阅读说明：本技术 一种Ni85Se100/碳纳米管复合物的制备方法 (Preparation method of Ni85Se 100/carbon nanotube composite ) 是由 申士杰 张欢欢 钟文武 林志萍 王宗鹏 于 2020-12-22 设计创作，主要内容包括：本发明公开一种Ni85Se100/碳纳米管复合物的制备方法,所述方法包括制备前驱体,水热反应等步骤。制备的复合物具备优异的电催化析氢性能。(The invention discloses a preparation method of a Ni85Se 100/carbon nanotube composite, which comprises the steps of precursor preparation, hydrothermal reaction and the like. The prepared compound has excellent electro-catalytic hydrogen evolution performance.)

1. A preparation method of a Ni85Se 100/carbon nanotube composite is characterized by comprising the following steps: soaking 500mg of carbon nano tube in a mixed solution of nitric acid and sulfuric acid, wherein the mass specifications of the nitric acid and the sulfuric acid are 70% and 96% respectively, and the volume ratio of the nitric acid to the sulfuric acid is 1: 1; placing the mixed solution in an oil bath at 90 ℃ for 1 hour; after cooling to room temperature, the liquid was filtered off with filter paper; dispersing the carbon nanotubes in the filter paper in deionized water; centrifugally cleaning for 5 times; drying in an oven for 24 hours to obtain a precursor I; weighing 0.632g of selenium powder and 0.378g of sodium borohydride, dissolving in 65mL of dimethylformamide, and continuously stirring for 20 minutes; 0.9508g of nickel chloride were added; adding the precursor I according to the concentration of 1mg/mL, and stirring for 20 min; transferring the solution into a 100 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, centrifugally cleaning with deionized water for 2 times, and centrifugally cleaning with ethanol for 1 time; vacuum drying at 60 deg.C for 12 hr; the Ni85Se 100/carbon nano tube compound is obtained.

2. The Ni85Se 100/carbon nanotube composite prepared by the method of claim 1.

3. The use of the Ni85Se 100/carbon nanotube composite of claim 2 in the field of electrocatalytic hydrogen evolution.

Technical Field

The invention relates to a preparation method of a Ni85Se 100/carbon nanotube composite.

Technical Field

Hydrogen is considered an environmentally friendly clean energy source. The product of burning hydrogen is only water, unlike traditional fuels which emit greenhouse gases or polluting gases such as carbon dioxide and sulfur dioxide. Therefore, the hydrogen is more environment-friendly as a new energy source. The electrocatalytic decomposition of water can prepare high-purity hydrogen, and is one of the effective methods for preparing hydrogen at present. Noble metals have been the most active catalysts in this field. However, the cost of precious metals is prohibitively high, and researchers have been continually searching for new non-precious metal electrocatalysts to reduce costs in recent years.

There are many ways to explore new non-noble metal electrocatalysts, where new methods of preparation often produce samples with unexpected superior properties. Although the solvothermal method is a conventional production method, since reaction raw materials are various and various additives can be added, the components of a sample obtained by the solvothermal method are often difficult to predict in advance. Therefore, how to prepare a novel electrocatalyst with excellent performance by a solvothermal method is a problem to be solved urgently.

Disclosure of Invention

The invention aims to provide a preparation method of a Ni85Se 100/carbon nanotube composite with excellent performance. (for convenience of presentation, Ni85Se100 is hereinafter replaced with Ni0.85Se).

The preparation method of the Ni0.85Se/carbon nanotube composite comprises the following steps: soaking 500mg of carbon nano tube in a mixed solution of nitric acid and sulfuric acid, wherein the mass specifications of the nitric acid and the sulfuric acid are 70% and 96% respectively, and the volume ratio of the nitric acid to the sulfuric acid is 1: 1; placing the mixed solution in an oil bath at 90 ℃ for 1 hour; after cooling to room temperature, the liquid was filtered off with filter paper; dispersing the carbon nanotubes in the filter paper in deionized water; centrifugally cleaning for 5 times; drying in an oven for 24 hours to obtain a precursor I; weighing 0.632g of selenium powder and 0.378g of sodium borohydride, dissolving in 65mL of dimethylformamide, and continuously stirring for 20 minutes; 0.9508g of nickel chloride were added; adding the precursor I according to the concentration of 1mg/mL, and stirring for 20 min; transferring the solution into a 100 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, centrifugally cleaning with deionized water for 2 times, and centrifugally cleaning with ethanol for 1 time; vacuum drying at 60 deg.C for 12 hr; obtaining the Ni0.85Se/carbon nano tube compound.

Compared with the prior art, the sample provided by the invention has the following advantages: the prepared electro-catalyst has excellent performance and small hydrogen evolution overpotential.

Drawings

Fig. 1 is XRD patterns of the example sample and the comparative example sample.

FIG. 2 is a linear voltammogram of a sample of the example.

Detailed Description

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

The preparation method of the Ni0.85Se/carbon nanotube composite comprises the following steps: soaking 500mg of carbon nano tube in a mixed solution of nitric acid and sulfuric acid, wherein the mass specifications of the nitric acid and the sulfuric acid are 70% and 96% respectively, and the volume ratio of the nitric acid to the sulfuric acid is 1: 1; placing the mixed solution in an oil bath at 90 ℃ for 1 hour; after cooling to room temperature, the liquid was filtered off with filter paper; dispersing the carbon nanotubes in the filter paper in deionized water; centrifugally cleaning for 5 times; drying in an oven for 24 hours to obtain a precursor I; weighing 0.632g of selenium powder and 0.378g of sodium borohydride, dissolving in 65mL of dimethylformamide, and continuously stirring for 20 minutes; 0.9508g of nickel chloride were added; adding the precursor I according to the concentration of 1mg/mL, and stirring for 20 min; transferring the solution into a 100 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, centrifugally cleaning with deionized water for 2 times, and centrifugally cleaning with ethanol for 1 time; vacuum drying at 60 deg.C for 12 hr; obtaining the Ni0.85Se/carbon nano tube compound.

To illustrate the technical effects of the example samples, comparative example samples were prepared as follows: weighing 0.632g of selenium powder and 0.378g of sodium borohydride, dissolving in 65mL of dimethylformamide, and continuously stirring for 20 minutes; 0.9508g of nickel chloride were added; stirring for 20 min; transferring the solution into a 100 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, centrifugally cleaning with deionized water for 2 times, and centrifugally cleaning with ethanol for 1 time; vacuum drying at 60 deg.C for 12 hr; a sample of NiSe2 was obtained.

In order to illustrate the technical effects of the present example, the example samples and the comparative example samples were characterized. Fig. 1 is an XRD spectrum of both. The lower 3 vertical lines in the figure correspond to standard data of Ni0.85Se (PDF # 18-0888, space group P63/mmc), carbon (PDF #75-1621, space group P63/mmc) and NiSe2 (PDF # 65-1843, space group Pa-3) in the hexagonal system, respectively. For the example samples, it can be seen that the diffraction peaks of the samples match the standard data for Ni0.85Se of hexagonal system (PDF # 18-0888, space group P63/mmc) and carbon of hexagonal system (PDF #75-1621, space group P63/mmc), indicating that the samples are Ni0.85Se/carbon nanotube composites. For the comparative sample, the diffraction peak matched the standard data for cubic NiSe2 (PDF # 65-1843, space group Pa-3), indicating that the sample was NiSe 2. The above results show that the method of the example can promote the phase transition from NiSe2 to Ni0.85Se, achieving unexpected technical effects.

The samples of the examples were tested for their electrocatalytic hydrogen evolution overpotential with a 0.5M sulfuric acid solution as the electrolyte. FIG. 2 is a linear voltammogram of a sample of an example from which the electrocatalytic overpotential for hydrogen evolution (10 mA/cm) of the sample of the example can be seen²When the voltage is higher than the threshold value), the voltage is 162 mV. The result shows that the sample of the embodiment has excellent electrocatalytic hydrogen evolution performance.

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.