阅读说明：本技术 一种碳纳米管复合镍硒纳米片电催化剂的制备方法 (Preparation method of carbon nanotube composite nickel-selenium nanosheet 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：本发明公开一种碳纳米管复合镍硒纳米片电催化剂的制备方法,包括以下步骤：将Se粉、硼氢化钠、碳纳米管和硝酸镍溶于乙腈和乙二醇的混合溶液中,在180℃微波辅助反应24小时。(The invention discloses a preparation method of a carbon nano tube composite nickel-selenium nanosheet electrocatalyst, which comprises the following steps of: se powder, sodium borohydride, carbon nano tubes and nickel nitrate are dissolved in a mixed solution of acetonitrile and ethylene glycol, and microwave-assisted reaction is carried out for 24 hours at 180 ℃.)

1. A preparation method of a carbon nanotube composite nickel-selenium nanosheet electrocatalyst comprises the following steps: adding 0.4mmol Se powder and 1mmol sodium borohydride into 60mL of mixed solution of acetonitrile and ethylene glycol, wherein each volume of acetonitrile and ethylene glycol is 30mL, and magnetically stirring for 1 hour; adding 50mg of carbon nano tube and 0.35mmol of nickel nitrate into the solution, and magnetically stirring for 1 hour; sealing the solution 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 180 ℃, the microwave frequency is set to be 1500 MHz, and the microwave power is set to be 140 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.

2. A carbon nanotube composite nickel selenium nanosheet electrocatalyst, prepared by the method of claim 1.

Technical Field

The invention relates to a preparation method of a carbon nano tube composite nickel-selenium nanosheet electrocatalyst.

Technical Field

The rapid development of human society causes the excessive consumption of conventional energy and the waste of natural resources, and the environmental pollution is more and more serious, thereby influencing the long-term development of human beings. Therefore, the use of clean energy has recently attracted much attention. Among them, hydrogen fuel is considered as the most promising green energy source due to its excellent combustion performance and high energy density. In addition, the source of hydrogen is very extensive and hydrogen energy is available in many ways. Among them, hydrogen production by electrolysis of water is considered to be the most effective means. Currently, the most efficient hydrogen evolution catalyst is the Pt-based metal. However, these extremely high cost precious metals are relatively scarce and are not widely used in the field of electrocatalysis. It is important to explore inexpensive and excellent electrocatalysts to replace noble metals.

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 carbon nanotube composite nickel selenium nanosheet electrocatalyst with low overpotential.

The implementation of the invention comprises the following steps: adding 0.4mmol Se powder and 1mmol sodium borohydride into 60mL of mixed solution of acetonitrile and ethylene glycol, wherein each volume of acetonitrile and ethylene glycol is 30mL, and magnetically stirring for 1 hour; adding 50mg of carbon nano tube and 0.35mmol of nickel nitrate into the solution, and magnetically stirring for 1 hour; sealing the solution 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 180 ℃, the microwave frequency is set to be 1500 MHz, and the microwave power is set to be 140 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.

Compared with the prior art, the sample preparation method has the following advantages: the prepared sample is of a nanosheet structure, more exposed active sites are exposed, and the overpotential is lower; the cost is low.

Drawings

Fig. 1 is an X-ray diffraction pattern of a carbon nanotube composite nickel selenium nanosheet electrocatalyst.

Fig. 2 is a scanning electron microscope atlas of the carbon nanotube composite nickel selenium nanosheet electrocatalyst.

Fig. 3 is a scanning electron microscope atlas of nickel selenium nanosheet electrocatalyst.

FIG. 4 is a scanning electron micrograph of carbon nanotubes.

Fig. 5 is an overpotential curve of a carbon nanotube composite nickel selenium nanosheet electrocatalyst and a nickel selenium nanosheet 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: adding 0.4mmol Se powder and 1mmol sodium borohydride into 60mL of mixed solution of acetonitrile and ethylene glycol, wherein each volume of acetonitrile and ethylene glycol is 30mL, and magnetically stirring for 1 hour; adding 50mg of carbon nano tube and 0.35mmol of nickel nitrate into the solution, and magnetically stirring for 1 hour; sealing the solution 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 180 ℃, the microwave frequency is set to be 1500 MHz, and the microwave power is set to be 140 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.

In order to illustrate the technical effect when no carbon nanotube is added, a nickel selenium nanosheet sample is also prepared according to the following steps: adding 0.4mmol Se powder and 1mmol sodium borohydride into 60mL of mixed solution of acetonitrile and ethylene glycol, wherein each volume of acetonitrile and ethylene glycol is 30mL, and magnetically stirring for 1 hour; adding 0.35mmol of nickel nitrate into the solution, and magnetically stirring for 1 hour; sealing the solution 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 180 ℃, the microwave frequency is set to be 1500 MHz, and the microwave power is set to be 140 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.

In order to illustrate the technical effects of the embodiment, a sample prepared according to the method steps of the embodiment is characterized, fig. 1 is diffraction data measured by an X-ray diffraction method, the diffraction peak position of the sample is respectively consistent with the diffraction peak positions of Ni _0.85 Se and a carbon nano tube in a standard database, the synthesized sample is a composite of Ni _0.85 Se and the carbon nano tube, the sample is characterized by a scanning electron microscope, and the result is shown in fig. 2-4, Ni _0.85 Se is the morphology of a nanosheet structure, the carbon nano tube is the morphology of the nano tube, the morphology of the carbon nano tube composite nickel selenium nanosheet is shown as Ni _0.85 Se nanosheet dispersed in the carbon nano tube, the overpotential characterization condition is that 0.5M vitriol solution is used as electrolyte, the sample is coated on the 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. 5, the overpotential curve of the sample is generally evaluated by the overpotential of-10 mA/cm 64, the overpotential of the carbon nano tube composite nickel selenium nanosheet is shown as-161 mV, the overpotential comparison result of the carbon nano tube, the overpotential of the carbon nano tube is shown in the publication of-30 mV-254 mV, the overpotential comparison result of the carbon nano tube publication of the overpotential comparison of the carbon nano tube publication of the copper nanosheet is shown in the publication of.

The invention also discloses a carbon nanotube composite nickel-selenium nanosheet electrocatalyst prepared by 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.