CN114318392A - MoS2-NiS2NF hydrogen evolution material and preparation method and application thereof - Google Patents
MoS2-NiS2NF hydrogen evolution material and preparation method and application thereof Download PDFInfo
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- CN114318392A CN114318392A CN202111442986.4A CN202111442986A CN114318392A CN 114318392 A CN114318392 A CN 114318392A CN 202111442986 A CN202111442986 A CN 202111442986A CN 114318392 A CN114318392 A CN 114318392A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000001257 hydrogen Substances 0.000 title claims abstract description 84
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 84
- 239000000463 material Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910021508 nickel(II) hydroxide Inorganic materials 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 17
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 17
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 238000001354 calcination Methods 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 8
- 238000011144 upstream manufacturing Methods 0.000 claims description 8
- 239000012670 alkaline solution Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000001035 drying Methods 0.000 description 12
- 239000006260 foam Substances 0.000 description 12
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 5
- 229910021607 Silver chloride Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 4
- 239000010411 electrocatalyst Substances 0.000 description 4
- 230000001588 bifunctional effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000002815 nickel Chemical group 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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 relates to the technical field of hydrogen energy, in particular to a MoS2‑NiS2/NF hydrogen evolution material, and a preparation method and application thereof. Firstly, dissolving sodium molybdate dihydrate, nickel nitrate hexahydrate and urotropine in deionized water to obtain a first mixed solution; then transferring the first mixed solution to a reaction kettle, taking foamed nickel as a carrier, and obtaining MoO through hydrothermal reaction2‑Ni(OH)2/NF; finally, MoO is added2‑Ni(OH)2/NF and sulfur powder are calcined under the anaerobic condition to obtain MoS2‑NiS2/NF hydrogen evolution material. MoS of the invention2‑NiS2the/N hydrogen evolution material is used for electrocatalytic hydrogen evolution reaction. Compared with the prior art, the MoS prepared by the invention2‑NiS2Raw material cost of/NF hydrogen evolution materialLow cost, simple preparation method, good hydrogen evolution effect in alkaline solution and hopeful industrial development.
Description
Technical Field
The invention relates to the technical field of hydrogen energy, in particular to a MoS2-NiS2/NF hydrogen evolution material, and a preparation method and application thereof.
Background
With the increasing exhaustion of fossil fuels, various new energy sources are continuously developed and utilized. The hydrogen energy is used as a renewable secondary energy source, has wide source, high heat value, cleanness and good combustion stability, and is a new generation of energy carrier widely adopted after non-renewable energy sources such as fossil fuel and the like. Chemical water splitting is strongly dependent on mass transport and active centers, however, difficulty in promoting mass transport and exposing enough active centers are the major bottlenecks of the two half-reactions of total water splitting, namely: hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER). The alkaline electrolysis of water for hydrogen production is the most potential technical means leading to hydrogen economy, but the reaction energy consumption is larger due to the existence of hydrogen evolution and oxygen evolution overpotential in the electrolysis process. In order to reduce energy consumption, it is of great significance to develop a cathode electrode material with low cost and high catalytic activity. The CN 113249753A Jiangquan invented molybdenum sulfide @ cobalt-MOF/NF hydrogen evolution material, the in-situ synthesis method and the application thereof are used for hydrogen evolution in alkaline solution, and no method is available for simultaneously carrying out oxygen evolution reaction. The high-efficiency electrolytic water contains hydrogen evolution and oxygen evolution reactions, and particularly, compared with a single-metal sulfide, a double-metal sulfide hybrid shows superior catalytic performance. When two or more metal species are combined, more active sites may be exposed, thereby improving the kinetics of the electrochemical reaction.
At present, noble metal based electrocatalysts (Pt, RuO)2And IrO2) Are considered highly efficient, ideal HER and OER catalysts that can reduce overpotentials and achieve relatively high energy conversion efficiencies. However, the drawbacks and high cost of these noble metal-based materials have hindered their large-scale use. To reverse this unfavorable situation, a large-scale research is ongoing to find advanced, economical, earth-rich bifunctional electrocatalysts for bulk water splitting, which is still a huge challenge to date.
Disclosure of Invention
In order to solve the above problems, it is an object of the present invention to provide a MoS2-NiS2/NF hydrogen evolution material, and a preparation method and application thereof.
The invention aims to overcome the problems of catalytic hydrolysis in the prior art and provides MoS2-NiS2A NF hydrogen evolution material, a preparation method thereof and application in electrocatalytic hydrogen evolution. MoS of the invention2-NiS2The NF hydrogen evolution material is used as a hydrogen evolution catalyst, has lower synthesis cost than most catalysts, and has sufficient earth reserve of main elements.
In the molybdenum metal, the 3d orbit is in a half-filled state and has strong adsorption effect on hydrogen atoms; in metallic nickel, the valence layer d orbital is not filled, and the nickel atom is easily complexed due to the existence of the empty d orbital, and nickel is combined with the hydroxyl group to form nickel hydroxide, thereby promoting the oxygen evolution. MoS2-NiS2After the nickel foam is combined with the nickel foam, the hydrogen evolution performance of the nickel foam is greatly enhanced, the electrochemical performance is improved, and the synthesis method is simple.
The purpose of the invention can be realized by the following technical scheme:
an object of the present invention is to provide a MoS2-NiS2The preparation method of the/NF hydrogen evolution material comprises the following steps:
(1) dissolving sodium molybdate dihydrate, nickel nitrate hexahydrate and urotropine in deionized water to obtain a first mixed solution;
(2) transferring the first mixed solution obtained in the step (1) to a reaction kettle, and carrying out hydrothermal reaction by using foamed nickel as a carrier to obtain MoO2-Ni (OH)2/NF；
(3) MoO obtained in the step (2)2-Ni(OH)2/NF and sulfur powder are calcined under the anaerobic condition to obtain MoS2-NiS2/NF hydrogen evolution material.
In one embodiment of the present invention, in the step (1), the ratio of the amounts of sodium molybdate dihydrate, nickel nitrate hexahydrate, urotropin and deionized water is 1 mmol: 1 mmol: 1 mmol: (40-50) mL.
In one embodiment of the present invention, in the step (2), the reaction temperature is 130-180 ℃ and the reaction time is 5-8h during the hydrothermal reaction.
In one embodiment of the present invention, in step (3), MoO2-Ni(OH)2The mass ratio of the/NF to the sulfur powder is 1: (1-10).
In one embodiment of the present invention, in step (3), the calcination process is carried out in a resistance furnace with sulfur powder upstream and MoO2-Ni(OH)2the/NF is downstream.
In one embodiment of the invention, the calcination process is carried out in a nitrogen environment.
In one embodiment of the invention, the calcination temperature is 300-500 ℃ and the calcination time is 1-3 h.
It is a second object of the present invention to provide a MoS prepared by the above method2-NiS2/NF hydrogen evolution material.
It is a third object of the present invention to provide the above MoS2-NiS2Application of/NF hydrogen evolution material and MoS2-NiS2the/NF hydrogen evolution material is used for electrocatalytic hydrogen evolution reaction.
In one embodiment of the invention, the MoS is operated2-NiS2The NF hydrogen evolution material is directly used as a working electrode during reaction,and fixed with an electrode clamp.
In one embodiment of the present invention, the MoS2-NiS2the/NF hydrogen evolution material is washed clean by ethanol and deionized water and then is placed in a vacuum oven for drying for later use.
The purpose of the hydrothermal reaction in the invention is: the reaction is promoted to be carried out in a high-temperature and high-pressure environment, and the obtained MoO2-Ni(OH)2the/NF is uniform, has no agglomeration and good crystal form, and can be better loaded on the foam nickel.
The purpose of the calcination in the present invention is: under the protection of nitrogen and high temperature, the calcination can effectively carry out vulcanization to form MoS on the foamed nickel2-NiS2Obtaining MoS2-NiS2/NF hydrogen evolution material.
The invention prepares MoS in strong alkaline solution2-NiS2the/NF bimetallic sulfide nano-particles are used as bifunctional electrocatalysts for integral water decomposition. Thanks to the synergistic effect of bimetallic sulfide and NF and unique 3D hollow structure, MoS2-NiS2the/NF not only provides a rich active site, but also provides a variety of ways to transport mass and electrons quickly and efficiently.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the invention, the foam nickel is a sound-absorbing porous metal with a three-dimensional full-through mesh structure and excellent performance, the porosity of the foam nickel is about 95 percent, water or gas can pass through the foam nickel smoothly without resistance, the nickel frameworks are hollow and are mutually connected in a metallurgical state, and the foam nickel has the advantages of good stability, high porosity, thermal shock resistance, small bulk density, large specific surface area and the like; the 3d orbit of the molybdenum is in a half-filled state, and has strong adsorption effect on hydrogen atoms; the metal nickel has unfilled valence layer d orbitals, and nickel atoms easily form complexes due to the existence of empty d orbitals, so that the hydrogen evolution performance of the foamed nickel is greatly improved after the nickel is combined with the foamed nickel. Therefore, the metal which is not filled with the orbit is introduced to be combined with the foamed nickel, so that the desorption of hydrogen atoms adsorbed on the surface of the electrode is facilitated, and the hydrogen evolution performance of the metal nickel electrode is improved;
(2) MoS prepared by the invention2-NiS2the/NF hydrogen evolution material is of a composite structure, and can increase the active specific surface area and increase the contact area between the material and a solution. MoS2-NiS2The nanoparticles interact strongly with the porous NF, giving them excellent performance towards HER.
(3) MoS prepared by the invention2-NiS2MoS in NF hydrogen evolution material2-NiS2The heterogeneous lattice interface in (1) promotes H2Dissociation of the O molecule.
(4) MoS prepared by the invention2-NiS2The NF hydrogen evolution material has low raw material cost and simple preparation method, and the material has good stability due to the introduction of non-noble metal elements.
(5) MoS prepared by the invention2-NiS2The NF hydrogen evolution material electrolyzes water in an alkaline medium, and has good hydrogen evolution effect and lower cost.
Detailed Description
The invention provides a MoS2-NiS2The preparation method of the/NF hydrogen evolution material comprises the following steps:
(1) dissolving sodium molybdate dihydrate, nickel nitrate hexahydrate and urotropine in deionized water to obtain a first mixed solution;
(2) transferring the first mixed solution obtained in the step (1) to a reaction kettle, taking foamed nickel as a carrier, and obtaining MoO through hydrothermal reaction2-Ni(OH)2/NF；
(3) MoO obtained in the step (2)2-Ni(OH)2/NF and sulfur powder are calcined under the anaerobic condition to obtain MoS2-NiS2/NF hydrogen evolution material.
In one embodiment of the present invention, in the step (1), the ratio of the amounts of sodium molybdate dihydrate, nickel nitrate hexahydrate, urotropin and deionized water is 1 mmol: 1 mmol: 1 mmol: (40-50) mL.
In one embodiment of the present invention, in the step (2), the reaction temperature is 130-180 ℃ and the reaction time is 5-8h during the hydrothermal reaction.
In one embodiment of the present invention, in step (3),MoO2-Ni(OH)2the mass ratio of the/NF to the sulfur powder is 1: (1-10).
In one embodiment of the present invention, in step (3), the calcination process is carried out in a resistance furnace with sulfur powder upstream and MoO2-Ni(OH)2the/NF is downstream.
In one embodiment of the invention, the calcination process is carried out in a nitrogen environment.
In one embodiment of the invention, the calcination temperature is 300-500 ℃ and the calcination time is 1-3 h.
The invention provides MoS prepared by the method2-NiS2/NF hydrogen evolution material.
The invention provides the MoS2-NiS2Application of/NF hydrogen evolution material and MoS2-NiS2the/NF hydrogen evolution material is used for electrocatalytic hydrogen evolution reaction.
In one embodiment of the invention, the MoS is operated2-NiS2the/NF hydrogen evolution material is directly used as a working electrode during reaction and is fixed by an electrode clamp.
In one embodiment of the present invention, the MoS2-NiS2the/NF hydrogen evolution material is washed clean by ethanol and deionized water and then is placed in a vacuum oven for drying for later use.
The purpose of the hydrothermal reaction in the invention is: the reaction is promoted to be carried out in a high-temperature and high-pressure environment, and the obtained MoO2-Ni(OH)2the/NF is uniform, has no agglomeration and good crystal form, and can be better loaded on the foam nickel;
the purpose of the calcination in the present invention is: under the protection of nitrogen and high temperature, the calcination can effectively carry out vulcanization to form MoS on the foamed nickel2-NiS2Obtaining MoS2-NiS2/NF hydrogen evolution material.
The invention prepares MoS in strong alkaline solution2-NiS2the/NF bimetallic sulfide nano-particles are used as bifunctional electrocatalysts for integral water decomposition. Thanks to the synergistic effect of bimetallic sulfide and NF and unique 3D hollow structure, MoS2-NiS2the/NF not only provides a rich active site, but also provides a variety of ways to transport mass and electrons quickly and efficiently.
The present invention will be described in detail with reference to specific examples.
The raw materials used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
1.5mmol of sodium molybdate dihydrate
Nickel nitrate hexahydrate 1.5mmol
Urotropin 1.5mmol
Deionized water 60ml
Sulfur powder 10 times MoO2-Ni(OH)2mass/NF
MoS2-NiS2the/NF hydrogen evolution material is prepared by the following steps:
dissolving 1.5mmol of sodium molybdate dihydrate, 1.5mmol of nickel nitrate hexahydrate and 1.5mmol of urotropine in 60mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 5min until the mixture is stirred and dissolved to obtain a first mixed solution. After the first mixed solution had no solid particles, the first mixed solution was transferred to a high-pressure autoclave, and a piece of nickel foam of 8mm × 8mm × 1mm was placed therein and heated at 150 ℃ for 6 hours. Taking out MoO2-Ni(OH)2the/NF is put into a resistance furnace after being treated, nitrogen is introduced to lead the sulfur powder to be at the upstream and the MoO2-Ni(OH)2NF downstream, sulfur powder amount is MoO2-Ni(OH)2Calcining the mixture for 1 hour at the temperature of 350 ℃ by 10 times of the mass of the NF to finally obtain the MoS2-NiS2/NF hydrogen evolution material.
Example 2
The MoS of example 1 was added2-NiS2the/NF hydrogen evolution material is washed clean by ethanol and deionized water, and is dried in a vacuum oven for drying overnight and dried.
(1) Drying the MoS2-NiS2the/NF hydrogen evolution material is clamped by an electrode clamp and directly used as a working electrode for testing.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalysis electrolyte, introducing nitrogen to drive off air, and connecting a working electrode, an Ag/AgCl electrode and a stone grinding rod electrode to an electrochemical workstation.
Example 3
1.5mmol of sodium molybdate dihydrate
Nickel nitrate hexahydrate 1.5mmol
Urotropin 1.5mmol
68ml of deionized water
5 times MoO of sulfur powder2-Ni(OH)2mass/NF
MoS2-NiS2the/NF hydrogen evolution material is prepared by the following steps:
dissolving 1.5mmol of sodium molybdate dihydrate, 1.5mmol of nickel nitrate hexahydrate and 1.5mmol of urotropine in 68mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 5min until the mixture is stirred and dissolved to obtain a first mixed solution. After the first mixed solution had no solid particles, the first mixed solution was transferred to a high-pressure autoclave, and a piece of nickel foam of 8mm × 8mm × 1mm was placed and heated at 130 ℃ for 5 hours. Taking out MoO2-Ni(OH)2the/NF is put into a resistance furnace after being treated, nitrogen is introduced to lead the sulfur powder to be at the upstream and the MoO2-Ni(OH)2NF downstream, sulfur powder amount is MoO2-Ni(OH)25 times of NF mass, calcining for 2 hours at the temperature of 300 ℃ to finally obtain MoS2-NiS2/NF hydrogen evolution material.
Example 4
The MoS of example 3 was added2-NiS2the/NF hydrogen evolution material is washed clean by ethanol and deionized water, and is dried in a vacuum oven for drying overnight and dried.
(1) Drying the MoS2-NiS2the/NF hydrogen evolution material is clamped by an electrode clamp and directly used as a working electrode for testing.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalysis electrolyte, introducing nitrogen to drive off air, and connecting a working electrode, an Ag/AgCl electrode and a stone grinding rod electrode to an electrochemical workstation.
Example 5
1.5mmol of sodium molybdate dihydrate
Nickel nitrate hexahydrate 1.5mmol
Urotropin 1.5mmol
Deionized water 75ml
1 time MoO of sulfur powder2-Ni(OH)2mass/NF
MoS2-NiS2the/NF hydrogen evolution material is prepared by the following steps:
dissolving 1.5mmol of sodium molybdate dihydrate, 1.5mmol of nickel nitrate hexahydrate and 1.5mmol of urotropine in 70mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 5min until the mixture is stirred and dissolved to obtain a first mixed solution. After the first mixed solution is free of solid particles, transferring the first mixed solution to a high-pressure reaction kettle, adding a piece of foamed nickel with the thickness of 8mm multiplied by 1mm, and carrying out hydrothermal treatment at 180 ℃ for 8 hours. Taking out MoO2-Ni(OH)2the/NF is put into a resistance furnace after being treated, nitrogen is introduced to lead the sulfur powder to be at the upstream and the MoO2-Ni(OH)2NF downstream, sulfur powder amount is MoO2-Ni(OH)2Calcining for 3 hours at the temperature of 500 ℃ by 1 time of the mass of/NF to finally obtain MoS2-NiS2/NF hydrogen evolution material.
Example 6
MoS of example 52-NiS2the/NF hydrogen evolution material is washed clean by ethanol and deionized water, and is dried in a vacuum oven for drying overnight and dried.
(1) Drying the MoS2-NiS2the/NF hydrogen evolution material is clamped by an electrode clamp and directly used as a working electrode for testing.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalysis electrolyte, introducing nitrogen to drive off air, and connecting a working electrode, an Ag/AgCl electrode and a stone grinding rod electrode to an electrochemical workstation.
Example 7
1.5mmol of sodium molybdate dihydrate
Nickel nitrate hexahydrate 1.5mmol
Urotropin 1.5mmol
Deionized water 60ml
Sulfur powder 10 times MoO2-Ni(OH)2mass/NF
MoS2-NiS2The NF hydrogen evolution material is prepared by the following stepsThe preparation method comprises the following steps:
dissolving 1.5mmol of sodium molybdate dihydrate, 1.5mmol of nickel nitrate hexahydrate and 1.5mmol of urotropine in 60mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 5min until the mixture is stirred and dissolved to obtain a first mixed solution. After the first mixed solution had no solid particles, the first mixed solution was transferred to a high-pressure autoclave, and a piece of nickel foam of 8mm × 8mm × 1mm was placed and heated at 130 ℃ for 6 hours. Taking out MoO2-Ni(OH)2the/NF is put into a resistance furnace after being treated, nitrogen is introduced to lead the sulfur powder to be at the upstream and the MoO2-Ni(OH)2the/NF is downstream. The amount of the sulfur powder is MoO2-Ni(OH)2Calcining the mixture for 1 hour at the temperature of 350 ℃ by 10 times of the mass of the NF to finally obtain the MoS2-NiS2/NF hydrogen evolution material.
Example 8
MoS of example 72-NiS2the/NF hydrogen evolution material is washed clean by ethanol and deionized water, and is dried in a vacuum oven for drying overnight and dried.
(1) Drying the MoS2-NiS2the/NF hydrogen evolution material is clamped by an electrode clamp and directly used as a working electrode for testing.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalysis electrolyte, introducing nitrogen to drive off air, and connecting a working electrode, an Ag/AgCl electrode and a stone grinding rod electrode to an electrochemical workstation.
Example 9
1.5mmol of sodium molybdate dihydrate
Nickel nitrate hexahydrate 1.5mmol
Urotropin 1.5mmol
Deionized water 60ml
Sulfur powder 10 times MoO2-Ni(OH)2mass/NF
MoS2-NiS2the/NF hydrogen evolution material is prepared by the following steps:
dissolving 1.5mmol of sodium molybdate dihydrate, 1.5mmol of nickel nitrate hexahydrate and 1.5mmol of urotropine in 60mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 5min until the mixture is stirred and dissolved to obtain a first mixed solution. See no solid particles in the first mixed solutionThereafter, the first mixed solution was transferred to a high-pressure autoclave, and a piece of foamed nickel of 8mm × 8mm × 1mm was put therein and heated at 150 ℃ for 6 hours. Taking out MoO2-Ni(OH)2the/NF is put into a resistance furnace after being treated, nitrogen is introduced to lead the sulfur powder to be at the upstream and the MoO2-Ni(OH)2NF downstream, sulfur powder amount is MoO2-Ni(OH)2Calcining for 1h at the temperature of 300 ℃ by 10 times of the mass of the/NF to finally obtain the MoS2-NiS2/NF hydrogen evolution material.
Example 10
The MoS of example 92-NiS2the/NF hydrogen evolution material is washed clean by ethanol and deionized water, and is dried in a vacuum oven for drying overnight and dried.
(1) Drying the MoS2-NiS2the/NF hydrogen evolution material is clamped by an electrode clamp and directly used as a working electrode for testing.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalysis electrolyte, introducing nitrogen to drive off air, and connecting a working electrode, an Ag/AgCl electrode and a stone grinding rod electrode to an electrochemical workstation.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. MoS2-NiS2The preparation method of the/NF hydrogen evolution material is characterized by comprising the following steps:
(1) dissolving sodium molybdate dihydrate, nickel nitrate hexahydrate and urotropine in deionized water to obtain a first mixed solution;
(2) transferring the first mixed solution obtained in the step (1) to a reaction kettle, taking foamed nickel as a carrier, and obtaining MoO through hydrothermal reaction2-Ni(OH)2/NF；
(3) MoO obtained in the step (2)2-Ni(OH)2/NF and sulfur powder are calcined under the anaerobic condition to obtain MoS2-NiS2/NF hydrogen evolution material.
2. A MoS according to claim 12-NiS2The preparation method of the/NF hydrogen evolution material is characterized in that in the step (1), the dosage ratio of sodium molybdate dihydrate, nickel nitrate hexahydrate, urotropine and deionized water is 1 mmol: 1 mmol: 1 mmol: (40-50) mL.
3. A MoS according to claim 12-NiS2The preparation method of the NF hydrogen evolution material is characterized in that in the step (2), the reaction temperature is 130-.
4. A MoS according to claim 12-NiS2The preparation method of the/NF hydrogen evolution material is characterized in that in the step (3), MoO2-Ni(OH)2The mass ratio of the/NF to the sulfur powder is 1: (1-10).
5. A MoS according to claim 12-NiS2The preparation method of the/NF hydrogen evolution material is characterized in that in the step (3), the calcination process is carried out in a resistance furnace, wherein sulfur powder is at the upstream and MoO is adopted2-Ni(OH)2the/NF is downstream.
6. A MoS according to claim 52-NiS2The preparation method of the/NF hydrogen evolution material is characterized in that the calcination process is carried out in a nitrogen environment.
7. A MoS according to claim 52-NiS2The preparation method of the NF hydrogen evolution material is characterized in that the calcination temperature is 300-500 ℃ and the calcination time is 1-3h in the calcination process.
8. MoS prepared by the method of any one of claims 1 to 72-NiS2/NF hydrogen evolution material.
9. The MoS of claim 82-NiS2Use of/NF hydrogen evolution material, characterized in that said MoS2-NiS2the/NF hydrogen evolution material is used for electrocatalytic hydrogen evolution reaction.
10. A MoS according to claim 92-NiS2Use of/NF hydrogen evolution material, characterized in that, in operation, MoS is converted into2-NiS2the/NF hydrogen evolution material is directly used as a working electrode during reaction and is fixed by an electrode clamp.
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