CN109110812B - 3D multilevel structure VS2Hydrogen evolution electrocatalyst and preparation method thereof - Google Patents
3D multilevel structure VS2Hydrogen evolution electrocatalyst and preparation method thereof Download PDFInfo
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- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 53
- 239000004744 fabric Substances 0.000 claims abstract description 50
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 229910020700 Na3VO4 Inorganic materials 0.000 claims abstract description 7
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract 2
- 238000002791 soaking Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 229920000463 Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) Polymers 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- 239000011593 sulfur Substances 0.000 claims description 7
- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 3
- 239000002057 nanoflower Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002135 nanosheet Substances 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- -1 polyethylene Polymers 0.000 abstract description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract 1
- 239000004698 Polyethylene Substances 0.000 abstract 1
- 239000004743 Polypropylene Substances 0.000 abstract 1
- 229920000573 polyethylene Polymers 0.000 abstract 1
- 229920001155 polypropylene Polymers 0.000 abstract 1
- 229920000428 triblock copolymer Polymers 0.000 abstract 1
- NGTSQWJVGHUNSS-UHFFFAOYSA-N bis(sulfanylidene)vanadium Chemical compound S=[V]=S NGTSQWJVGHUNSS-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000003213 activating effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- FHANEPRSLAMSJU-UHFFFAOYSA-N vanadium(4+);disulfide Chemical compound [S-2].[S-2].[V+4] FHANEPRSLAMSJU-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
-
- B01J35/33—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention provides a 3D multilevel VS2Hydrogen evolution electrocatalyst having a composition of VS2The flower-ball-shaped appearance formed by stacking the nanosheets is prepared by the following steps: soaking the conductive carbon base in a solution containing (1-3) mol ratio (4-6) mol ratio0.1 to 0.4) of Na3VO4·12H2O、CH3CSNH2And in the dispersion of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (PEO-PPO-PEO), carrying out hydrothermal reaction to obtain the 3D multi-stage structure VS2A hydrogen evolution electrocatalyst. The nano-sheet prepared by the method grows on the carbon cloth substrate to form a 3D multi-level structure nano-flower. The nanoflower with the 3D multilevel structure is very favorable for free entry and exit of ions, so that more active sites are exposed, and the electro-catalytic hydrogen evolution performance is improved.
Description
Technical Field
The invention belongs to the technical field of electrocatalytic hydrogen evolution catalysts, and particularly relates to a 3D multi-stage structure VS2A hydrogen evolution electrocatalyst and a preparation method thereof.
Background
The transition metal disulfide has unique electrochemical property and catalytic property, can be widely applied to the field of energy sources, such as lithium battery electrodes, catalysts and the like, and is a very important material. In particular vanadium disulphide (VS)2) Is particularly concerned by people.
The vanadium disulfide has a unique layered structure, is beneficial to the adsorption and the desorption of ions, can be embedded with metal ions such as Li and the like in different proportions, and can be used as an electrode material, thereby greatly improving the property of the electrode. With the further understanding of the properties of the vanadium disulfide, the application fields and the application modes of the vanadium disulfide must be greatly widened, and the social benefit and the economic benefit are generated.
At present, with respect to VS2Reports of solution growth of nanostructures are very limited, and more importantly, they are all prepared in powder form, which requires additional binders (e.g., Nafion), to assist in the film casting or coating procedure. The obtained electrode has limited active area (blocked by the binder)Plugs) diffusion is slow and conductivity is poor. To further increase VS2Direct growth of VS on a conductive substrate with a large surface area2Nanostructures are of critical importance. In the patent, a 3D multilevel structure VS is realized on a carbon cloth substrate2The product has good hydrogen evolution activity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the preparation method of the vanadium disulfide with the 3D hierarchical structure, the method is simple to operate, the reaction condition is mild, and the prepared VS is2The product has high purity and uniform appearance and size. 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 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 50-70 ℃ for 6-8 hours to obtain treated carbon cloth;
(2) separately weighing Na3VO4·12H2O、TAA（CH3CSNH2) And PEO-PPO-PEO, the molar ratio is (1-3): (4-6): 0.1-0.3), the solution is dissolved in 25-40 ml deionized water, the concentration of the vanadium source is (0.02-0.075) mol/L, the concentration of the sulfur source is (0.1-0.15) mol/L, the concentration of the PEO-PPO-PEO is (0.0025-0.0075) mol/L, and the solution is magnetically stirred 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 160-200 ℃ and the reaction time to be 18-28 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 50-70 ℃ to obtain the 3D multi-stage structure VS2。
Further, PEO-PPO-PEO employs P123 (PEO)20PPO70PEO20）
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;
(2) the product prepared by the method has uniform chemical composition, high purity and uniform appearance;
(3) the nano-sheet prepared by the method grows on the carbon cloth substrate to form a 3D multi-level structure nano-flower. The nanoflower with the 3D multilevel structure is very favorable for free entry and exit of ions, so that more active sites are exposed, and the electro-catalytic hydrogen evolution performance is improved.
Drawings
FIG. 1 is a graph of VS grown on carbon cloth prepared in example 1 of the present invention2An X-ray diffraction (XRD) pattern of the nanoflower array;
FIG. 2 is VS grown on carbon cloth prepared in example 2 of the present invention2A Scanning Electron Microscope (SEM) photograph of the nanoflower array at 1100 x magnification;
FIG. 3 is VS grown on carbon cloth prepared in example 2 of the present invention2A Scanning Electron Microscope (SEM) photograph of the nanoflower array at 450 x magnification;
FIG. 4 is VS grown on carbon cloth prepared in example 3 of the present invention2Linear Sweep Voltammetry (LSV) performance test plots of nanoflower 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, refluxing and activating in concentrated nitric acid at 120 ℃ for 1 hour, then respectively cleaning with ethanol and deionized water for 3 times, and drying at 50 ℃ for 8 hours to obtain the treated carbon cloth;
(2) separately weighing Na3VO4·12H2O、TAA（CH3CSNH2) And P123 (PEO)20PPO70PEO20) The molar ratio is 1: 4: 0.1, dissolving in 25ml of deionized water, wherein the concentration of the vanadium source is 0.04mol/LMagnetically stirring the mixture at room temperature for 40min to obtain a clear solution, wherein the concentration of a sulfur source is 0.133mol/L and the concentration of P123 is 0.0033 mol/L;
(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, 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 8 hours at 50 ℃ to obtain the uniform 3D multi-stage structure nano flower-shaped VS2。
FIG. 1 shows VS growth on carbon cloth prepared in this example2An X-ray diffraction (XRD) pattern of the nanoflower array. From fig. 1, it can be seen that the surface of the carbon cloth is grown with material, and the product is VS2, which has a very high degree of crystallinity.
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) separately weighing Na3VO4·12H2O、TAA（CH3CSNH2) And P123 (PEO)20PPO70PEO20) The molar ratio is 1.5: 5: 0.2, dissolving in 35ml of deionized water, wherein the concentration of a vanadium source is 0.043mol/L, the concentration of a sulfur source is 0.143mol/L, and the concentration of P123 is 0.0057mol/L, 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 180 ℃ and the reaction time to be 22 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 8 hours at 50 ℃ to obtain the uniform 3D multi-stage structure nano flower-shaped VS2。
FIG. 2 and FIG. 3 show the growth of the present exampleVS on carbon cloth2Scanning Electron Microscope (SEM) photographs of the nanoflower array. It can be seen from the SEM images of fig. 2 and 3 that the sample is a 3D nanoflower structure grown on a carbon cloth.
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) separately weighing Na3VO4·12H2O、TAA（CH3CSNH2) And P123 (PEO)20PPO70PEO20) The molar ratio is 2: 4.5: 0.2, dissolving in 35ml of deionized water, wherein the concentration of a vanadium source is 0.057mol/L, the concentration of a sulfur source is 0.128mol/L, the concentration of P123 is 0.0057mol/L, 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, 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 7 hours at the temperature of 60 ℃ to obtain the uniform 3D multi-stage structure nano flower-shaped VS2。
FIG. 4 shows VS growth on carbon cloth prepared in this example2Linear Sweep Voltammetry (LSV) performance test plots of nanoflower arrays. As can be seen from the linear scanning voltammogram of FIG. 4, the sample has a current density of 10mA/cm2When the overpotential is 305mV, the current density is 50mA/cm2Its overpotential is 407 mV. Has good electrocatalytic hydrogen evolution activity.
Example 4:
(1) cutting the carbon cloth into a rectangle of 1 × 5cm, performing reflux activation in concentrated nitric acid at 120 ℃ for 3 hours, 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) separately weighing Na3VO4·12H2O、TAA（CH3CSNH2) And P123 (PEO)20PPO70PEO20) The molar ratio is 3: 6: 0.3, dissolving in 40ml of deionized water, wherein the concentration of a vanadium source is 0.075mol/L, the concentration of a sulfur source is 0.15mol/L, the concentration of P123 is 0.0075mol/L, 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 200 ℃ and the reaction time to be 28 hours;
(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 6 hours at 70 ℃ to obtain the uniform 3D multi-stage structure nano flower-shaped VS2。
Claims (4)
1. 3D multilevel structure VS2The preparation method of the hydrogen evolution electrocatalyst is characterized by comprising the following steps of:
soaking conductive carbon base in Na-containing solution3VO4·12H2O、CH3CSNH2And in the dispersion of PEO-PPO-PEO, the concentration of a vanadium source is 0.025-0.075 mol/L, the concentration of a sulfur source is 0.1-0.15 mol/L, and the concentration of PEO-PPO-PEO is 0.0025-0.0075 mol/L; then carrying out hydrothermal reaction at the reaction temperature of 160-200 ℃ for 18-28 h to obtain the 3D multi-stage structure VS2A hydrogen evolution electrocatalyst;
Na3VO4·12H2O：CH3CSNH2: the molar ratio of PEO-PPO-PEO is (1-3) to (4-6) to (0.1-0.3).
2. 3D multilevel structure VS according to claim 12The preparation method of the hydrogen evolution electrocatalyst is characterized in that the conductive carbon base is carbon cloth.
3. 3D multilevel structure VS according to claim 22Preparation of hydrogen evolution electrocatalystThe preparation method is characterized in that the carbon cloth is activated by refluxing for 1-3 hours at 80-120 ℃ before use.
4. A3D multilevel structure VS according to any of claims 1-32The preparation method of the hydrogen evolution electrocatalyst is characterized by comprising the following specific steps of:
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 50-70 ℃ for 6-8 hours to obtain treated carbon cloth;
2) respectively weighing Na with the molar ratio of (1-3) to (4-6) to (0.1-0.3)3VO4·12H2O、CH3CSNH2And dissolving PEO-PPO-PEO in 25-40 mL of deionized water, wherein the concentration of a vanadium source is 0.025-0.075 mol/L, the concentration of a sulfur source is 0.1-0.15 mol/L, and the concentration of PEO-PPO-PEO is 0.0025-0.0075 mol/L, 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, and carrying out hydrothermal reaction, wherein the reaction temperature is set to be 160-200 ℃, and the reaction time is 18-28 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 50-70 ℃ to obtain the 3D multi-stage structure VS2。
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| CN110064409B (en) * | 2019-05-10 | 2022-03-11 | 深圳大学 | Pt/VS2Catalytic material, preparation method and application thereof |
| CN111715249B (en) * | 2020-07-22 | 2023-03-24 | 陕西科技大学 | Spherical FeP electrocatalyst and preparation method thereof |
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