阅读说明：本技术 一种析氧电极材料的制备方法 (Preparation method of oxygen evolution electrode material ) 是由 孙蓉 康佳慧 盛家利 谢金麒 符显珠 于 2018-08-27 设计创作，主要内容包括：本发明实施例提供一种析氧电极材料的制备方法,涉及电池材料制备技术领域。其中,该方法包括：在泡沫铜上生长氢氧化铜/氧化铜纳米管活性材料,得到氢氧化铜/氧化亚铜纳米管活性材料,将氢氧化铜/氧化亚铜纳米管活性材料置于浓度为0.01～5mol/L的氯钯酸盐溶液中浸泡1～60min,干燥,得到氢氧化铜/氧化亚铜纳米管活性材料上负载有贵金属钯的析氧电极材料。该析氧电极材料可以促进活性物质与电解液的接触,增强了析氧催化剂的性能和稳定性。(The embodiment of the invention provides a preparation method of an oxygen evolution electrode material, and relates to the technical field of battery material preparation. Wherein, the method comprises the following steps: growing a copper hydroxide/copper oxide nanotube active material on the copper foam to obtain the copper hydroxide/cuprous oxide nanotube active material, soaking the copper hydroxide/cuprous oxide nanotube active material in a chloropalladate solution with the concentration of 0.01-5 mol/L for 1-60 min, and drying to obtain the oxygen evolution electrode material loaded with noble metal palladium on the copper hydroxide/cuprous oxide nanotube active material. The oxygen evolution electrode material can promote the contact of active substances and electrolyte, and enhance the performance and stability of the oxygen evolution catalyst.)

1. A method of preparing an oxygen evolving electrode material, the method comprising:

growing a copper hydroxide/copper oxide nanotube active material on the foamy copper to obtain the copper hydroxide/cuprous oxide nanotube active material;

and (3) placing the copper hydroxide/cuprous oxide nanotube active material in a chloropalladate solution with the concentration of 0.01-5 mol/L for soaking for 1-60 min, and drying to obtain the oxygen evolution electrode material loaded with noble metal palladium on the copper hydroxide/cuprous oxide nanotube active material.

2. The method of claim 1, wherein growing copper hydroxide/copper oxide nanotube active material on copper foam comprises:

soaking the foamy copper in an acid solution and water for 2-15 min in sequence;

then the copper foam is put into alkaline solution and (NH)₄)₂S₂O₈Soaking the copper hydroxide/cuprous oxide nanotube active material in the mixed solution for 10-50 min, taking out and drying when the foamy copper is changed from orange to blue, and obtaining the copper hydroxide/cuprous oxide nanotube active material, wherein the concentration of the alkaline solution is 0.1-6 mol/L, (NH)₄)₂S₂O₈The concentration of the solution is 0.05-0.8 mol/L.

3. The method of claim 1, wherein the alkaline solution is NaOH solution, KOH solution, or Na₂CO₃At least one of the solutions.

4. The method of claim 2, wherein the acidic solution is dilute hydrochloric acid or dilute sulfuric acid.

5. The method according to claim 2, wherein the concentration of the alkaline solution is 1 to 4 mol/L.

6. The method of claim 2, wherein (NH4)₂S₂O₈The concentration of the solution is 0.1-0.5 mol/L.

7. The method of claim 2, wherein the copper foam is in an alkaline solution and (NH4)₂S₂O₈Soaking the mixture in the solution for 20-40 min.

8. The method according to claim 1, wherein the chloropalladate solution is any one of a sodium chloropalladate solution, a potassium chloropalladate solution, or a magnesium chloropalladate solution.

9. The method according to claim 1 or 8, wherein the concentration of the chloropalladate solution is 0.1 to 0.5 mol/L.

10. An oxygen evolution electrode material, characterized in that it is produced by the method of any one of claims 1 to 8.

Technical Field

The invention belongs to the technical field of battery material preparation, and particularly relates to a preparation method of an oxygen evolution electrode material.

Background

At present, the environmental and energy problems are becoming more serious, and the development of renewable energy sources is imminent. The hydrogen energy is an environment-friendly energy storage material with high energy density and good stability, the obtaining way is simple and easy to obtain, and the hydrogen energy can be obtained by electric hydrolysis. Under general conditions, the electric energy is converted into hydrogen energy to be stored, and the problem that the photovoltaic system cannot obtain energy to be stored in rainy days or at night can be solved.

In the application of hydrogen energy, the hydrogen evolution half-reaction is greatly influenced by the oxygen evolution half-reaction, wherein the efficiency of hydrogen evolution is influenced because the oxygen evolution reaction is slower than the hydrogen evolution reaction. Generally, the oxygen evolution catalyst helps to increase the rate of the hydrogen evolution reaction. The traditional oxygen evolution catalyst is generally of a solid structure, has few active sites, large density and large active area, and has small catalytic action on oxygen evolution reaction. In addition, the commercially available high efficiency oxygen evolution catalyst is typically RuO₂Or IrO₂Active materials based on these are expensive. Third, in the preparation of conventional oxygen evolution catalytic electrodes, they are usually made by mixing with polymers, increasing the internal resistance of the electrode.

Due to the above drawbacks of the oxygen evolution catalyst and the electrode material, the application of hydrogen energy is limited.

Disclosure of Invention

The invention provides a preparation method of an oxygen evolution electrode material, aiming at solving the problem that the application of hydrogen energy is limited due to the defects of small catalytic action, high price and large internal resistance of the electrode material of an oxygen evolution catalyst.

The invention provides a preparation method of an oxygen evolution electrode material, which comprises the following steps:

growing a copper hydroxide/copper oxide nanotube active material on the foamy copper to obtain the copper hydroxide/cuprous oxide nanotube active material;

and (3) placing the copper hydroxide/cuprous oxide nanotube active material in a chloropalladate solution with the concentration of 0.01-5 mol/L for soaking for 1-60 min, and drying to obtain the oxygen evolution electrode material loaded with noble metal palladium on the copper hydroxide/cuprous oxide nanotube active material.

According to the preparation method of the oxygen evolution electrode material, the copper hydroxide/cuprous oxide nanotube active material is grown in situ on the high-conductivity foamy copper and is soaked in the noble metal palladium solution, so that the noble metal palladium is loaded on the copper hydroxide/cuprous oxide nanotube active material, the advantage of high specific surface area of a tubular structure is fully utilized, the conductivity of the active material is improved, the using amount of the noble metal palladium can be reduced, the cost is reduced, and the problem of high internal resistance caused by using a polymer can be avoided due to the fact that the electrode is an integrated electrode. In addition, the oxygen evolution electrode material can promote the contact of active substances and electrolyte, and greatly enhances the performance and stability of the oxygen evolution catalyst.

Detailed Description

In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention provides a preparation method of an oxygen evolution electrode material, which comprises the following steps:

growing a copper hydroxide/copper oxide nanotube active material on the foamy copper to obtain the copper hydroxide/cuprous oxide nanotube active material;

and secondly, placing the copper hydroxide/cuprous oxide nanotube active material in a chloropalladate solution with the concentration of 0.01-5 mol/L for soaking for 1-60 min, and drying to obtain the oxygen evolution electrode material with the noble metal palladium loaded on the copper hydroxide/cuprous oxide nanotube active material.

According to the preparation method of the oxygen evolution electrode material, the copper hydroxide/cuprous oxide nanotube active material is grown in situ on the high-conductivity foamy copper and is soaked in the noble metal palladium solution, so that the noble metal palladium is loaded on the copper hydroxide/cuprous oxide nanotube active material, the advantage of high specific surface area of a tubular structure is fully utilized, the conductivity of the active material is improved, the using amount of the noble metal palladium can be reduced, the cost is reduced, and the problem of high internal resistance caused by using a polymer can be avoided due to the fact that the electrode is an integrated electrode. In addition, the oxygen evolution electrode material can promote the contact of active substances and electrolyte, and greatly enhances the performance and stability of the oxygen evolution catalyst.

Further, the step one of growing the copper hydroxide/copper oxide nanotube active material on the copper foam comprises the following steps:

soaking the foamy copper in an acid solution and water for 2-15 min in sequence;

the impurities of the copper foam can be removed by soaking and cleaning the copper foam in acid and water, and the oxygen evolution stability of the oxygen evolution electrode is further improved.

Then the copper foam is put into alkaline solution and (NH)₄)₂S₂O₈And soaking the solution in the mixed solution for 10-50 min, and taking out and drying the foam copper when the foam copper is changed from orange to blue to obtain the copper hydroxide/cuprous oxide nanotube active material.

Wherein the concentration of the alkaline solution is 0.1-6 mol/L, (NH)₄)₂S₂O₈The concentration of the solution is 0.05-0.8 mol/L.

Specifically, the alkaline solution is NaOH solution, KOH solution or Na₂CO₃At least one of solution solutions. The acid solution is dilute hydrochloric acid or dilute sulfuric acid. Preferably, the concentration of the alkaline solution is 1-4 mol/L. (NH)₄)₂S₂O₈The concentration of the solution is 0.1-0.5 mol/L. Copper foam in alkaline solution and (NH)₄)₂S₂O₈Soaking the mixture in the solution for 20-40 min.

Specifically, the chloropalladate solution is any one of a sodium chloropalladate solution, a potassium chloropalladate solution or a magnesium chloropalladate solution. Preferably, the concentration of the chloropalladate solution is 0.1-0.5 mol/L.

Optionally, growing copper hydroxide/copper oxide nanotube active material on the copper foam further comprises:

soaking the foamy copper in sulfuric acid for 5-15 min, then soaking the foamy copper into an alkaline solution, taking out the foamy copper when the surface of the foamy copper is blue, and drying to obtain the copper hydroxide/cuprous oxide nanotube active material.