阅读说明：本技术 一种钴硒纳米球电催化剂的制备方法 (Preparation method of cobalt-selenium nanosphere electrocatalyst ) 是由 申士杰 张欢欢 钟文武 林志萍 王宗鹏 于 2019-09-21 设计创作，主要内容包括：本发明公开一种钴硒纳米球电催化剂的制备方法,包括以下步骤：将氯化钴溶于丙三醇和乙醇的混合溶液中,在150℃溶剂热反应24小时；再与甲亚硒酸在150℃微波辅助反应24小时。(The invention discloses a preparation method of a cobalt-selenium nanosphere electrocatalyst, which comprises the following steps of: dissolving cobalt chloride in a mixed solution of glycerol and ethanol, and carrying out solvothermal reaction for 24 hours at 150 ℃; and then the reaction product is reacted with selenious acid A for 24 hours at 150 ℃ in a microwave-assisted manner.)

1. A preparation method of a cobalt-selenium nanosphere electrocatalyst comprises the following steps: dissolving 180mg of cobalt chloride in a mixed solution of glycerol and ethanol, wherein the glycerol and the ethanol are respectively 30 mL; then stirring for 30 minutes by magnetic force; sealing the solution in a 100mL reaction kettle, placing the reaction kettle in an oven at 150 ℃ and keeping the temperature for 24 hours; cooling to room temperature; cleaning the precipitate in the solution with alcohol for 3 times, and placing in an oven at 50 ℃ for 24 hours; placing 30mg of the dried precipitate and 100mg of selenious acid A in 60mL of dimethylformamide solution and magnetically stirring for 30 minutes; sealing the reaction kettle in a 100mL reaction kettle, and placing the reaction kettle in a microwave-assisted heating muffle furnace for 24 hours, wherein the temperature of the muffle furnace is set to be 150 ℃, the microwave frequency is set to be 2000 MHz, and the microwave power is set to be 150W; cooling to room temperature; the precipitate in the solution was washed with alcohol 3 times and then placed in an oven at 50 ℃ for 24 hours.

2. A cobalt selenium nanosphere electrocatalyst prepared as claimed in claim 1.

Technical Field

The invention relates to a preparation method of a cobalt-selenium nanosphere electrocatalyst.

Technical Field

Global energy crisis and environmental pollution from the burning of fossil fuels are problems faced during human development. This has motivated efforts to develop clean and renewable energy alternatives. In recent years, the search for hydrogen as a future energy carrier has received increasing attention. In particular, sustainable hydrogen production by electrically induced water decomposition is of great importance. To date, the most effective hydrogen evolution electrocatalysts are Pt metalloids. But its large-scale application is severely limited by its high cost and low abundance. Therefore, finding an inexpensive hydrogen evolution electrocatalyst with high activity remains a challenge.

One of the indexes for measuring the performance of the electrocatalyst is overpotential. Too high an overpotential may result in excessive energy waste during the production of hydrogen by electrocatalysis. Therefore, the search for non-noble metal electrocatalysts with lower overpotentials is an urgent problem to be solved.

Disclosure of Invention

The invention aims to provide a preparation method of a cobalt-selenium nanosphere electrocatalyst with low overpotential.

The implementation of the invention comprises the following steps: dissolving 180mg of cobalt chloride in a mixed solution of glycerol and ethanol, wherein the glycerol and the ethanol are respectively 30 mL; then stirring for 30 minutes by magnetic force; sealing the solution in a 100mL reaction kettle, placing the reaction kettle in an oven at 150 ℃ and keeping the temperature for 24 hours; cooling to room temperature; cleaning the precipitate in the solution with alcohol for 3 times, and placing in an oven at 50 ℃ for 24 hours; placing 30mg of the dried precipitate and 100mg of selenious acid A in 60mL of dimethylformamide solution and magnetically stirring for 30 minutes; sealing the reaction kettle in a 100mL reaction kettle, and placing the reaction kettle in a microwave-assisted heating muffle furnace for 24 hours, wherein the temperature of the muffle furnace is set to be 150 ℃, the microwave frequency is set to be 2000 MHz, and the microwave power is set to be 150W; cooling to room temperature; the precipitate in the solution was washed with alcohol 3 times and then placed in an oven at 50 ℃ for 24 hours.

Compared with the prior art, the sample preparation method has the following advantages: the prepared sample has a nanosphere structure; the overpotential is low; the cost is low.

Drawings

Figure 1 is an X-ray diffraction pattern of cobalt selenium nanosphere electrocatalyst.

FIG. 2 is a scanning electron microscope atlas of cobalt selenium nanosphere electrocatalyst.

Figure 3 is an overpotential graph of cobalt selenium nanosphere electrocatalyst.

Detailed Description

The following describes the implementation of the present invention in detail with reference to specific embodiments.

The specific steps of this example are as follows: dissolving 180mg of cobalt chloride in a mixed solution of glycerol and ethanol, wherein the glycerol and the ethanol are respectively 30 mL; then stirring for 30 minutes by magnetic force; sealing the solution in a 100mL reaction kettle, placing the reaction kettle in an oven at 150 ℃ and keeping the temperature for 24 hours; cooling to room temperature; cleaning the precipitate in the solution with alcohol for 3 times, and placing in an oven at 50 ℃ for 24 hours; placing 30mg of the dried precipitate and 100mg of selenious acid A in 60mL of dimethylformamide solution and magnetically stirring for 30 minutes; placing the reaction kettle in a microwave-assisted heating muffle furnace for 24 hours, wherein the temperature of the muffle furnace is set to be 150 ℃, the microwave frequency is set to be 2000 MHz, and the microwave power is set to be 150 watts; cooling to room temperature; the precipitate in the solution was washed with alcohol 3 times and then placed in an oven at 50 ℃ for 24 hours.

FIG. 1 is diffraction data measured by an X-ray diffraction method, wherein the diffraction peak position of the sample is consistent with that of Co _0.85 Se reported in the literature, the synthesized sample is Co _0.85 Se., the sample is subjected to scanning electron microscope characterization, and the result is shown in FIG. 2, the sample is in a shape of a nanosphere structure, the diameter of the nanosphere is between 200nm and 400nm, the overpotential characterization conditions are that a 0.5M sulfuric acid solution is used as an electrolyte, the sample is coated on a glassy carbon electrode to serve as a working electrode, a calomel electrode is used as a reference electrode, a graphite electrode is used as a counter electrode, the overpotential curve of the sample is shown in FIG. 3, the overpotential at-10 mA/cm ² is generally adopted to evaluate the good or bad catalytic performance, and the overpotential of the sample in the example is-190 mV, so that the sample shows excellent electrocatalytic performance.

The invention also discloses a cobalt-selenium nanosphere electrocatalyst which is prepared by adopting the method in the embodiment.

It should be noted that the above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above examples. It is to be understood that other modifications and variations, which may be directly derived or suggested to one skilled in the art without departing from the basic concept of the invention, are to be considered as included within the scope of the invention.