CN110801854A - Electrocatalyst composed of molybdenum disulfide coated silicon carbide nanowires and preparation method thereof - Google Patents
Electrocatalyst composed of molybdenum disulfide coated silicon carbide nanowires and preparation method thereof Download PDFInfo
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- CN110801854A CN110801854A CN201911077153.5A CN201911077153A CN110801854A CN 110801854 A CN110801854 A CN 110801854A CN 201911077153 A CN201911077153 A CN 201911077153A CN 110801854 A CN110801854 A CN 110801854A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 66
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 47
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- 239000002070 nanowire Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002135 nanosheet Substances 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 20
- 239000001257 hydrogen Substances 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 239000011733 molybdenum Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001308 synthesis method Methods 0.000 claims description 10
- 238000004891 communication Methods 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 239000012808 vapor phase Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 11
- 230000009286 beneficial effect Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- -1 molybdate ions Chemical class 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 230000010287 polarization Effects 0.000 description 5
- 229920000557 Nafion® Polymers 0.000 description 3
- 241000571645 Sabellastarte magnifica Species 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
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- 239000007864 aqueous solution Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910021397 glassy carbon Inorganic materials 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
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- 229910052961 molybdenite Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- 238000005054 agglomeration Methods 0.000 description 1
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
Images
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- 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
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
- B01J27/224—Silicon carbide
-
- 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
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/23—
-
- B01J35/33—
-
- 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
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- 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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 discloses an electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires and a preparation method thereof, belonging to the field of inorganic nanometer functional materials. The electrocatalyst is composed of 83.3-98.8% of molybdenum disulfide and 1.2-16.7% of silicon carbide by mass percentage; the molybdenum disulfide is a molybdenum disulfide nanosheet, the silicon carbide is a silicon carbide nanowire, and the molybdenum disulfide nanosheet is uniformly coated on the silicon carbide nanowire to form a one-dimensional nanostructure. The preparation method of the electrocatalyst adopted by the invention is an in-situ hydrothermal method, and as the surface of the silicon carbide is positively charged, molybdate ions are preferentially adsorbed on the surface of the silicon carbide, and under the hydrothermal condition, through carbon-molybdenum bond combination, a good interface can be formed between molybdenum disulfide and silicon carbide, thus being beneficial to improving the structure and catalytic stability of the material, and the method has simple process and is beneficial to large-scale production.
Description
Technical Field
The invention belongs to the field of inorganic nano functional materials, and particularly relates to an electrocatalyst formed by molybdenum disulfide-coated silicon carbide nanowires and a preparation method thereof.
Background
With the increasing prominence of the energy crisis and environmental pollution problems caused by fossil fuel consumption, hydrogen energy is attracting more and more attention as a renewable clean energy source. The hydrogen production by electrolysis of water is recognized as a promising hydrogen production mode with high energy conversion efficiency and zero emission, wherein the design and development of novel electrocatalytic materials are the key of the application of the electrocatalytic hydrogen production technology. Noble metals have the highest electrocatalytic hydrogen production performance, but their high cost and rarity limit their industrial applications.
The molybdenum disulfide has the advantages of low cost and good catalytic performance, and can be an ideal substitute material of noble metals. Theoretical and experimental results show that: the edge of the molybdenum disulfide nanosheet has high hydrogen production catalytic activity. However, the molybdenum disulfide used for electrocatalytic hydrogen production has the defects of low conductivity, easy stacking and agglomeration of nanosheets and high water activation energy barrier. The defects are overcome by compounding with other nano materials, and the electrocatalytic hydrogen production performance of the molybdenum disulfide can be expected to be further improved.
Silicon carbide is a common semiconductor and has the advantages of low cost, high stability, good conductivity, environmental friendliness and the like. The water molecules can be catalytically decomposed into-H and-OH on the surface of the silicon carbide nano-crystal, so that the silicon carbide nano-material can reduce the water activation energy barrier, thereby being beneficial to improving the electro-catalytic hydrogen production performance. In 2013, Guo and its collaborators assembled silicon carbide and molybdenum disulfide nanosheets into a nanoflower-shaped material, which showed higher photocatalytic performance. In 2018, Wang and coworkers prepared the nano flower-shaped material through self-assembly of the silicon carbide nanoparticles and the molybdenum disulfide nanosheets, and the nano flower-shaped material has high carbon dioxide catalytic reduction performance. The silicon carbide nanosheets and nanoparticles are mainly used at present, and the problems of low conductivity, insufficient catalytic activity and the like exist. Compared with a silicon carbide nanosheet and nanoparticles, the high-communication silicon carbide nanowire composite molybdenum disulfide has higher conductivity and larger specific surface area, and is beneficial to the dispersion of the molybdenum disulfide nanosheet, so that the catalytic activity of the material is improved. Compared with a two-step assembly method, a good interface can be formed between the molybdenum disulfide and the silicon carbide by adopting an in-situ hydrothermal method, and the stability of the material is improved. In addition, no report about the direct application of the molybdenum disulfide composite silicon carbide nanowire to electrocatalysis hydrogen production is found.
Disclosure of Invention
The invention aims to provide an electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires and a preparation method thereof, the electrocatalyst has a microstructure similar to a feather duster, can be used for electrocatalytic hydrogen evolution reaction, and has the advantages of high catalytic activity, stable catalytic performance and the like.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses an electrocatalyst formed by molybdenum disulfide-coated silicon carbide nanowires, which consists of 83.3 to 98.8 mass percent of molybdenum disulfide and 1.2 to 16.7 mass percent of silicon carbide; the molybdenum disulfide is a molybdenum disulfide nanosheet, the silicon carbide is a silicon carbide nanowire, and the molybdenum disulfide nanosheet is uniformly coated on the silicon carbide nanowire to form a one-dimensional nanostructure.
Preferably, the micro-morphology of the electrocatalyst is a one-dimensional nano material, the diameter is 35-145 nm, and the length is 20-500 μm.
Preferably, the electrocatalyst has electrocatalytic hydrogen production performance, and the Tafel slope and the starting point position of the electrocatalyst are respectively 54-57 mV/dec and 75-89 mV.
The invention also discloses a preparation method of the electrocatalyst formed by the molybdenum disulfide coated silicon carbide nanowire, which comprises the following steps:
1) adding the high-communication silicon carbide nanowires prepared by the vapor phase synthesis method into water, and uniformly stirring to obtain a suspension; wherein the diameter of the high-communication silicon carbide nanowire prepared by the gas phase synthesis method is 20-100nm, and the length of the high-communication silicon carbide nanowire is 20-500 mu m;
2) adding a molybdenum source and a sulfur source into the suspension obtained in the step 1), and uniformly stirring, wherein the molar ratio of the molybdenum source to the sulfur source is 0.35-0.55;
3) carrying out hydrothermal reaction on the suspension added with the molybdenum source and the sulfur source in the step 2);
4) centrifuging and washing the reaction product obtained in the step 3), and drying to obtain the molybdenum disulfide coated silicon carbide nanowire electrocatalyst.
Preferably, in the step 1), the reaction dosage of the high-communication silicon carbide nanowire prepared by the gas-phase synthesis method and water is 0.010 g: (50-60) mL.
Preferably, the mass ratio of the added molybdenum source to the high-communication silicon carbide nanowire is (60-150): 1.
preferably, in the step 1) and the step 2), the stirring time is 10-30 min.
Preferably, in the step 2), the molybdenum source is one or two of ammonium molybdate and sodium molybdate; the sulfur source is one or two of thioacetamide and thiourea.
Preferably, in the step 3), the temperature of the hydrothermal reaction is 180-.
Preferably, in the step 4), the temperature of the drying treatment is 60-90 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the electro-catalyst formed by the molybdenum disulfide-coated silicon carbide nanowire disclosed by the invention fully utilizes the hydrogen production catalytic activity of the molybdenum disulfide nanosheet and the good conductivity and low water activation energy barrier of the silicon carbide nanowire, and the two cooperate to jointly enhance the electro-catalytic hydrogen production performance of the material. From the structure, the electrocatalyst has a novel microstructure similar to a feather duster, and utilizes one-dimensional/two-dimensional material hybridization to expose the active sites at the edges of the molybdenum disulfide nanosheets, thereby being beneficial to fully exerting the catalytic activity of molybdenum disulfide.
The preparation method of the electrocatalyst adopted by the invention is an in-situ hydrothermal method, and as the surface of the silicon carbide is positively charged, molybdate ions are preferentially adsorbed on the surface of the silicon carbide, and under the hydrothermal condition, through carbon-molybdenum bond combination, a good interface can be formed between molybdenum disulfide and silicon carbide, thus being beneficial to improving the structure and catalytic stability of the material, and the method has simple process and is beneficial to large-scale production.
Drawings
FIG. 1 is (a) an SEM image, (b) low power and (c) high power TEM images of a molybdenum disulfide coated silicon carbide nanowire electrocatalyst prepared according to the present invention, (d) elemental distribution diagrams;
FIG. 2 is an XRD spectrum of a molybdenum disulfide coated silicon carbide nanowire electrocatalyst, a silicon carbide nanowire and hydrothermally synthesized molybdenum disulfide prepared in the present invention;
FIG. 3 is a hydrogen production polarization curve of the molybdenum disulfide-coated silicon carbide nanowire electrocatalyst, the silicon carbide nanowire and the hydrothermally synthesized molybdenum disulfide prepared by the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
the high-connectivity silicon carbide nanowire prepared by the gas phase synthesis method is the silicon carbide nanowire prepared by the method disclosed in the patent with the publication number of CN 107188527A.
Example 1:
a preparation method of an electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires comprises the following steps of adding 0.010g of high-connectivity silicon carbide nanowires prepared by a vapor phase synthesis method into 60mL of deionized water, and stirring for 30 minutes; then adding 1.210g of sodium molybdate and 1.503g of thioacetamide, and stirring for 30 minutes; transferring the suspension into a 100mL hydrothermal kettle, and carrying out hydrothermal reaction at 220 ℃ for 24 h; and (3) centrifugally washing the hydrothermal reaction product, and drying at 60 ℃ to obtain the molybdenum disulfide coated silicon carbide nano-wire electrocatalyst.
Fig. 1 is an SEM image (a), a low-magnification TEM image (b), a high-magnification TEM image (c), and an element distribution diagram (d) of the molybdenum disulfide-coated silicon carbide nanowire electrocatalyst manufactured in this embodiment, which shows that molybdenum disulfide nanosheets are uniformly coated on the silicon carbide nanowire, and the microstructure thereof is similar to a feather duster. FIG. 2 is the XRD spectrum, showing diffraction peaks of molybdenum disulfide and silicon carbide.
A typical three-electrode system is adopted to test the catalytic hydrogen production performance of the molybdenum disulfide coated silicon carbide nano-wire electrocatalyst, a 0.5M sulfuric acid solution is used as an electrolyte, and an Ag/AgCl electrode and a platinum electrode are respectively used as a reference electrode and a counter electrode. 4mg of the molybdenum disulfide-coated silicon carbide nanowire electrocatalyst prepared in the embodiment and 30 μ L of nafion solution (5 wt.%) are dispersed in 1mL of ethanol aqueous solution (the volume ratio of water to ethanol is 3:1), and after 30 minutes of ultrasonic treatment, 5 μ L of the solution is dropped on a glassy carbon electrode with the thickness of 3 square millimeters to serve as a working electrode. The scan rate was 5mV/s and the polarization curve of the electrocatalyst was tested. FIG. 3 is a graph showing the polarization curves obtained, in FIG. 3, the red line (uppermost) represents SiCnw, and the blue line (middle) represents MoS2The black line (lower) represents MoS2the/SiCnw shows good electrocatalytic hydrogen production performance, and the Tafel slope and the starting point are 54mV/dec and 88mV respectively.
Example 2:
a preparation method of an electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires comprises the following steps of adding 0.010g of high-connectivity silicon carbide nanowires prepared by a vapor phase synthesis method into 60mL of deionized water, and stirring for 30 minutes; then 0.605g of sodium molybdate and 0.751g of thioacetamide are added and stirred for 30 minutes; transferring the suspension into a 100mL hydrothermal kettle, and carrying out hydrothermal reaction at 220 ℃ for 24 h; and (3) centrifugally washing the hydrothermal reaction product, and drying at 60 ℃ to obtain the molybdenum disulfide coated silicon carbide nano-wire electrocatalyst.
A typical three-electrode system is adopted to test the catalytic hydrogen production performance of the molybdenum disulfide coated silicon carbide nano-wire electrocatalyst, a 0.5M sulfuric acid solution is used as an electrolyte, and an Ag/AgCl electrode and a platinum electrode are respectively used as a reference electrode and a counter electrode. 4mg of catalyst and 30. mu.L of nafion solution (5 wt.%) are dispersed in 1mL of ethanol aqueous solution (the volume ratio of water to ethanol is 3:1), and after 30 minutes of ultrasonic treatment, 5. mu.L of solution is dropped onto a glassy carbon electrode with the thickness of 3 square millimeters to serve as a working electrode. The sweep rate was 5mV/s and the polarization curve of the electrocatalyst was tested and had a Tafel slope of 77 mV/dec.
Example 3:
a preparation method of an electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires comprises the following steps of adding 0.010g of high-connectivity silicon carbide nanowires prepared by a vapor phase synthesis method into 60mL of deionized water, and stirring for 30 minutes; then 2.420g of sodium molybdate and 3.006g of thioacetamide are added and stirred for 30 minutes; transferring the suspension into a 100mL hydrothermal kettle, and carrying out hydrothermal reaction at 220 ℃ for 24 h; and (3) centrifugally washing the hydrothermal reaction product, and drying at 60 ℃ to obtain the molybdenum disulfide coated silicon carbide nano-wire electrocatalyst.
A typical three-electrode system is adopted to test the catalytic hydrogen production performance of the molybdenum disulfide coated silicon carbide nano-wire electrocatalyst, a 0.5M sulfuric acid solution is used as an electrolyte, and an Ag/AgCl electrode and a platinum electrode are respectively used as a reference electrode and a counter electrode. 4mg of catalyst and 30. mu.L of nafion solution (5 wt.%) are dispersed in 1mL of ethanol aqueous solution (the volume ratio of water to ethanol is 3:1), and after 30 minutes of ultrasonic treatment, 5. mu.L of solution is dropped onto a glassy carbon electrode with the thickness of 3 square millimeters to serve as a working electrode. The sweep rate was 5mV/s and the polarization curve of the electrocatalyst was tested with a Tafel slope of 56 mV/dec.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. An electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires is characterized in that the electrocatalyst consists of 83.3-98.8% of molybdenum disulfide and 1.2-16.7% of silicon carbide in percentage by mass; the molybdenum disulfide is a molybdenum disulfide nanosheet, the silicon carbide is a silicon carbide nanowire, and the molybdenum disulfide nanosheet is uniformly coated on the silicon carbide nanowire to form a one-dimensional nanostructure.
2. The electrocatalyst made of molybdenum disulfide coated silicon carbide nanowires as claimed in claim 1, wherein the electrocatalyst has a one-dimensional nanomaterial in its micro-morphology, a diameter of 35-145 nm and a length of 20-500 μm.
3. The electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires as claimed in claim 1, wherein the electrocatalyst has electrocatalytic hydrogen production performance, and the tafel slope and the starting point position are 54-57 mV/dec and 75-89 mV respectively.
4. The method for preparing the electrocatalyst formed by the molybdenum disulfide coated silicon carbide nanowires as claimed in any one of claims 1 to 3, comprising the steps of:
1) adding the high-communication silicon carbide nanowires prepared by the vapor phase synthesis method into water, and uniformly stirring to obtain a suspension; wherein the diameter of the high-communication silicon carbide nanowire prepared by the gas phase synthesis method is 20-100nm, and the length of the high-communication silicon carbide nanowire is 20-500 mu m;
2) adding a molybdenum source and a sulfur source into the suspension obtained in the step 1), and uniformly stirring, wherein the molar ratio of the molybdenum source to the sulfur source is 0.35-0.55;
3) carrying out hydrothermal reaction on the suspension added with the molybdenum source and the sulfur source in the step 2);
4) centrifuging and washing the reaction product obtained in the step 3), and drying to obtain the molybdenum disulfide coated silicon carbide nanowire electrocatalyst.
5. The method for preparing the electrocatalyst composed of molybdenum disulfide coated silicon carbide nanowires according to claim 4, wherein in step 1), the reaction amount of the high-connectivity silicon carbide nanowires prepared by the vapor synthesis method and water is 0.010 g: (50-60) mL.
6. The preparation method of the electrocatalyst formed by molybdenum disulfide coated silicon carbide nanowires according to claim 4, wherein the mass ratio of the added molybdenum source to the high-connectivity silicon carbide nanowires is (60-150): 1.
7. the method for preparing the electrocatalyst composed of molybdenum disulfide-coated silicon carbide nanowires according to claim 4, wherein the stirring time in step 1) and step 2) is 10-30 min.
8. The method for preparing the electrocatalyst composed of molybdenum disulfide-coated silicon carbide nanowires according to claim 4, wherein in the step 2), the molybdenum source is one or two of ammonium molybdate and sodium molybdate; the sulfur source is one or two of thioacetamide and thiourea.
9. The method as claimed in claim 4, wherein the hydrothermal reaction temperature in step 3) is 180-230 ℃ and the hydrothermal reaction time is 12-36 h.
10. The method for preparing the electrocatalyst composed of molybdenum disulfide-coated silicon carbide nanowires according to claim 4, wherein the temperature of the drying treatment in step 4) is 60 to 90 ℃.
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