrylate (PMMA), then fix the silicon template with adhesive tape and connect it with copper wire as the cathode material; polypropylene (pp ) mesh-coated high-purity (99.99%) electrolytic nickel sheet is the anode material; the electrolyte is prepared with analytically pure grade chemical reagents and deionized water, and the composition of the electrolyte is nickel sulfamate (Ni(NH 2 SO 3 ) 2 4H 2 O), boric acid (H 3 BO 3 ) and sodium lauryl sulfate (NaC 12 h 25 SO 4 ), where Ni(NH 2 SO 3 ) 2 4H 2O provides nickel ions with a concentration of 120g / L, H 3 BO 3 The concentration is 30g / L, and 0.5g of NaC in powder form is added to each liter of electrolyte 12 h 25 SO 4...

Embodiment 3

[0037] Embodiment 3: the modification of Ni-NG electrode

[0038] In the electrocatalytic oxidation process, the electrocatalytic OER activity of Ni-NG is not high enough, and the introduction of transition metal atoms to modify the Ni-NG interface can significantly optimize its OER catalytic activity and durability. First, use ultrapure water to prepare concentrations of 0.5g / 100mLFeCl 3 , 0.5g / 100mL CoCl 2 , 0.5g / 100mL molybdic acid solution, take three Ni-NG electrodes with an area of ​​1cm×1cm and soak them in the prepared FeCl 3 、CoCl 2 , Molybdenum acid solution, soaking time is 30min, rinse gently with deionized water for 2-3min after soaking, then place the sample in an oven for drying treatment, and finally use a tube furnace to dry the obtained material in an Ar atmosphere Then, the temperature was increased from room temperature to 250 °C at a rate of 5 °C / min for calcination and maintained for 2 h, and finally Ni-NG-Fe, Ni-NG-Co, Ni-NG-Mo electrode materials wer...

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Abstract

The invention discloses a preparation method of a nickel nanowire array electrode and an application of the nickel nanowire array electrode as an electrochemical oxygen evolution active material, and relates to the field of electrochemical oxygen evolution. The method comprises the steps: firstly, preparing the nickel nanowire array electrode with a high specific surface area by combining a deep reactive ion etching technology and an electroplating method; secondly, modifying a nickel nanowire array electrode substrate with doped metal atoms (Fe, Co and Mo) capable of strengthening or exciting the catalytic activity of the nickel nanowire array electrode substrate to prepare various composite material electrocatalysts, and further strengthening the catalytic activity of the nickel nanowire array electrode; and finally, deeply characterizing the crystal microstructure of the obtained material and testing the electrocatalytic oxygen evolution performance of the material, thereby exploring the application of the nickel nanowire array electrode as the efficient electrochemical oxygen evolution active material. The nickel nanowire array electrode prepared by the method has a high specific surface area and an excellent response signal, and shows relatively good electrocatalytic oxygen evolution activity and stability, so that direct scientific basis and technical means are provided for designing and constructing a stable and efficient electrocatalytic oxygen evolution active material.

Description

technical field [0001] The invention relates to a method for preparing and modifying a nickel nanowire array (hereinafter referred to as Ni-NG) electrode, and applies the obtained Ni-NG electrode material to the field of electrocatalysis, especially to the field of electrochemical oxygen evolution. Background technique [0002] With the depletion of traditional fossil fuels and the increasingly serious environmental pollution problems, the development of cheap and efficient electrocatalytic oxygen evolution (OER) active materials is crucial for the development of electrochemical hydrogen production, CO 2 Clean energy technologies such as reduction are critical. Typically, noble metal-based materials, iridium oxide / ruthenium oxide (IrO 2 / RuO 2 ) is the most active OER catalyst. But large-scale deployment of these materials has been difficult due to their high cost and scarcity of resources. Therefore, many research efforts are devoted to the development of relatively ine...

Claims

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Application Information

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IPC IPC(8): C25B11/046C25B1/04C25D3/12C25D5/02C25D7/00
CPCC25B1/04C25D5/022C25D7/00C25D3/12Y02E60/36
Inventor 严勇刘春越刘浩岑
Owner BEIJING UNIV OF TECH
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