CN111468144B - MoS 2 /MoO 2 Ru composite material and preparation method and application thereof - Google Patents
MoS 2 /MoO 2 Ru composite material and preparation method and application thereof Download PDFInfo
- Publication number
- CN111468144B CN111468144B CN202010425463.8A CN202010425463A CN111468144B CN 111468144 B CN111468144 B CN 111468144B CN 202010425463 A CN202010425463 A CN 202010425463A CN 111468144 B CN111468144 B CN 111468144B
- Authority
- CN
- China
- Prior art keywords
- mos
- composite material
- moo
- water
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 title description 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 150000003839 salts Chemical class 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000003756 stirring 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
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 18
- 239000001257 hydrogen Substances 0.000 abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000203 mixture Substances 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 7
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 238000010586 diagram Methods 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
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- 230000010287 polarization Effects 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
- 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
- 238000007865 diluting 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
- 239000007788 liquid Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000002057 nanoflower Substances 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
- 239000000843 powder Substances 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
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 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
Images
Classifications
-
- 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
-
- 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
-
- 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
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of electro-catalysis hydrogen production, and discloses a MoS 2 /MoO 2 a/Ru composite material, a preparation method and application thereof. The preparation method comprises the following steps: mixing the nano MoS 2 Adding the mixture into water, performing ultrasonic dispersion uniformly under an ice bath condition, and then placing the ultrasonically dispersed mixed solution 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 sequence 2 O 2 Uniformly stirring, controlling the temperature to be 80-95 ℃ for reaction of 4-6h, centrifuging, washing and drying to obtain MoS 2 /RuO 2 A composite material; the prepared MoS 2 /RuO 2 The composite material is fully and uniformly ground, and the grinding speed is N 2 Calcining 3-6 h at 400-800 ℃ in a gas or inert atmosphere, and naturally cooling to room temperature to obtain MoS 2 /MoO 2 A Ru composite material. The composite material is used as a catalyst for electrocatalytic hydrogen evolution reaction. MoS prepared by the method of the invention 2 /MoO 2 the/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 MoS 2 /MoO 2 a/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 MoS 2 /MoO 2 a/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 MoS 2 、MoO 2 And Ru.
The preparation method of the composite material comprises the following steps:
（1）、MoS 2 /RuO 2 preparing a composite material:
mixing the nano MoS 2 Adding 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 sequence 2 O 2 Stirring uniformly, controlling the temperature to be 80-95 ℃ for reaction of 4-6h, centrifuging, washing and dryingDrying to obtain MoS 2 /RuO 2 A 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 nano 2 The molar ratio of the water-soluble Ru salt to the water-soluble Ru salt is more than 1: 3, and the addition amount of the water is 30-60 mL/0.2 g nano MoS 2 ，H 2 O 2 The addition amount of (A) is 2-4 mL/0.6 mmol of water-soluble Ru salt;
（2）、MoS 2 /MoO 2 preparation of the/Ru composite material:
the MoS prepared in the step (1) is added 2 /RuO 2 The composite material is fully and uniformly ground, and the grinding speed is N 2 Calcining 3-6 h at 400-800 ℃ in a gas or inert atmosphere, and naturally cooling to room temperature to obtain MoS 2 /MoO 2 A/Ru composite material.
Preferably, in the step (1), the nano MoS 2 Is MoS 2 And (4) nano flowers.
Preferably, in the step (1), the water-soluble Ru salt is RuCl 3 ·3H 2 O。
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 calcination.
The composite material is used as a catalyst for electrocatalytic hydrogen evolution reaction.
In the invention, the nano MoS 2 Can be prepared according to the prior art. The invention utilizes brand new solid phase reaction to prepare MoS 2 /MoO 2 Composite materials of/Ru, i.e. MoS 2 /RuO 2 After the composite material is calcined, the oxidation-reduction reaction between two solid substances occurs, and the reaction equation is as follows:
MoS 2 + 3 RuO 2 = MoO 2 + 2 Ru + 2 SO 2 ↑。
MoS prepared by the method of the invention 2 /MoO 2 the/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 1 2 、MoS 2 /RuO 2 Composite material and MoS 2 /MoO 2 XRD pattern of the/Ru composite.
FIG. 2: moS prepared in example 1 2 /MoO 2 SEM image of/Ru composite.
FIG. 3: moS corresponding to FIG. 2 2 /MoO 2 EDS diagram of the/Ru composite.
FIG. 4: moS prepared in example 1 2 /RuO 2 Temperature-variable XRD patterns of the composite materials.
FIG. 5: moS prepared in example 1 2 /MoO 2 Schematic diagram of electrocatalytic hydrogen generation performance of the/Ru composite material under different PH conditions.
Detailed Description
The present invention is further illustrated by the following 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
MoS 2 /MoO 2 The preparation method of the/Ru composite material comprises the following steps:
(1) Nano MoS 2 The 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 ) 6 Mo 7 O 24 ·4H 2 O and 1.78 g NH 2 CSNH 2 Adding 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 a precipitate by a centrifuge, alternately washing with ethanol and deionized water for three times, and putting the product into a vacuum drying oven for drying at 60 ℃ for 12 h to obtain 3D flower-shaped nano molybdenum disulfide;
（2）、MoS 2 /RuO 2 preparing a composite material:
taking 0.2 g MoS prepared in step (1) 2 Dispersing into 40 ml deionized water, ultrasonic treating 3 h under ice bath condition, and mixing the ultrasonic dispersionThe solution is placed in a cell crusher for 30 min by ultrasonic treatment, and 0.1308 g RuCl is taken 3 ·3H 2 Adding O into the mixed solution; 3 ml of 30 wt% H was taken 2 O 2 Diluting to 20 ml with deionized water, and adding 20 ml H 2 O 2 Slowly 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 at 95 ℃ for 5 h, centrifuging, alternately washing with ethanol and deionized water for three times, putting into a vacuum drying oven, and drying at 60 ℃ for 12 h to obtain MoS 2 /RuO 2 A composite material;
（3）、MoS 2 /MoO 2 preparation of the/Ru composite:
mixing the MoS prepared in the step (2) 2 /RuO 2 The composite material is fully ground and evenly paved in a high-temperature resistant quartz boat, then the quartz boat is placed in a tubular electric furnace, nitrogen is introduced for 30 min to exhaust air in the quartz tube of the tubular electric furnace, the temperature is raised to 500 ℃ at the speed of 10 ℃/min, and the quartz boat is calcined in the nitrogen atmosphere for 6h, after the temperature of the tubular electric furnace is naturally reduced to the room temperature, a black powder sample is taken out, namely MoS 2 /MoO 2 A/Ru composite material.
FIG. 1 shows the MoS prepared 2 、MoS 2 /RuO 2 Composite material and MoS 2 /MoO 2 XRD pattern of the/Ru composite. As can be seen from fig. 1: the starting material is MoS 2 And MoS 2 /RuO 2 XRD pattern of composite material due to RuO 2 Covering at MoS 2 (JCPDS: 00-075-1539) and XRD test shows that the obtained signal only shows RuO 2 (JCPDS: 00-040-1290); in MoS 2 /MoO 2 The XRD pattern of the/Ru composite material can be clearly found to correspond to MoO 2 Three peaks of (JCPDS: 00-32-0671): peaks at 26.0 ° (011), 37.0 ° (211), and 53.5 ° (312), and Ru (JCPDS: 00-001-1253) 43.9 ° (101). The solid phase reaction is interface solid phase reaction, which is difficult to completely carry out, moS in XRD 2 The signal of (a) was not clear and was further analyzed by SEM and EDS.
FIGS. 2 and 3 are MoS, respectively 2 /MoO 2 SEM picture and EDS picture of/Ru composite materialBy pairing MoS 2 /MoO 2 Elemental analysis of the/Ru composite showed: except Mo, O and Ru, S element remains, which proves that the composite material still contains MoS 2 。
By combining the information of fig. 1-3, it is confirmed that: the MoS is prepared by the invention 2 /MoO 2 A Ru composite material.
Comparative example
The difference from example 1 is that: in the step (3), moS is added 2 /RuO 2 The 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 MoS 2 /RuO 2 Temperature-changing XRD pattern, namely MoS, of composite material 2 /RuO 2 XRD patterns of the products obtained after the composite materials are calcined at different calcining temperatures can be seen from the patterns: at 400 ℃ MoS 2 /RuO 2 The 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 MoS prepared in example 1 was weighed 2 /MoO 2 the/Ru composite material is used as a catalyst, 500 muL of absolute ethyl alcohol is transferred to a 1 mL centrifuge tube, 50 muL of Nafion solution (5 wt%) is added, and the mixture is subjected to ultrasonic dispersion treatment to be in a uniform ink dispersion state; then, 15 μ L (load amount-0.418 mg-cm) is moved –2 ) The suspension liquid is dripped onto 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 and graphite rod as auxiliary electrode). Respectively at 1M KOH and 0.5M H 2 SO 4 1M PBS electrolyte, converting the overpotential measured 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 MoS 2 /MoO 2 Schematic diagram of electrocatalytic hydrogen generation performance of the/Ru composite material under different PH conditions. As can be seen from fig. 5: moS 2 /MoO 2 When 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 acid-base conditions were 49 mV, 12 mV, 51 mV, respectively. Among them, the hydrogen production performance under alkaline condition is particularly outstanding, which shows that the MoS 2 /MoO 2 the/Ru composite material as a catalyst has excellent electro-catalysis hydrogen production performance.
Claims (4)
1. MoS 2 /MoO 2 The preparation method of the/Ru composite material is characterized by comprising the following steps:
（1）、MoS 2 /RuO 2 preparing a composite material:
mixing 3D flower-shaped nano MoS 2 Adding 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 sequence 2 O 2 Stirring, transferring the solution into a high-pressure reaction kettle, controlling the temperature at 80-95 ℃ for reaction for 4-6h, centrifuging, washing and drying to obtain MoS 2 /RuO 2 A 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 3D flower-shaped nano MoS 2 The mol ratio of the water-soluble Ru salt is more than 1: 3, and the addition amount of water is 30-60 mL/0.2 g of 3D flower-shaped nano MoS 2 ，H 2 O 2 The adding amount of the (A) is 2-4 mL/0.6 mmol of water-soluble Ru salt;
（2）、MoS 2 /MoO 2 preparation of the/Ru composite material:
the MoS prepared in the step (1) is added 2 / RuO 2 The composite material is fully and uniformly ground at N 2 Calcining 3-6 h at 400-800 ℃ in a gas or inert atmosphere, and naturally cooling to room temperature to obtain MoS 2 /MoO 2 Ru composite materialAnd (5) feeding.
2. The MoS of claim 1 2 /MoO 2 The preparation method of the/Ru composite material is characterized by comprising the following steps: in the step (1), the water-soluble Ru salt is RuCl 3 ·3H 2 O。
3. The MoS of claim 1 2 /MoO 2 The preparation method of the/Ru composite material is characterized by comprising the following steps: in the step (1), the drying temperature is 60-80 ℃, and the drying time is 8-12 h.
4. The MoS of claim 1 2 /MoO 2 The preparation method of the/Ru composite material is characterized by comprising the following steps: in the step (2), during calcination, the temperature is increased at the rate of 5-10 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010425463.8A CN111468144B (en) | 2020-05-19 | 2020-05-19 | MoS 2 /MoO 2 Ru composite material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010425463.8A CN111468144B (en) | 2020-05-19 | 2020-05-19 | MoS 2 /MoO 2 Ru composite material and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111468144A CN111468144A (en) | 2020-07-31 |
| CN111468144B true CN111468144B (en) | 2022-10-25 |
Family
ID=71762796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010425463.8A Active CN111468144B (en) | 2020-05-19 | 2020-05-19 | MoS 2 /MoO 2 Ru composite material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111468144B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113145146B (en) * | 2021-03-05 | 2023-03-07 | 广东工业大学 | Molybdenum carbide-molybdenum oxide catalyst and preparation method and application thereof |
| CN113584504A (en) * | 2021-08-06 | 2021-11-02 | 郑州大学 | Ru/RuO2/MoO2Composite material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109950509A (en) * | 2019-04-09 | 2019-06-28 | 武汉轻工大学 | A kind of MoO2/MoS2Combination electrode material and preparation method thereof |
Family Cites Families (1)
| 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 |
-
2020
- 2020-05-19 CN CN202010425463.8A patent/CN111468144B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109950509A (en) * | 2019-04-09 | 2019-06-28 | 武汉轻工大学 | A kind of MoO2/MoS2Combination electrode material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Improve charge injection of the edge aligned MoS2 /MoO2 hybrid nanosheets for highly robust and efficient electrocatalysis of H2 production;Shuaishuai Li 等;《Nanoscale》;20200124;第1-12页 * |
| Single-Atom Ru Doping Induced Phase Transition of MoS2 and S Vacancy for Hydrogen Evolution Reaction;Junmeng Zhang 等;《Small Methods》;20191231;第1-9页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111468144A (en) | 2020-07-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111468144B (en) | MoS 2 /MoO 2 Ru composite material and preparation method and application thereof | |
| CN107670679B (en) | MoS2Preparation method and application of/rGO-CN composite material | |
| CN110227531B (en) | Preparation method of molybdenum-doped cobalt-iron oxide nanosheet bifunctional electrocatalyst | |
| CN109518219B (en) | Preparation method and application of graphene-based nickel-cobalt bimetallic oxygen evolution catalyst | |
| CN112108149A (en) | Preparation method of electrocatalytic material, corresponding material and use method | |
| CN106824198B (en) | Cobalt-based produces VPO catalysts and preparation method thereof and a kind of alkaline hydrogen manufacturing electrolytic cell | |
| CN110339845B (en) | Preparation method and hydrogen evolution application of molybdenum disulfide flower-like nanospheres | |
| CN113019398B (en) | High-activity self-supporting OER electrocatalyst material and preparation method and application thereof | |
| CN113060770B (en) | Preparation method of heterojunction CoO/CoS porous nanorod, obtained material and application | |
| CN110624573A (en) | Nickel-doped cobalt selenide electro-catalysis hydrogen evolution catalyst and preparation method thereof | |
| CN109585861B (en) | Preparation method of dual-functional cobalt monoxide and nitrogen-doped carbon in-situ composite electrode | |
| CN114045525A (en) | Nickel-based self-supporting water electrolysis catalyst and preparation method thereof | |
| CN108097269A (en) | A kind of ultra-thin porous Ce-Ni-O-S nanometer sheets and its preparation method and application | |
| CN108435211A (en) | A kind of preparation method of the Ni-Fe-Ce ternary sulfide oxygen-separating catalysts of Ce doping | |
| CN113445073A (en) | Preparation and electrocatalysis application of carbon cloth-loaded polyacid-derived cobalt molybdenum sulfide | |
| CN113443610B (en) | Ruthenium selenide nanosphere electrocatalyst and preparation method and application thereof | |
| Wu et al. | NiCo nitride/carbon nanoflakes as low-cost bifunctional electrocatalysts for carbohydrate-assisted electrolytic H2 generation | |
| CN113652708A (en) | Pt/Ni alloy3N@Mo2Preparation method of C hydrogen hydroxide evolution electrocatalyst | |
| CN110787820B (en) | Heteroatom nitrogen surface modification MoS2Preparation and application of nano material | |
| CN115029709B (en) | Cobalt-nickel metal sulfide bifunctional electrocatalyst and preparation method and application thereof | |
| CN116855963A (en) | Ru/Co/g-C 3 N 4 Composite material, preparation method and application thereof | |
| CN113584504A (en) | Ru/RuO2/MoO2Composite material and preparation method and application thereof | |
| CN110721700A (en) | Copper-cobalt-sulfur nanosheet array/molybdenum foil composite material, and preparation method and application thereof | |
| CN109999863A (en) | A kind of preparation method of nano nickel phosphide carbon composite catalytic agent | |
| CN113755880B (en) | Application of ruthenate material in electrocatalytic hydrogen evolution reaction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |