CN108325539B - Rod-like vanadium modified Ni self-assembled into flower ball shape3S2Synthesis method of electrocatalyst - Google Patents
Rod-like vanadium modified Ni self-assembled into flower ball shape3S2Synthesis method of electrocatalyst Download PDFInfo
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Abstract
Hair brushA rod-shaped self-assembled flower-shaped ball-shaped vanadium modified Ni is disclosed3S2The synthesis method of the electrocatalyst comprises the following steps: soaking clean foam nickel into suspension with the concentration of a vanadium source of 5-30 mM and the molar ratio of the vanadium source to a sulfur source of 1 (0.5-12), performing microwave solvothermal reaction, and after full reaction, obtaining rod-like vanadium-modified Ni self-assembled into a flower ball shape3S2An electrocatalyst material. The method has the advantages of simple operation, mild reaction conditions and short time consumption, and the prepared rod-shaped vanadium-modified Ni which is self-assembled into a flower ball shape3S2The product has high purity and uniform appearance and size.
Description
Technical Field
The invention belongs to the field of new energy material preparation, and particularly relates to a rod-shaped self-assembled flower-ball-shaped vanadium-modified Ni3S2A method for synthesizing an electrocatalyst.
Background
The electro-catalytic water cracking technology is a new technology in the field of energy environment, substances such as carbide, phosphide, sulfide and the like have excellent electro-catalytic performance and are widely concerned by people, wherein WS is used2、MoS2Is a representative substance and has excellent electrocatalytic hydrogen production activity. However, at present, the oxidation of water as a speed control step in the water splitting process still restricts the whole process of water splitting. Currently, most oxygen-generating electrocatalysts still have high overpotentials and high costs, limiting large-scale use. Ni3S2The material has intrinsic metallic properties due to the continuous Ni-Ni bond network throughout the entire structure. High conductivity, inexpensive Ni3S2Has been widely used in many fields. Prepared Ni reported at present3S2The material appearance comprises a sheet shape, a flower shape, a rod shape and the like.
Chinese invention announcementPatent No. 201610552386.6 discloses a lithium ion battery cathode GO-PANT-Ni3S2The preparation method of the composite material has complex operation steps, long reaction period and great technical difficulty. The Chinese patent No. 201610252105.5 discloses an array type nickel disulfide-carbon nanotube composite electrode and a preparation method and application thereof, wherein a hydrothermal method is used for reaction, and a heat treatment method is used for obtaining the array type nickel disulfide-carbon nanotube composite electrode material, so that the reaction period is long, the reaction conditions are harsh, and the cost is high. Chinese patent No. 201310320738.1 discloses a composite catalytic electrode for electrolyzing water to generate oxygen and its preparation method, wherein the rod-like Ni (OH) is prepared by hydrothermal method2/ Ni3S2The composite electrode has large overpotential, cannot be used under a high-current condition and has poor catalytic activity.
The patent uses vanadium-based material and Ni3S2The combination of materials has important significance for exploiting the oxygen evolution electrocatalyst with special appearance, high efficiency, low cost and simple preparation process.
Disclosure of Invention
In order to overcome the defects of the materials, the patent provides a rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2The method for synthesizing the electrocatalyst is simple to operate, mild in reaction conditions and short in time consumption, and the prepared rod-shaped vanadium-modified Ni self-assembled into a flower ball shape3S2The product has high purity and uniform appearance and size. In order to achieve the above object, the present invention adopts the following technical solutions.
In order to achieve the purpose, the invention adopts the technical scheme that: rod-like vanadium modified Ni self-assembled into flower ball shape3S2A method of electrocatalyst, comprising the steps of:
(1) soaking the foam nickel to be treated in acetone for ultrasonic cleaning, soaking the foam nickel in 0.5-4 mol/L hydrochloric acid for ultrasonic cleaning, finally alternately washing with ethanol and deionized water respectively, and performing vacuum drying to obtain pretreated foam nickel;
(2) weighing a certain mass of a vanadium source and a sulfur source, controlling the molar ratio of the vanadium source to the sulfur source to be 1 (0.5-12), dissolving the vanadium source and the sulfur source in a proper amount of solvent to enable the concentration of the vanadium source to be 5-30 mM, and stirring for 3-20 min to obtain a suspension A;
(3) placing the stirred suspension A and the foam nickel pretreated in the step (1) into a microwave hydrothermal instrument for reaction;
(4) after the reaction is finished, the product is alternately washed for a plurality of times by deionized water and ethanol, and is dried in vacuum to obtain the rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
And (2) carrying out ultrasonic cleaning for 5-15 min in the step (1).
The vacuum drying in the step (1) is carried out for 3-15 h at the temperature of 10-60 ℃.
And (3) the vanadium source in the step (2) is one or more of vanadium pentoxide, sodium metavanadate, sodium vanadate, sodium dodecahydrate, ammonium metavanadate and vanadyl acetylacetonate.
The sulfur source in the step (2) is one or more of thiourea, thioacetamide, sodium sulfide, sodium diethylthiocarbamate and elemental sulfur.
The solvent in the step (2) is one or more of deionized water, absolute ethyl alcohol, methanol and glycol.
The reaction temperature in the step (3) is 60-120 ℃, the power is 200-400W, and the reaction time is 0.5-2 h.
And (4) vacuum drying at 10-60 ℃ for 3-15 h.
The invention also provides vanadium modified Ni with uniform appearance prepared by the method3S2An electrocatalyst material.
Compared with the prior art, the invention can obtain the following beneficial effects:
(1) the invention adopts a microwave solvothermal method to directly synthesize vanadium-modified Ni with uniform appearance3S2The electrocatalyst material has the advantages of low synthesis temperature, short synthesis time, wide raw material source, low cost, environmental friendliness and suitability for large-scale production.
(2) Vanadium modified Ni prepared by the invention3S2Electro-catalyst material to obtain rod-shaped self-assembled flower-ball-shaped vanadium modified Ni with special structure3S2The specific surface area of the material is increased by the electrocatalyst material, so that the catalytic active sites of the material are increased, and the unique three-dimensional porous structure of the foam nickel substrate reduces the contact resistance of the material, improves the charge transmission capability and enhances the electrochemical performance of the material.
(3) The invention greatly improves the catalytic activity of the catalyst by introducing a proper vanadium source and the synergistic effect of the two, can be used as an excellent electro-catalytic oxygen production electro-catalyst at 10 mA/cm2The overpotential can be as low as 180 mV at 100 mA/cm2The overpotential can be as low as 440 mV at the current density of (1).
Drawings
FIG. 1 shows vanadium modified Ni grown on nickel foam prepared in example 2 of the present invention3S2An X-ray diffraction (XRD) pattern of the electrocatalyst material;
FIG. 2 shows vanadium modified Ni grown on nickel foam prepared in example 2 of the present invention3S2A 700 x Scanning Electron Microscope (SEM) magnification of the electrocatalyst material;
FIG. 3 shows vanadium modified Ni grown on nickel foam prepared in example 2 of the present invention3S24000-fold magnified Scanning Electron Microscope (SEM) photographs of the electrocatalyst material;
FIG. 4 shows vanadium modified Ni grown on nickel foam prepared in example 2 of the present invention3S220000 times magnified Scanning Electron Microscope (SEM) photograph of the electrocatalyst material;
FIG. 5 shows vanadium modified Ni grown on nickel foam prepared in example 2 of the present invention3S2Linear Sweep Voltammetry (LSV) performance test plots of the electrocatalyst materials.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and specific embodiments, but the present invention is not limited to the following embodiments.
Example 1:
(1) sequentially immersing (2 x 5) cm of foamed nickel into acetone and hydrochloric acid for ultrasonic cleaning for 5 min, then alternately washing for 3 times by using ethanol and deionized water respectively, wherein the concentration of the hydrochloric acid is 0.5 mol/L, and then carrying out vacuum drying for 3 h at 10 ℃ to obtain the treated foamed nickel;
(2) selecting vanadium pentoxide and thiourea as raw materials, taking 0.075 mmol of vanadyl acetylacetonate, and controlling the molar ratio of a vanadium source to a sulfur source to be 1: 0.5, adding into 15 ml of absolute ethyl alcohol, and magnetically stirring for 3 min at room temperature to obtain a suspension A;
(3) placing the stirred suspension A and the metal nickel processed in the step (1) into a microwave reactor, carrying out solvothermal reaction for 30 min at the temperature of 60 ℃ and the power of 200W,
(4) after the reaction is finished and the reaction product is cooled, the product is alternately washed by deionized water and ethanol for 3 times, and then is dried in vacuum for 3 hours at the temperature of 10 ℃ to obtain the rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
Example 2:
(1) sequentially immersing (2 x 5) cm of foamed nickel into acetone and hydrochloric acid for ultrasonic cleaning for 5 min, then alternately washing for 3 times by using ethanol and deionized water respectively, wherein the concentration of the hydrochloric acid is 1 mol/L, and then carrying out vacuum drying at 10 ℃ for 5h to obtain the treated foamed nickel;
(2) selecting vanadium pentoxide and thioacetamide as raw materials, taking 0.15 mmol of vanadyl acetylacetonate, and controlling the molar ratio of a vanadium source to a sulfur source to be 1: 1, simultaneously adding the mixture into 15 ml of absolute ethyl alcohol, and magnetically stirring the mixture for 5 min at room temperature to obtain suspension A;
(3) placing the stirred suspension A and the metal nickel processed in the step (1) into a microwave reactor, carrying out solvothermal reaction for 60 min at the temperature of 80 ℃ and the power of 200W,
(4) after the reaction is finished and the reaction product is cooled, the product is alternately washed by deionized water and ethanol for 3 times, and then is dried in vacuum for 3 hours at the temperature of 20 ℃ to obtain the rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2ElectrocatalysisA catalyst material.
Vanadium modified Ni prepared in this example3S2The electrocatalyst material, the position where the X-ray powder diffraction peak appears as seen in FIG. 1, is denoted as Ni3S2Almost no other peaks appear, indicating that V is present in the material in doped form.
Vanadium modified Ni can be seen in the 700-fold magnified SEM image of FIG. 23S2The electrocatalyst material grows uniformly on the surface of the foamed nickel, and the vanadium modified Ni can be seen from the SEM photographs of FIGS. 3 and 43S2The electrocatalyst material was self-assembled in rod-like arrays into flower-like spheres, as seen in the linear scanning voltammogram of FIG. 5, at a current density of 10 mA/cm2It has a low overpotential of 180 mV at 100 mA/cm2Has over-potential as low as 440 mV, which shows that the material has good electrocatalytic oxygen evolution activity.
Example 3:
(1) sequentially immersing (2 x 5) cm of foamed nickel into acetone and hydrochloric acid for ultrasonic cleaning for 10 min, then alternately washing for 3 times by using ethanol and deionized water respectively, wherein the concentration of the hydrochloric acid is 2 mol/L, and then carrying out vacuum drying for 10 h at 20 ℃ to obtain the treated foamed nickel;
(2) selecting sodium metavanadate and a sulfur simple substance as raw materials, taking 0.3 mmol of vanadyl acetylacetonate, and controlling the molar ratio of a vanadium source to a sulfur source to be 1: 4, simultaneously adding the mixture into 15 ml of absolute ethyl alcohol, and magnetically stirring the mixture for 10 min at room temperature to obtain suspension A;
(3) placing the stirred suspension A and the metal nickel processed in the step (1) into a microwave reactor, carrying out solvothermal reaction for 90 min at the temperature of 100 ℃ and the power of 300W,
(4) after the reaction is finished and the reaction product is cooled, the product is alternately washed by deionized water and ethanol for 3 times, and then is dried in vacuum for 5 hours at the temperature of 30 ℃ to obtain the rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
Example 4:
(1) sequentially immersing (2 x 5) cm of foamed nickel into acetone and hydrochloric acid for ultrasonic cleaning for 10 min, then alternately washing for 3 times by using ethanol and deionized water respectively, wherein the concentration of the hydrochloric acid is 2.5 mol/L, and then carrying out vacuum drying for 10 h at 40 ℃ to obtain the treated foamed nickel;
(2) selecting sodium vanadate and diethylthiocarbamic acid as raw materials, taking 0.4 mmol of vanadyl acetylacetonate, and controlling the molar ratio of a vanadium source to a sulfur source to be 1: 5, simultaneously adding the mixture into a mixture of 20 ml of absolute ethyl alcohol and water, and magnetically stirring the mixture for 15 min at room temperature to obtain suspension A;
(3) placing the stirred suspension A and the metal nickel treated in the step (1) into a microwave reactor, carrying out microwave hydrothermal reaction for 90 min at the temperature of 100 ℃ and the power of 300W,
(4) after the reaction is finished and the reaction product is cooled, the product is alternately washed by deionized water and ethanol for 3 times, and then is dried in vacuum for 10 hours at the temperature of 40 ℃ to obtain the rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
Example 5:
(1) sequentially immersing (2 x 5) cm of foamed nickel into acetone and hydrochloric acid for ultrasonic cleaning for 15 min, then alternately washing for 3 times by using ethanol and deionized water respectively, wherein the concentration of the hydrochloric acid is 3 mol/L, and then carrying out vacuum drying for 15h at 40 ℃ to obtain the treated foamed nickel;
(2) selecting sodium vanadate dodecahydrate and sodium sulfide as raw materials, taking 0.4 mmol of vanadyl acetylacetonate, and controlling the molar ratio of a vanadium source to a sulfur source to be 1: 10, simultaneously adding the mixture into 20 ml of ethylene glycol, and magnetically stirring the mixture for 15 min at room temperature to obtain suspension A;
(3) placing the stirred suspension A and the metal nickel treated in the step (1) into a microwave reactor, carrying out solvothermal reaction for 120 min at the temperature of 120 ℃ and the power of 400W,
(4) after the reaction is finished and the reaction product is cooled, the product is alternately washed by deionized water and ethanol for 3 times, and then is dried in vacuum for 10 hours at the temperature of 20 ℃ to obtain the rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
Example 6:
(1) sequentially immersing (2 x 5) cm of foamed nickel into acetone and hydrochloric acid for ultrasonic cleaning for 15 min, then alternately washing for 3 times by using ethanol and deionized water respectively, wherein the concentration of the hydrochloric acid is 4 mol/L, and then carrying out vacuum drying for 15h at 60 ℃ to obtain the treated foamed nickel;
(2) selecting vanadyl acetylacetonate and thioacetamide as raw materials, taking 0.9 mmol of vanadyl acetylacetonate, and controlling the molar ratio of a vanadium source to a sulfur source to be 1: 12, simultaneously adding the mixture into a mixed solution of 30 ml of glycol and water, and magnetically stirring the mixture for 20 min at room temperature to obtain a suspension A;
(3) placing the stirred suspension A and the metal nickel treated in the step (1) into a microwave reactor, carrying out solvothermal reaction for 120 min at the temperature of 120 ℃ and the power of 400W,
(4) after the reaction is finished and the reaction product is cooled, the product is alternately washed by deionized water and ethanol for 3 times, and then is dried in vacuum for 15 hours at the temperature of 60 ℃ to obtain the rod-shaped vanadium modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
Claims (7)
1. Rodlike V-modified Ni self-assembled into flower ball shape3S2A method of electrocatalysts, comprising the steps of:
soaking clean foam nickel into suspension with the concentration of a vanadium source of 5-30 mM and the molar ratio of the vanadium source to a sulfur source of 1 (0.5-12), performing microwave solvothermal reaction, and after full reaction, obtaining the rod-like V-modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material; the reaction temperature of the microwave solvothermal reaction is 60-120 ℃, the power is 200-400W, and the reaction time is 0.5-2 h;
the solvent of the suspension is absolute ethyl alcohol, ethylene glycol, a mixture of the absolute ethyl alcohol and water, or a mixture of the ethylene glycol and the water.
2. The rod-shaped self-assembled flower-ball-shaped V-modified Ni as claimed in claim 13S2The method of the electrocatalyst is characterized in that the vanadium source is vanadium pentoxide, sodium metavanadate, sodium vanadate, vanadium dodecahydrateOne or more of sodium, ammonium metavanadate and vanadyl acetylacetonate.
3. The rod-shaped self-assembled flower-ball-shaped V-modified Ni as claimed in claim 13S2The method of the electrocatalyst is characterized in that the sulfur source is one or more of thiourea, thioacetamide, sodium sulfide, sodium diethylthiocarbamate and elemental sulfur.
4. The rod-shaped self-assembled flower-ball-shaped V-modified Ni as claimed in claim 13S2The method of the electrocatalyst is characterized in that the foamed nickel is pretreated, is sequentially soaked in acetone and hydrochloric acid for ultrasonic cleaning, is alternately washed by ethanol and deionized water, and is dried to obtain the clean foamed nickel.
5. The rod-shaped self-assembled flower-ball-shaped V-modified Ni as claimed in claim 13S2The method of the electrocatalyst is characterized in that after the reaction is finished, the product is washed and dried to obtain the rod-shaped V modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
6. The rod-like self-assembled flower-ball-shaped V-modified Ni according to any one of claims 2 to 53S2The method for preparing the electrocatalyst is characterized by comprising the following specific steps of:
1) soaking the foam nickel to be treated in acetone for ultrasonic cleaning, soaking the foam nickel in 0.5-4 mol/L hydrochloric acid for ultrasonic cleaning, finally alternately washing with ethanol and deionized water respectively, and performing vacuum drying to obtain pretreated foam nickel; the ultrasonic cleaning is carried out for 5-15 min;
2) weighing a certain mass of a vanadium source and a sulfur source, controlling the molar ratio of the vanadium source to the sulfur source to be 1 (0.5-12), dissolving the vanadium source and the sulfur source in a proper amount of solvent to enable the concentration of the vanadium source to be 5-30 mM, and stirring for 3-20 min to obtain a suspension A;
3) placing the stirred suspension A and the foam nickel pretreated in the step 1) into a microwave hydrothermal instrument for reaction;
4) after the reaction is finished, the product is alternately washed for a plurality of times by deionized water and ethanol, and is dried in vacuum to obtain the rod-shaped V-modified Ni which is self-assembled into a flower ball shape3S2An electrocatalyst material.
7. The rod-shaped self-assembled flower-ball-shaped V-modified Ni as claimed in claim 63S2The method for preparing the electrocatalyst is characterized in that the vacuum drying in the step 1) and the step 4) is performed for 3-15 hours at the temperature of 10-60 ℃.
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| CN110180574B (en) * | 2019-06-05 | 2022-03-22 | 北京工业大学 | Preparation and application of nitrogen-doped ternary sulfide electrocatalyst material |
| CN110227496B (en) * | 2019-06-17 | 2022-05-06 | 安徽师范大学 | Microspherical Fe-doped trinickel disulfide nano-structure material composed of nanosheets, and preparation method and application thereof |
| CN111468140B (en) * | 2020-06-02 | 2022-11-29 | 陕西科技大学 | Ni 3 S 2 Preparation method of NiV-LDH heterogeneous nanocone electrocatalyst |
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