CN111468144A - MoS2/MoO2Ru composite material and preparation method and application thereof - Google Patents
MoS2/MoO2Ru composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 54
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 52
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- QXYJCZRRLLQGCR-UHFFFAOYSA-N molybdenum(IV) oxide Inorganic materials O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims abstract description 32
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(IV) oxide Inorganic materials O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical group [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 4
- 229910019891 RuCl3 Inorganic materials 0.000 claims description 3
- 239000002057 nanoflower Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000003746 solid phase reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 description 1
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001991 steam methane reforming Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- 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
- C25B11/093—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 at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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- 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
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Abstract
The invention belongs to the technical field of electro-catalysis hydrogen production, and discloses a MoS2/MoO2a/Ru composite material, a preparation method and application thereof. The preparation method comprises the following steps: mixing the nano MoS2Adding into water, performing ultrasonic dispersion under ice bath condition, and then placing the mixed solution subjected to ultrasonic dispersion into a cell crushing instrument for ultrasonic treatment for at least 30 min; adding water-soluble Ru salt and H with the concentration of 4-6 wt% into the obtained mixed solution in sequence2O2Stirring uniformly, controlling the temperature to be 80-95 ℃ for reaction for 4-6h, centrifuging, washing and drying to obtain MoS2/RuO2A composite material; the prepared MoS2/RuO2The composite material is fully and uniformly ground, and the grinding speed is N2Calcining at 400-800 ℃ for 3-6 h in the atmosphere of gas or inert gas, and naturally cooling to room temperature to obtain MoS2/MoO2A/Ru composite material. The composite material is used as a catalyst for electrocatalytic hydrogen evolution reaction. MoS prepared by the method of the invention2/MoO2the/Ru composite material has uniform appearance and excellent electrocatalytic performance, and meanwhile, in the preparation process, the reaction condition is simple, the operation is easy, the yield is high, and the industrial production is easy.
Description
Technical Field
The invention belongs to the technical field of electro-catalysis hydrogen production, and particularly relates to MoS2/MoO2a/Ru composite material, a preparation method and application thereof.
Background
Hydrogen energy has attracted much attention as a competitive clean energy candidate. In addition to this, more than 6000 million tons of hydrogen are used annually for different industrial uses, involving synthetic ammonia production, hydrocracking and fossil fuel refining. However, more than 95% of the hydrogen comes from coal gasification or steam methane reforming, which results in high energy consumption and large carbon dioxide emissions. Electrochemical water splitting is a more sustainable method to produce hydrogen, and then electrical energy can be stored in the chemical bonds of hydrogen, which provides a better method for low cost electricity using existing renewable energy sources. The heart of the Hydrogen Evolution Reaction (HER) is to find an efficient catalyst-triggered reaction.
Disclosure of Invention
Aiming at overcoming the defects in the prior art, the invention aims to provide a MoS2/MoO2a/Ru composite material, a preparation method and application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a composite material is prepared from MoS2、MoO2And Ru.
The preparation method of the composite material comprises the following steps:
（1）、MoS2/RuO2preparing a composite material:
mixing the nano MoS2Adding into water, performing ultrasonic dispersion under ice bath condition, and then placing the mixed solution subjected to ultrasonic dispersion into a cell crushing instrument for ultrasonic treatment for at least 30 min; adding water-soluble Ru salt and H with the concentration of 4-6 wt% into the obtained mixed solution in sequence2O2Stirring uniformly, controlling the temperature to be 80-95 ℃ for reaction for 4-6h, centrifuging, washing and drying to obtain MoS2/RuO2A composite material; wherein the molar weight of the water-soluble Ru salt is measured by the molar weight of Ru element contained in the water-soluble Ru salt, and the MoS is nano2The molar ratio of the water-soluble Ru salt to the water-soluble Ru salt is more than 1: 3, and the addition amount of water is 30-60 m L/0.2 g of nano MoS2，H2O2The addition amount of (A) is 2-4 m L/0.6 mmol water-soluble Ru salt;
（2）、MoS2/MoO2preparation of the/Ru composite material:
the MoS prepared in the step (1) is added2/RuO2The composite material is fully and uniformly ground, and the grinding speed is N2Calcining at 400-800 ℃ for 3-6 h in the atmosphere of gas or inert gas, and naturally cooling to room temperature to obtain MoS2/MoO2A/Ru composite material.
Preferably, in the step (1), the nano MoS2Is MoS2And (4) nano flowers.
Preferably, in the step (1), the water-soluble Ru salt is RuCl3·3H2O。
Preferably, in the step (1), the drying temperature is 60-80 ℃ and the drying time is 8-12 h.
Preferably, in the step (2), the temperature is raised at a rate of 5 to 10 ℃/min during the calcination.
The composite material is used as a catalyst for electrocatalytic hydrogen evolution reaction.
In the invention, the nano MoS2Can be prepared according to the prior art. The invention utilizes brand new solid phase reaction to prepare MoS2/MoO2Composite materials of/Ru, i.e. MoS2/RuO2After the composite material is calcined, the oxidation-reduction reaction between two solid substances occurs, and the reaction equation is as follows:
MoS2+ 3 RuO2= MoO2+ 2 Ru + 2 SO2↑。
MoS prepared by the method of the invention2/MoO2the/Ru composite material has uniform appearance and excellent electrocatalytic performance, and meanwhile, in the preparation process, the reaction condition is simple, the operation is easy, the yield is high, and the industrial production is easy.
Drawings
FIG. 1: MoS prepared in example 12、MoS2/RuO2Composite material and MoS2/MoO2XRD pattern of the/Ru composite.
FIG. 2: MoS prepared in example 12/MoO2SEM image of/Ru composite.
FIG. 3: MoS corresponding to FIG. 22/MoO2EDS diagram of the/Ru composite.
FIG. 4: MoS prepared in example 12/RuO2Temperature-variable XRD patterns of the composite materials.
FIG. 5: MoS prepared in example 12/MoO2Schematic diagram of electrocatalytic hydrogen generation performance of the/Ru composite material under different PH conditions.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1
MoS2/MoO2The preparation method of the/Ru composite material comprises the following steps:
(1) nano MoS2The preparation of (1):
preparing 3D flower-shaped nano molybdenum disulfide by using ammonium molybdate tetrahydrate and thiourea as raw materials: 0.2 g PVP (K-30) was dissolved in 100 ml deionized water,1.22 g (NH)4)6Mo7O24·4H2O and 1.78 g NH2CSNH2Adding into the above solution, and stirring for 30 min to obtain clear solution; transferring the solution into a 200 ml high-pressure reaction kettle, reacting at 200 ℃ for 24 h, cooling, separating out precipitate by a centrifuge, alternately washing with ethanol and deionized water for three times, and drying the product in a vacuum drying oven at 60 ℃ for 12 h to obtain 3D flower-shaped nano molybdenum disulfide;
（2）、MoS2/RuO2preparing a composite material:
0.2 g of MoS prepared in step (1) was taken2Dispersing in 40 ml deionized water, performing ultrasonic treatment for 3 h under ice bath condition, then placing the ultrasonic dispersed mixed solution in a cell pulverizer, performing ultrasonic treatment for 30 min, and taking 0.1308 g RuCl3·3H2Adding O into the mixed solution; 3 ml of 30 wt% H was taken2O2Adding deionized water to dilute to 20 ml, and adding 20 ml of H2O2Slowly dropping the diluent into the mixed solution in which ruthenium trichloride is fully dissolved, fully and uniformly stirring, transferring the solution into a 100 ml high-pressure reaction kettle, reacting for 5 h at 95 ℃, centrifuging, alternately washing with ethanol and deionized water for three times, putting into a vacuum drying oven, and drying for 12 h at 60 ℃ to obtain MoS2/RuO2A composite material;
（3）、MoS2/MoO2preparation of the/Ru composite material:
mixing the MoS prepared in the step (2)2/RuO2Fully grinding the composite material uniformly and flatly paving the composite material in a high-temperature-resistant quartz boat, then placing the quartz boat in a tubular electric furnace, introducing nitrogen for 30 min to exhaust air in a quartz tube of the tubular electric furnace, heating to 500 ℃ at the speed of 10 ℃/min, calcining for 6h in the nitrogen atmosphere, and taking out a black powder sample after the tubular electric furnace is naturally cooled to room temperature, wherein the black powder sample is MoS2/MoO2A/Ru composite material.
FIG. 1 shows the MoS prepared2、MoS2/RuO2Composite material and MoS2/MoO2XRD pattern of the/Ru composite. As can be seen from fig. 1: starting material is MoS2And MoS2/RuO2Composite materialXRD pattern of (1), due to RuO2Covering at MoS2(JCPDS: 00-075-1539) surface, the signal obtained by XRD test detection only shows RuO2(JCPDS: 00-040-1290); in MoS2/MoO2The XRD pattern of the/Ru composite material can be clearly found to correspond to MoO2Three peaks of (JCPDS: 00-32-0671): 26.0 ° (011), 37.0 ° (211) and 53.5 ° (312), and Ru (JCPDS: 00-001-. The solid phase reaction is interface solid phase reaction, which is difficult to completely carry out, MoS in XRD2The signal of (a) was not clear and was further analyzed by SEM and EDS.
FIGS. 2 and 3 are MoS, respectively2/MoO2SEM and EDS of/Ru composites by comparison with MoS2/MoO2Elemental analysis of the/Ru composite showed: except Mo, O and Ru, S element remains, which proves that the composite material still contains MoS2。
Combining the information of fig. 1-3, it is confirmed that: the MoS is prepared by the invention2/MoO2A/Ru composite material.
Comparative example
The difference from example 1 is that: in the step (3), MoS is added2/RuO2The calcination temperatures of the composite materials were adjusted to 100 ℃, 200 ℃, 300 ℃, 400 ℃, 600 ℃, 700 ℃ and 800 ℃ respectively, and the other steps were performed in the same manner as in example 1.
FIG. 4 is a MoS2/RuO2Temperature-changing XRD pattern, namely MoS, of composite material2/RuO2XRD patterns of the products obtained after the composite materials are calcined at different calcining temperatures can be seen from the patterns: at 400 ℃ MoS2/RuO2The peak shape of the composite material XRD changes, solid phase reaction begins to occur, the reaction is more thorough along with the increase of the temperature, and the peak intensity of Ru increases.
And (3) testing the electrocatalytic performance:
preparation of a working electrode:
3 mg of MoS prepared in example 1 were weighed2/MoO2Taking the/Ru composite material as a catalyst, transferring 500 mu L absolute ethyl alcohol into a 1 m L centrifuge tube, and adding 50 percentMu L Nafion solution (5 wt%), ultrasonically dispersing the mixture to uniform ink dispersion state, and then removing 15 mu L (load-0.418 mg-cm)–2) The suspension is dropped on a Glassy Carbon Electrode (GCE) with the diameter of 5 mm to be naturally dried to be used as a working electrode for standby.
The experimental process comprises the following steps: at room temperature using an electrochemical workstation (CHI-760E) under a standard three-electrode system (saturated calomel electrode as reference electrode, graphite rod as auxiliary electrode). Respectively at 1M KOH, 0.5M H2SO41M PBS electrolyte, converting the measured overpotential relative to the saturated calomel electrode into the relative reversible hydrogen electrode potential (E RHE=E SCE+0.241+0.0591 pH). The linear polarization curves were tested at a sweep rate of 2 mV/s, and none of the resulting polarization curves were IR corrected.
FIG. 5 shows MoS2/MoO2Schematic diagram of electrocatalytic hydrogen generation performance of the/Ru composite material under different PH conditions. As can be seen from fig. 5: MoS2/MoO2When the/Ru composite material is used as an electrocatalytic hydrogen production (HER) catalyst, hydrogen production under the condition of full PH can be realized. The overpotentials under the acid and alkali conditions were 49 mV, 12 mV, and 51 mV, respectively. Among them, the hydrogen production performance under alkaline condition is particularly outstanding, which shows that the MoS2/MoO2the/Ru composite material as a catalyst has excellent electro-catalysis hydrogen production performance.
Claims (7)
1. A composite material characterized by: from MoS2、MoO2And Ru.
2. A method of preparing the composite material of claim 1, comprising the steps of:
（1）、MoS2/RuO2preparing a composite material:
mixing the nano MoS2Adding into water, performing ultrasonic dispersion under ice bath condition, and then placing the mixed solution subjected to ultrasonic dispersion into a cell crushing instrument for ultrasonic treatment for at least 30 min; adding water-soluble Ru salt and H with the concentration of 4-6 wt% into the obtained mixed solution in sequence2O2Stirring uniformly, controlling the temperature to be 80-95 ℃ for reaction for 4-6h, centrifuging, washing and drying to obtain MoS2/RuO2A composite material; wherein the molar weight of the water-soluble Ru salt is measured by the molar weight of Ru element contained in the water-soluble Ru salt, and the MoS is nano2The molar ratio of the water-soluble Ru salt to the water-soluble Ru salt is more than 1: 3, and the addition amount of water is 30-60 m L/0.2 g of nano MoS2，H2O2The addition amount of (A) is 2-4 m L/0.6 mmol water-soluble Ru salt;
（2）、MoS2/MoO2preparation of the/Ru composite material:
the MoS prepared in the step (1) is added2/ RuO2The composite material is fully and uniformly ground, and the grinding speed is N2Calcining at 400-800 ℃ for 3-6 h in the atmosphere of gas or inert gas, and naturally cooling to room temperature to obtain MoS2/MoO2A/Ru composite material.
3. A method of preparing the composite material of claim 2, wherein: in the step (1), the nano MoS2Is MoS2And (4) nano flowers.
4. A method of preparing the composite material of claim 2, wherein: in the step (1), the water-soluble Ru salt is RuCl3·3H2O。
5. A method of preparing the composite material of claim 2, wherein: in the step (1), the drying temperature is 60-80 ℃, and the drying time is 8-12 h.
6. A method of preparing the composite material of claim 2, wherein: in the step (2), during calcination, the temperature is increased at the rate of 5-10 ℃/min.
7. Use of a composite material according to claim 1, wherein: as a catalyst for electrocatalytic hydrogen evolution reaction.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112371119A (en) * | 2020-11-13 | 2021-02-19 | 中南大学深圳研究院 | Preparation method and application of multi-metal paired alkaline catalyst |
| CN113584504A (en) * | 2021-08-06 | 2021-11-02 | 郑州大学 | Ru/RuO2/MoO2Composite material and preparation method and application thereof |
| WO2022183578A1 (en) * | 2021-03-05 | 2022-09-09 | 广东工业大学 | Molybdenum carbide-molybdenum oxide catalyst, preparation method therefor and use thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150167181A1 (en) * | 2013-12-16 | 2015-06-18 | Timothy D. Vaden | Synthesis of Molybdenum Catalyst Formulations for Hydrogen Generation |
| CN108682873A (en) * | 2018-05-28 | 2018-10-19 | 南京晓庄学院 | A kind of Ru-MoO3-x/ rGO composite material and preparation methods and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112371119A (en) * | 2020-11-13 | 2021-02-19 | 中南大学深圳研究院 | Preparation method and application of multi-metal paired alkaline catalyst |
| CN112371119B (en) * | 2020-11-13 | 2023-07-07 | 中南大学深圳研究院 | Preparation method and application of multi-metal pairing alkaline catalyst |
| WO2022183578A1 (en) * | 2021-03-05 | 2022-09-09 | 广东工业大学 | Molybdenum carbide-molybdenum oxide catalyst, preparation method therefor and use thereof |
| CN113584504A (en) * | 2021-08-06 | 2021-11-02 | 郑州大学 | Ru/RuO2/MoO2Composite material and preparation method and application thereof |
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