CN109225267B - Vanadium disulfide nanorod array electrocatalyst and preparation method thereof - Google Patents
Vanadium disulfide nanorod array electrocatalyst and preparation method thereof Download PDFInfo
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- CN109225267B CN109225267B CN201811266185.5A CN201811266185A CN109225267B CN 109225267 B CN109225267 B CN 109225267B CN 201811266185 A CN201811266185 A CN 201811266185A CN 109225267 B CN109225267 B CN 109225267B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention provides a vanadium disulfide nanorod array electrocatalyst, which is prepared by the following steps: soaking conductive carbon base in NaVO3：CH3CSNH2：C6H12N4The mass ratio is (0.1-0.5) (0.2-0.8): (0.5-1.5) in the solution, performing hydrothermal reaction to obtain uniform nano-rod-shaped VS2. The method has the advantages of low synthesis temperature, simple process, easy operation, cheap and easily-obtained raw materials, low cost, high yield, no need of post-treatment, environmental friendliness and suitability for large-scale production; the prepared product has uniform chemical composition, high purity and uniform appearance, can show excellent electrochemical performance when being used as an electrolytic water electrode material, and has an over potential of about 206mV under the current density of 10mA/cm 2.
Description
Technical Field
The invention belongs to the technical field of water electrolysis catalysts, and particularly relates to a vanadium disulfide nanorod array electrocatalyst and a preparation method thereof.
Background
The electrocatalytic water decomposition technology is a method for preparing hydrogen widely applied to industrial production at present due to simple process equipment, is the most potential technology for developing sustainable clean energy, and is also an important direction for research in the scientific research field. Platinum group noble metals such as Pt and Pd are the best catalysts for the electrolytic water-separation of ammonia, but are difficult to be widely applied to large-scale industrial production due to their high price, low earth reserves, easy poisoning, and the like, and thus the search for alternative electrolytic water catalysts is an important subject in this field. Research shows that vanadium has flexible valence state (+3, +4, +5) and excellent reaction activity, and the combination of the catalyst and the conducting substrate can promote charge transmission effectively and raise the catalytic activity and stability obviously.
The method adopts a high-efficiency, simple and low-cost one-step hydrothermal method, prepares the vanadium disulfide nanorod array on the carbon cloth substrate, and effectively improves the conductivity, thereby improving the hydrogen evolution performance of electrolyzed water.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the preparation method of the vanadium disulfide nanorod array catalyst, which is simple to operate, mild in reaction condition, short in time consumption, high in purity of the prepared vanadium disulfide product, uniform in appearance and size, and excellent in electrocatalytic hydrogen evolution performance.
In order to achieve the above object, the present invention adopts the following technical solutions.
(1) Cutting the carbon cloth into rectangles of 1 x 5cm, performing reflux activation for 1-3 hours at 80-120 ℃, then respectively cleaning for 3-5 times by using ethanol and deionized water, and drying for 6-8 hours at 40-70 ℃ to obtain the treated carbon cloth;
(2) separately weighing (0.1 g-0.5 g) NaVO3、(0.2g~0.8g) CH3CSNH2And (0.5 g-1.5 g) C6H12N4Dissolving the mixture in 20-40 ml of deionized water, and magnetically stirring the mixture at room temperature for 40-60 min to obtain a clear solution;
(3) putting the carbon cloth treated in the step (1) into a reaction lining, pouring the clear solution obtained in the step (2), sealing for hydrothermal reaction, setting the reaction temperature to be 160-220 ℃ and the reaction time to be 18-30 h;
(4) after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the carbon cloth, respectively cleaning the carbon cloth for 3 times by using ethanol and deionized water, and finally drying the carbon cloth for 5-8 hours at the temperature of 40-70 ℃ to obtain uniform nano-rod-shaped VS2。
The invention has the beneficial effects that:
(1) the method adopts one-step hydrothermal reaction to directly synthesize the final product, so that the method has the advantages of low synthesis temperature, simple process, easy operation, cheap and easily-obtained raw materials, low cost, high yield, no need of post-treatment, environmental friendliness and suitability for large-scale production;
(3) the product prepared by the method has uniform chemical composition, high purity and uniform appearance, can show excellent electrochemical performance when being used as an electrolytic water electrode material, and has the electrochemical performance of 10mA/cm2The overpotential of (2) is about 206mV at the current density of (2).
Drawings
FIG. 1 is VS grown on carbon cloth prepared in example 3 of the present invention2An X-ray diffraction (XRD) pattern of the nanorod array;
FIG. 2 is VS grown on carbon cloth prepared in example 3 of the present invention2Scanning Electron Microscope (SEM) photographs of the nanorod arrays;
FIG. 3 is VS grown on carbon cloth prepared in example 3 of the present invention2Linear Sweep Voltammetry (LSV) performance test plots for nanorod arrays.
Detailed Description
The invention is explained in more detail below with reference to the drawings and the examples:
example 1:
(1) cutting the carbon cloth into a rectangle of 1 x 5cm, performing reflux activation in concentrated nitric acid at 80-120 ℃ for 1-3 hours, then respectively cleaning 3 times by using ethanol and deionized water, and drying for 8 hours at 50 ℃ to obtain the treated carbon cloth;
(2) 0.1g NaVO was weighed out separately3、0.2g TAA（CH3CSNH2) And 0.5g C6H12N4Dissolving in 20ml deionized water, and magnetically stirring at room temperature for 40min to obtain a clear solution;
(3) putting the carbon cloth treated in the step (1) into a reaction lining, pouring the clear solution obtained in the step (2), sealing to perform hydrothermal reaction, setting the reaction temperature to be 160 ℃, and setting the reaction time to be 18 h;
(4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, the carbon cloth is taken out, then ethanol and deionized water are respectively used for cleaning for 3 times, and finally the carbon cloth is dried for 8 hours at 50 ℃ to obtain uniform nano-rod-shaped VS2。
Example 2:
(1) cutting the carbon cloth into a rectangle with the size of 1 multiplied by 5cm, refluxing and activating in concentrated nitric acid at the temperature of 80 ℃ for 2 hours, then respectively cleaning with ethanol and deionized water for 4 times, and drying at the temperature of 50 ℃ for 8 hours to obtain the treated carbon cloth;
(2) 0.3g of NaVO was weighed out separately3、0.9g TAA（CH3CSNH2) And 0.8g C6H12N4Dissolving in 30ml deionized water, and magnetically stirring at room temperature for 40min to obtain a clear solution;
(3) putting the carbon cloth treated in the step (1) into a reaction lining, pouring the clear solution obtained in the step (2), sealing to perform hydrothermal reaction, setting the reaction temperature to be 200 ℃ and the reaction time to be 22 h;
(4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, the carbon cloth is taken out, then ethanol and deionized water are respectively used for cleaning for 3 times, and finally the carbon cloth is dried for 8 hours at 50 ℃ to obtain uniform nano-rod-shaped VS2。
Example 3:
(1) cutting the carbon cloth into a rectangle with the size of 1 multiplied by 5cm, refluxing and activating in concentrated nitric acid at the temperature of 80 ℃ for 2 hours, then respectively cleaning with ethanol and deionized water for 5 times, and drying at the temperature of 60 ℃ for 7 hours to obtain the treated carbon cloth;
(2) 0.4g NaVO was weighed out separately3、1.2g TAA（CH3CSNH2) And 1.2g C6H12N4Dissolving in 35ml deionized water, and magnetically stirring at room temperature for 60min to obtain a clear solution;
(3) putting the carbon cloth treated in the step (1) into a reaction lining, pouring the clear solution obtained in the step (2), sealing to perform hydrothermal reaction, setting the reaction temperature to be 180 ℃ and the reaction time to be 24 hours;
(4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, the carbon cloth is taken out, then the carbon cloth is respectively washed for 3 times by ethanol and deionized water, and finally the carbon cloth is dried for 7 hours at the temperature of 60 ℃, so that the uniform nano-rod-shaped VS is obtained2。
FIG. 1 shows VS growth on carbon cloth prepared in this example2X-ray diffraction of nanorod arraysJet (XRD) pattern. In the figure, the characteristic peak and VS in the XRD test result2The characteristic peaks are consistent, which shows that VS grows on carbon base2。
FIG. 2 is VS grown on carbon cloth prepared in example 3 of the present invention2Scanning Electron Microscope (SEM) photograph of nanorod array. SEM photograph shows that VS is grown on carbon base2Has irregular nanorod array morphology.
FIG. 3 is VS grown on carbon cloth prepared in example 3 of the present invention2Linear Sweep Voltammetry (LSV) performance test plots for nanorod arrays. LSV performance test shows that the temperature is 50mA/cm2The overpotential thereof is about 509mV at the current density of (1); at 100mA/cm2The overpotential of (2) is about 583mV at the current density of (3).
Example 4:
(1) cutting the carbon cloth into a rectangle of 1 × 5cm, performing reflux activation in concentrated nitric acid at 100 ℃ for 1 hour, then respectively cleaning with ethanol and deionized water for 4 times, and drying at 70 ℃ for 6 hours to obtain the treated carbon cloth;
(2) 0.5g NaVO was weighed out separately3、0.8g TAA（CH3CSNH2) And 1.5g C6H12N4Dissolving in 40ml deionized water, and magnetically stirring at room temperature for 60min to obtain a clear solution;
(3) placing the carbon cloth treated in the step (1) into a reaction lining, pouring the clear solution obtained in the step (2), sealing to perform hydrothermal reaction, setting the reaction temperature at 220 ℃ and the reaction time at 28 h;
(4) after the reaction is finished, the reaction kettle is naturally cooled to room temperature, the carbon cloth is taken out, then the carbon cloth is respectively washed for 3 times by ethanol and deionized water, and finally the carbon cloth is dried for 6 hours at 70 ℃, so that the uniform nano-rod-shaped VS is obtained2。
Claims (4)
1. A preparation method of a vanadium disulfide nanorod array electrocatalyst is characterized by comprising the following steps:
taking 0.1-0.5 g of NaVO30.2g to 0.8g of CH3CSNH2And 0.5g to1.5g of C6H12N4Dissolving the precipitate in 20-40 mL of deionized water, and magnetically stirring at room temperature for 40-60 min to obtain a clear solution; and soaking the conductive carbon base in the solution, and carrying out hydrothermal reaction at 160-220 ℃ for 18-30 h to obtain the uniform vanadium disulfide nanorod array electrocatalyst.
2. The method for preparing the vanadium disulfide nanorod array electrocatalyst according to claim 1, wherein the conductive carbon group is activated carbon cloth.
3. The method for preparing the vanadium disulfide nanorod array electrocatalyst according to claim 2, wherein the activated carbon cloth is obtained by a method comprising the following steps: and (3) carrying out reflux activation on the carbon cloth in concentrated nitric acid at the temperature of 80-120 ℃ for 1-3 hours, then respectively cleaning the carbon cloth with ethanol and deionized water for 3-5 times, and drying the carbon cloth at the temperature of 40-70 ℃ for 6-8 hours to obtain the treated carbon cloth.
4. The method for preparing the vanadium disulfide nanorod array electrocatalyst according to claim 1, comprising the following specific steps:
1) cutting the carbon cloth into rectangles of 1 x 5cm, performing reflux activation in concentrated nitric acid at 80-120 ℃ for 1-3 hours, then respectively cleaning 3-5 times by using ethanol and deionized water, and drying at 40-70 ℃ for 6-8 hours to obtain treated carbon cloth;
2) respectively weighing 0.1-0.5 g of NaVO30.2g to 0.8g of CH3CSNH2And 0.5g to 1.5g of C6H12N4Dissolving the precipitate in 20-40 mL of deionized water, and magnetically stirring at room temperature for 40-60 min to obtain a clear solution;
3) putting the carbon cloth treated in the step 1) into a reaction lining, pouring the clear solution obtained in the step 2), sealing for hydrothermal reaction, setting the reaction temperature to be 160-220 ℃ and the reaction time to be 18-30 h;
4) and after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the carbon cloth, respectively cleaning the carbon cloth for 3 times by using ethanol and deionized water, and finally drying the carbon cloth for 5-8 hours at the temperature of 40-70 ℃ to obtain the uniform vanadium disulfide nanorod array electrocatalyst.
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| CN109650493B (en) * | 2019-01-22 | 2021-09-07 | 陕西科技大学 | VS with hierarchical structure2Synthesis method of nanosheet array electrode material |
| CN110227494A (en) * | 2019-07-05 | 2019-09-13 | 陕西科技大学 | A kind of preparation method of vanadium disulfide/tetra- five vanadium composite electrocatalysts of vulcanization |
| CN110396598A (en) * | 2019-07-22 | 2019-11-01 | 广东环境保护工程职业学院 | A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles |
| CN114142048B (en) * | 2021-11-30 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Electrode modification method for vanadium battery |
| CN114142043B (en) * | 2021-11-30 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical performance of electrode for vanadium battery |
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| CN107902697B (en) * | 2017-11-02 | 2019-09-17 | 陕西科技大学 | A kind of nanometer sheet self assembled three-dimensional VS of (001) orientation2Micron bar and preparation method thereof |
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