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Method for preparing Ni-Mo-P nano alloy film electrode through ionic liquid electro-deposition

A nano-alloy, thin-film electrode technology, applied in electrodes, electrolysis process, electrolysis components, etc., can solve the problems of high hydrogen-induced defects in the coating layer, significant hydrogen evolution catalytic activity, unstable plating solution composition, etc., and achieve good surface morphology and interface. The effect of bonding force, excellent hydrogen evolution catalytic activity, and good interfacial bonding force

Active Publication Date: 2021-09-24
SUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve a series of problems such as the unstable composition of the plating solution, low deposition efficiency of the coating, high hydrogen-induced defects of the coating, and coarse structure in the preparation of Ni-Mo-P alloys by electrodeposition of traditional water-solvent electrolytes. A method for preparing Ni-Mo-P nano-alloy thin-film electrodes by solvent electrodeposition. The ionic liquid involved in the method is environmentally friendly, non-toxic, has a wide electrochemical window, and the obtained coating has a fine crystal structure and remarkable hydrogen evolution catalytic activity.

Method used

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  • Method for preparing Ni-Mo-P nano alloy film electrode through ionic liquid electro-deposition
  • Method for preparing Ni-Mo-P nano alloy film electrode through ionic liquid electro-deposition
  • Method for preparing Ni-Mo-P nano alloy film electrode through ionic liquid electro-deposition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of ionic liquid solvent: heat and mix dried choline chloride and ethylene glycol at 60°C in a molar ratio of 1:2 to obtain a colorless and transparent liquid, which is an ionic liquid;

[0028] (2) Preparation of ion plating solution: Take 50mL of the above-mentioned ionic liquid, add 0.05g of C 6 h 8 o 7 .H 2 O, stirred at 70°C for 20min, then 0.3g of (NH 4 ) 6 Mo 7 o 24 .4H 2 O was added into the above solution three times (0.1g each time, with an interval of 20 minutes), and continued to stir at 70°C for 40 minutes to form a light yellow solution, and then 0.6g of NaH 2 PO 2 .H 2 O continued to be added to the above mixed solution, stirred at 70°C for 30min to form a mixed solution without precipitation, and finally 8.06g of NiCl 2 .6H 2 O was added to the above mixed solution and continued to stir at 70°C for 1 hour to form a uniform, dark green solution without precipitation. In this plating solution, Ni 2+ :Mo 6+ is 20:1, Ni 2+ :HPO 2 ...

Embodiment 2

[0033] (1) The preparation of the ionic liquid solvent is the same as in Example 1;

[0034] (2) The preparation process of ion plating solution is the same as embodiment 1;

[0035] (3) Preparation of Ni-Mo-P nano-alloy thin film electrodes by electrodeposition is the same as in Example 1, except that the current density during electrodeposition is 30 mA / cm 2 ;

[0036] (4) Cleaning and drying of the Ni-Mo-P nano-alloy thin film electrodes are the same as in Example 1.

[0037] The surface of the Ni-Mo-P nano-alloy thin-film electrode obtained in Example 2 is still relatively smooth, the particle diameter slightly increases to 50-150nm, the Mo content in the alloy increases significantly to 11.2 wt%, and the P content changes little to 9.1 wt%, the phase composition is the same as in Example 1.

Embodiment 3

[0039] (1) The preparation of the ionic liquid solvent is the same as in Example 1;

[0040] (2) The preparation process of the ion plating solution is the same as in Example 1, except that the added C 6 h 8 o 7 .H 2 O is 0.1g, (NH 4 ) 6 Mo 7 o 24 .4H 2 O is 0.6g (3 times, 0.2g each time, with an interval of 20 minutes); in this plating solution, Ni 2+ :Mo 6+ is 10:1, Ni 2+ :HPO 2 - is 6:1;

[0041] (3) Preparation of Ni-Mo-P nano-alloy thin film electrode by electrodeposition is the same as in Example 2;

[0042] (4) Cleaning and drying of the Ni-Mo-P nano-alloy thin film electrodes are the same as in Example 1.

[0043] figure 2 (B) and image 3 (B) shows the phase analysis and microscopic morphology of the Ni-Mo-P nano-alloy thin film electrode obtained under the conditions of Example 3. From figure 2 (B) It can be seen that Ni begins to appear in the nanoalloy film 4 No trace of P element was found in the Mo diffraction peak, indicating that the Ni-Mo-...

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Abstract

The invention relates to a method for preparing a Ni-Mo-P nano alloy film electrode by utilizing ionic liquid electro-deposition. The method successfully solves the problems of low current efficiency, high waste liquid yield, coarse film tissue, high hydrogen-induced defects and the like in the traditional method for preparing a nickel-based alloy film electrode by utilizing aqueous solution electrodeposition. The method for preparing the Ni-Mo-P nano alloy film electrode through ionic liquid electro-deposition comprises the following steps that a phosphate, citric acid, a molybdenum salt and a nickel salt are added into an ionic solvent formed by mixing choline chloride and ethylene glycol, and an ionic plating solution is obtained; a brass sheet is used as a substrate, the Ni-Mo-P nano-alloy film electrode is prepared on the brass sheet in an electro-deposition mode through a constant current method, wherein the phosphate is NaH2PO2, the molybdenum salt is (NH4) 6Mo7O24, the nickel salt is NiCl2, and the temperature of a plating solution is 60-80 DEG C, the current density is 5-50 mA / cm < 2 >, and the electro-deposition time is 3-7 min. The Ni-Mo-P alloy film electrode prepared by the preparation method disclosed by the invention has good hydrogen evolution catalytic performance (eta 200 is equal to 169mV, and b is equal to 51.2 mV / dec).

Description

technical field [0001] The invention relates to a method for preparing a ternary nano-alloy thin film by ionic liquid electrodeposition, in particular to a method for preparing a Ni-Mo-P nano-alloy thin film electrode by using ionic liquid electrodeposition. Background technique [0002] Hydrogen production by electrolysis of water is one of the most popular hydrogen production technologies at present, but because the potential of the cathode hydrogen evolution electrode is higher than the theoretical potential, the energy consumption of hydrogen production by electrolysis of water is relatively high. The precious metals Pt, Ru and their alloys can accelerate the hydrogen evolution reaction, but because of limited reserves and high prices, they cannot be popularized and applied. Therefore, the development of low-cost, high-performance hydrogen evolution electrode catalytic materials is of great significance to the electrolysis of water for the hydrogen production industry. ....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/04C25B11/061C25B11/091
CPCC25B1/04C25B11/061C25B11/091Y02E60/36
Inventor 王慧华李林王德永屈天鹏徐英君胡绍岩田俊候栋
Owner SUZHOU UNIV
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