CN114016079A - Fe-Ni LDH-MoS2NGAs hydrogen evolution material and preparation method and application thereof - Google Patents
Fe-Ni LDH-MoS2NGAs hydrogen evolution material and preparation method and application thereof Download PDFInfo
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 239000001257 hydrogen Substances 0.000 title claims abstract description 116
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 116
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 62
- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 55
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 15
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 15
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 12
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 39
- 239000011259 mixed solution Substances 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 5
- 229920000557 Nafion® Polymers 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000006276 transfer reaction Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000012670 alkaline solution Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000003792 electrolyte Substances 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 14
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000004964 aerogel Substances 0.000 description 10
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 238000000227 grinding Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 8
- 229910021607 Silver chloride Inorganic materials 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- 239000007772 electrode material Substances 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000002604 ultrasonography Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000037361 pathway Effects 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 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
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002210 supercritical carbon dioxide drying Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Classifications
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- 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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
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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
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Catalysts (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention relates to the technical field of hydrogen energy, in particular to Fe-Ni LDH-MoS2/NGAs hydrogen evolution material and a preparation method and application thereof. Firstly, uniformly mixing a graphene oxide suspension and ethylenediamine, and then carrying out hydrothermal reaction to obtain NGAs; then sodium molybdate, thioacetamide and water are evenly mixed and pumped into a reaction kettle, NGAs is used as a carrier, and MoS is obtained through hydrothermal reaction2(ii)/NGAs; uniformly mixing ferric nitrate, nickel nitrate, ammonium fluoride, urea and water, and adding the mixture into MoS2in/NGAs, the mixture is transferred into a reaction kettle for hydrothermal reaction and dried to obtain Fe‑NiLDH‑MoS2/NGAs hydrogen evolving materials; the material is applied to electrocatalytic hydrogen evolution reaction. Compared with the prior art, the preparation method has the advantages of low raw material cost, simple preparation mode and good hydrogen and oxygen evolution effects in alkaline solution, and is expected to be oriented to industrial development.
Description
Technical Field
The invention relates to the technical field of hydrogen energy, in particular to Fe-Ni LDH-MoS2/NGAs 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 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.
In general, high activity HER electrocatalysts require several characteristics: inherently high specific surface area, high conductivity and fast electron transfer pathways, as well as a large number of active sites and fast mass transport pathways (including transport of reaction substrates and diffusion of gaseous products). Although Pt and Ru/Ir based composites are considered the most advanced electrocatalysts for HER and OER, their high cost and scarcity severely hamper large scale applications. Therefore, much research effort has been devoted to developing earth-abundant alternatives with high efficiency and stability.
Disclosure of Invention
In order to overcome the problem of catalytic hydrogen evolution in the prior art, the invention aims to provide Fe-Ni LDH-MoS2/NGAs hydrogen evolution material and a preparation method and application thereof. The Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is used as a catalyst, the synthesis cost is lower than that of most catalysts, and the earth reserves of main elements of Fe and Ni are sufficient. In the metal molybdenum, the 3d orbit is in a half-full state, has strong adsorption effect on hydrogen atoms, and is combined with the graphene oxide aerogel, so that the hydrogen evolution performance of the graphene oxide aerogel is greatly enhanced, the electrochemical performance of the graphene oxide aerogel is improved, and the synthesis method is simple.
The purpose of the invention can be realized by the following technical scheme:
the first purpose of the invention is to provide Fe-Ni LDH-MoS2The preparation method of the/NGAs hydrogen evolution material comprises the following steps:
(1) uniformly mixing the graphene oxide suspension with ethylenediamine, transferring the mixture to a hydrothermal kettle, and carrying out hydrothermal reaction to obtain NGAs;
(2) mixing sodium molybdate, thioacetamide and water uniformly to obtain a first mixed solution;
(3) adding the first mixed solution obtained in the step (2) into a reaction kettle, taking NGAs obtained in the step (1) as a carrier, and obtaining MoS after hydrothermal reaction2/NGAs；
(4) Mixing ferric nitrate and nitreUniformly mixing nickel acid, ammonium fluoride, urea and water, and adding the MoS obtained in the step (3)2In the/NGAs, standing to obtain a second mixed solution;
(5) carrying out hydrothermal reaction on the second mixed solution obtained in the step (4) in a transfer reaction kettle, and drying to obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
In one embodiment of the present invention, in the step (1), the volume ratio of the graphene oxide suspension to the ethylenediamine is 5: 1.
in one embodiment of the present invention, in the step (1), the reaction temperature is 150 ℃ to 200 ℃ and the reaction time is 10 to 15 hours during the hydrothermal reaction.
In one embodiment of the present invention, in step (2), the molar ratio of sodium molybdate to thioacetamide is 3: 4; the dosage ratio of the sodium molybdate to the water is 3 mmol: (150- & lt 250- & gt) mL.
In one embodiment of the present invention, in the step (3), the ratio of the amount of the first mixed solution to the amount of NGAs is 20 mL: 0.01 g.
In one embodiment of the present invention, in the step (3), the reaction temperature is 150-.
In one embodiment of the present invention, in step (4), the amount ratio of iron nitrate, nickel nitrate, ammonium fluoride and urea to water is 2 mmol: 3 mmol: 3 mmol: 1 mmol: 30 ml.
In one embodiment of the present invention, in the step (5), the reaction temperature is 110-150 ℃ and the reaction time is 10-15h during the hydrothermal reaction.
The second purpose of the invention is to provide Fe-Ni LDH-MoS prepared by the method2/NGAs hydrogen evolution materials.
The third purpose of the invention is to provide the Fe-Ni LDH-MoS2Application of/NGAs hydrogen evolution material, Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is used for electrocatalytic hydrogen and oxygen evolution reaction.
In one embodiment of the invention, Fe-Ni LDH-MoS is added2the/NGAs hydrogen evolution material is uniformly mixed with Nafion solution, dripped on a glassy carbon electrode, and driedThen obtaining the hydrogen evolution glassy carbon electrode which is used as a working electrode in the electrocatalytic hydrogen evolution reaction.
In one embodiment of the invention, Fe-Ni LDH-MoS2The application method of the NGAs hydrogen evolution material for electrocatalytic hydrogen and oxygen evolution reaction specifically comprises the following steps:
(1) weighing 5mg of Fe-Ni LDH-MoS2Dissolving the/NGAs hydrogen evolution material in 30 mu L of prepared 0.5 wt% of a Nation solution, uniformly dispersing for half an hour under ultrasonic, sucking 12-18 mu L of the solution on a glassy carbon electrode, and naturally airing to obtain the hydrogen evolution glassy carbon electrode;
(2) preparing 1.0M potassium hydroxide solution as electrocatalytic electrolyte, introducing nitrogen to remove air, cleaning the surface of the glassy carbon electrode by using 1.0M potassium hydroxide solution, connecting the hydrogen evolution glassy carbon electrode, the Ag/AgCl electrode and the graphite electrode to an electrochemical workstation, and carrying out electrocatalytic hydrogen evolution reaction in the electrolyte.
In one embodiment of the present invention, the purpose of the hydrothermal reaction is: the reaction is promoted to be carried out in a high-temperature and high-pressure environment, and the obtained NGAs are uniform, free of agglomeration, good in crystal form and MoS2Can be better loaded on the graphene oxide aerogel. The secondary hydrothermal reaction causes Fe-Ni LDH to be loaded on MoS2the/NGAs surface is tightly combined, and is more beneficial to hydrogen evolution and oxygen evolution. Wherein MoS2As the active site for hydrogen evolution, Fe-Ni LDH is taken as the active site for oxygen evolution, and the two sites supplement each other to further promote the complete decomposition of water.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the present invention, the graphene oxide aerogel is generally obtained by supercritical carbon dioxide drying or freeze drying of a wet gel to replace a solvent with air, and is a three-dimensional (3D) porous solid material including high porosity, excellent mass transfer capacity, and low bulk density and dielectric constant. The graphene oxide aerogel serving as one of graphene-based porous materials not only can inherit the excellent internal performance of graphene, but also has a large specific surface area, and the graphene oxide aerogel has high porosity and an interconnected network structure and can improve the material performance.
(2) Fe-Ni LDH-MoS prepared by the invention2The graphene oxide aerogel in the/NGAs hydrogen evolution material has a three-dimensional framework structure, and the re-stacking of graphene sheets can be effectively inhibited, so that the large specific surface area of graphene can be kept, and a plurality of accessible active sites can be exposed; the abundant porous structure can store electrolyte and provide more mass transfer channels, thereby shortening the mass transfer distance and accelerating the mass transfer; highly crystalline and interconnected graphene sheets can provide more electron transport paths, facilitating the conduction of electrons; the surface of the graphene oxide aerogel is easy to modify, and the graphene is endowed with a catalytic function.
(3) The invention relates to Fe-Ni LDH-MoS2The preparation method of the/NGAs hydrogen evolution material has low raw material cost and simple preparation mode, and the prepared Fe-Ni LDH-MoS2The NGAs hydrogen evolution material has good hydrogen evolution effect, and the introduction of non-noble metal elements ensures that the material has good stability. The water is electrolyzed in the alkaline medium, and the hydrogen evolution effect is good.
Detailed Description
The invention provides Fe-Ni LDH-MoS2The preparation method of the/NGAs hydrogen evolution material comprises the following steps:
(1) uniformly mixing the graphene oxide suspension with ethylenediamine, transferring the mixture to a hydrothermal kettle, and carrying out hydrothermal reaction to obtain NGAs;
(2) mixing sodium molybdate, thioacetamide and water uniformly to obtain a first mixed solution;
(3) adding the first mixed solution obtained in the step (2) into a reaction kettle, taking NGAs obtained in the step (1) as a carrier, and obtaining MoS after hydrothermal reaction2/NGAs；
(4) Uniformly mixing ferric nitrate, nickel nitrate, ammonium fluoride, urea and water, and adding the MoS obtained in the step (3)2In the/NGAs, standing to obtain a second mixed solution;
(5) carrying out hydrothermal reaction on the second mixed solution obtained in the step (4) in a transfer reaction kettle, and drying to obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
In one embodiment of the present invention, in the step (1), the volume ratio of the graphene oxide suspension to the ethylenediamine is 5: 1.
in one embodiment of the present invention, in the step (1), the reaction temperature is 150 ℃ to 200 ℃ and the reaction time is 10 to 15 hours during the hydrothermal reaction.
In one embodiment of the present invention, in step (2), the molar ratio of sodium molybdate to thioacetamide is 3: 4; the dosage ratio of the sodium molybdate to the water is 3 mmol: (150- > 250) mL.
In one embodiment of the present invention, in the step (3), the ratio of the amount of the first mixed solution to the amount of NGAs is 20 mL: 0.01 g.
In one embodiment of the present invention, in the step (3), the reaction temperature is 150-.
In one embodiment of the present invention, in step (4), the amount ratio of iron nitrate, nickel nitrate, ammonium fluoride and urea to water is 2 mmol: 3 mmol: 3 mmol: 1 mmol: 30 ml.
In one embodiment of the present invention, in the step (5), the reaction temperature is 110-150 ℃ and the reaction time is 10-15h during the hydrothermal reaction.
The invention provides Fe-Ni LDH-MoS prepared by the method2/NGAs hydrogen evolution materials.
The invention provides the Fe-Ni LDH-MoS2Application of/NGAs hydrogen evolution material, Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is used for electrocatalytic hydrogen and oxygen evolution reaction.
In one embodiment of the invention, Fe-Ni LDH-MoS is added2the/NGAs hydrogen evolution material is uniformly mixed with Nafion solution, then is dripped on a glassy carbon electrode, and is dried to obtain the hydrogen evolution glassy carbon electrode which is used as a working electrode in the electrocatalytic hydrogen evolution reaction.
In one embodiment of the invention, Fe-Ni LDH-MoS2The application method of the NGAs hydrogen evolution material for electrocatalytic hydrogen and oxygen evolution reaction specifically comprises the following steps:
(1) weighing 5mg of Fe-Ni LDH-MoS2Dissolving the/NGAs hydrogen evolution material in 30 mu L of prepared 0.5 wt% of Nation solution, uniformly dispersing for half an hour under ultrasound, and absorbing 12-Putting 18 mu L of the solution on a glassy carbon electrode, and naturally airing to obtain a hydrogen evolution glassy carbon electrode;
(2) preparing 1.0M potassium hydroxide solution as electrocatalytic electrolyte, introducing nitrogen to remove air, cleaning the surface of the glassy carbon electrode by using 1.0M potassium hydroxide solution, connecting the hydrogen evolution glassy carbon electrode, the Ag/AgCl electrode and the graphite electrode to an electrochemical workstation, and carrying out electrocatalytic hydrogen evolution reaction in the electrolyte.
In one embodiment of the present invention, the purpose of the hydrothermal reaction is: the reaction is promoted to be carried out in a high-temperature and high-pressure environment, and the obtained NGAs are uniform, free of agglomeration, good in crystal form and MoS2Can be better loaded on the graphene oxide aerogel. The secondary hydrothermal reaction causes Fe-Ni LDH to be loaded on MoS2the/NGAs surface is tightly combined, and is more beneficial to hydrogen evolution and oxygen evolution. Wherein MoS2As the active site for hydrogen evolution, Fe-Ni LDH is taken as the active site for oxygen evolution, and the two sites supplement each other to further promote the complete decomposition of water.
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
This example provides a Fe-Ni LDH-MoS2Preparation method of NGAs hydrogen evolution material.
Adding 2ml of ethylenediamine into 10ml of graphene oxide suspension, stirring, and then transferring to a hydrothermal kettle for reaction at 180 ℃ for 12h to obtain NGAs. Dissolving 0.3mmol of sodium molybdate and 0.4mmol of thioacetamide in 20mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 2 hours until the mixture is stirred and dissolved to obtain a first mixed solution. After no solid particles exist in the solution, NGAs is put into the first mixed solution, stands for 30 minutes and is transferred to a high-pressure reaction kettle, and then is heated for 24 hours under the temperature of 200 ℃. Remove the MoS2/NGAs. Adding 0.2mmol of ferric nitrate, 0.3mmol of nickel nitrate, 0.3mmol of ammonium fluoride and 0.1mmol of urea into 30ml of deionized water, stirring for 30 minutes, and adding MoS2/NGAs stands for 20 minutes to obtain a second mixed solution; then transferring the mixture into a hydrothermal kettle for reaction at 120 ℃ for 12h, cooling the mixture, taking out the mixture for washing at 60 DEG CVacuum drying overnight to finally obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
Example 2
The Fe-Ni LDH-MoS of example 1 was added2Grinding the/NGAs hydrogen evolution material, grinding the surface of the glassy carbon electrode by using 0.05 mu m of alumina, removing a residual sample, washing by using ethanol and deionized water, and airing.
(1) Nation solution was made up to 0.5 wt% with anhydrous methanol. Weighing 5mg of Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is dissolved in 30 mu L of prepared Nation solution and evenly dispersed for half an hour under ultrasound. Then sucking 12 mu L of the solution on a glassy carbon electrode, and naturally airing to obtain the hydrogen evolution glassy carbon electrode.
(2) Preparing 1.0M potassium hydroxide solution as an electrocatalytic electrolyte, introducing nitrogen to drive away air, cleaning the electrode surface of the hydrogen evolution glassy carbon electrode by using the 1.0M potassium hydroxide solution, connecting the hydrogen evolution glassy carbon electrode, the Ag/AgCl electrode and the graphite electrode to an electrochemical workstation, and measuring the electrocatalytic hydrogen evolution performance of the electrode material in the electrolyte.
Example 3
This example provides a Fe-Ni LDH-MoS2Preparation method of NGAs hydrogen evolution material.
Adding 2ml of ethylenediamine into 10ml of graphene oxide suspension, stirring, and then transferring to a hydrothermal kettle for reaction at 150 ℃ for 10h to obtain NGAs. Dissolving 0.3mmol of sodium molybdate and 0.4mmol of thioacetamide in 25mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 2 hours until the mixture is stirred and dissolved to obtain a first mixed solution. And after no solid particles exist in the solution, NGAs is put into the first mixed solution, stands for 30 minutes and is transferred to a high-pressure reaction kettle, and then is heated for 20 hours at 150 ℃. Remove the MoS2/NGAs. Adding 0.2mmol of ferric nitrate, 0.3mmol of nickel nitrate, 0.3mmol of ammonium fluoride and 0.1mmol of urea into 30ml of deionized water, stirring for 30 minutes, and adding MoS2/NGAs stands for 20 minutes to obtain a second mixed solution; then transferring the mixture into a hydrothermal kettle for reaction at 110 ℃ for 10h, cooling, taking out and washing, and carrying out vacuum drying at 60 ℃ overnight to finally obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
Example 4
The Fe-Ni LDH-MoS of example 3 was added2Grinding the/NGAs hydrogen evolution material, grinding the surface of the glassy carbon electrode by using 0.05 mu m of alumina, removing a residual sample, washing by using ethanol and deionized water, and airing.
(1) 0.5 wt% of Nation solution was prepared with anhydrous methanol. Weighing 5mg of Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is dissolved in 30 mu L of prepared Nation solution and is homogenized under ultrasound for half an hour. Then sucking 12 mu L of the solution on a glassy carbon electrode, and naturally airing to obtain the hydrogen evolution glassy carbon electrode.
(2) Preparing 1.0M potassium hydroxide solution as an electrocatalytic electrolyte, introducing nitrogen to drive away air, cleaning the electrode surface of the hydrogen evolution glassy carbon electrode by using the 1.0M potassium hydroxide solution, connecting the hydrogen evolution glassy carbon electrode, the Ag/AgCl electrode and the graphite electrode to an electrochemical workstation, and measuring the electrocatalytic hydrogen evolution performance of the electrode material in the electrolyte.
Example 5
This example provides a Fe-Ni LDH-MoS2Preparation method of NGAs hydrogen evolution material.
Adding 2ml of ethylenediamine into 10ml of graphene oxide suspension, stirring, and then transferring to a hydrothermal kettle for reaction at 200 ℃ for 15h to obtain NGAs. Dissolving 0.3mmol of sodium molybdate and 0.4mmol of thioacetamide in 15mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 2 hours until the mixture is stirred and dissolved to obtain a first mixed solution. And after no solid particles exist in the solution, NGAs is put into the first mixed solution, stands for 30 minutes and is transferred to a high-pressure reaction kettle, and then is heated for 22 hours at 180 ℃. Remove the MoS2/NGAs. Adding 0.2mmol of ferric nitrate, 0.3mmol of nickel nitrate, 0.3mmol of ammonium fluoride and 0.1mmol of urea into 30ml of deionized water, stirring for 30 minutes, and adding MoS2/NGAs stands for 20 minutes to obtain a second mixed solution; then transferring the mixture into a hydrothermal kettle to react for 15h at the temperature of 150 ℃, cooling the mixture, taking out the mixture to wash the mixture, and drying the mixture overnight in vacuum at the temperature of 60 ℃ to finally obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
Example 6
The Fe-Ni LDH-MoS of example 5 was added2Research on/NGAs hydrogen evolution materialGrinding, namely grinding the surface of the glassy carbon electrode by using 0.05 mu m of alumina, removing a residual sample, washing by using ethanol and deionized water, and airing.
(1) 0.5 wt% of Nation solution was prepared with anhydrous methanol. Weighing 5mg of Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is dissolved in 30 mu L of prepared Nation solution and evenly dispersed for half an hour under ultrasound. Then sucking 12 mu L of the solution on a glassy carbon electrode, and naturally airing to obtain the hydrogen evolution glassy carbon electrode.
(2) Preparing 1.0M potassium hydroxide solution as an electrocatalytic electrolyte, introducing nitrogen to drive away air, cleaning the electrode surface of the hydrogen evolution glassy carbon electrode by using the 1.0M potassium hydroxide solution, connecting the hydrogen evolution glassy carbon electrode, the Ag/AgCl electrode and the graphite electrode to an electrochemical workstation, and measuring the electrocatalytic hydrogen evolution performance of the electrode material in the electrolyte.
Example 7
This example provides a Fe-Ni LDH-MoS2Preparation method of NGAs hydrogen evolution material.
Adding 2ml of ethylenediamine into 10ml of graphene oxide suspension, stirring, and then transferring to a hydrothermal kettle for reaction at 150 ℃ for 10h to obtain NGAs. Dissolving 0.3mmol of sodium molybdate and 0.4mmol of thioacetamide in 20mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 2 hours until the mixture is stirred and dissolved to obtain a first mixed solution. And after no solid particles exist in the solution, NGAs is put into the first mixed solution, stands for 30 minutes and is transferred to a high-pressure reaction kettle, and then is heated for 20 hours at 150 ℃. Remove the MoS2/NGAs. Adding 0.2mmol of ferric nitrate, 0.3mmol of nickel nitrate, 0.3mmol of ammonium fluoride and 0.1mmol of urea into 30ml of deionized water, stirring for 30 minutes, and adding MoS2/NGAs stands for 20 minutes to obtain a second mixed solution; then transferring the mixture into a hydrothermal kettle for reaction at 110 ℃ for 10h, cooling, taking out and washing, and carrying out vacuum drying at 60 ℃ overnight to finally obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
Example 8
The Fe-Ni LDH-MoS of example 7 was added2Grinding the/NGAs hydrogen evolution material, grinding the surface of the glassy carbon electrode by using 0.05 mu m of aluminum oxide, removing the residual sample, and using ethanol and deionized waterAnd (5) washing and drying.
(1) 0.5 wt% of Nation solution was prepared with anhydrous methanol. Weighing 5mg of Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is dissolved in 30 mu L of prepared Nation solution and is homogenized under ultrasound for half an hour. Then sucking 12 mu L of the solution on a glassy carbon electrode, and naturally airing to obtain the hydrogen evolution glassy carbon electrode.
(2) Preparing 1.0M potassium hydroxide solution as an electrocatalytic electrolyte, introducing nitrogen to drive away air, cleaning the electrode surface of the hydrogen evolution glassy carbon electrode by using the 1.0M potassium hydroxide solution, connecting the hydrogen evolution glassy carbon electrode, the Ag/AgCl electrode and the graphite electrode to an electrochemical workstation, and measuring the electrocatalytic hydrogen evolution performance of the electrode material in the electrolyte.
Example 9
This example provides a Fe-Ni LDH-MoS2Preparation method of NGAs hydrogen evolution material.
Adding 2ml of ethylenediamine into 10ml of graphene oxide suspension, stirring, and then transferring to a hydrothermal kettle for reaction at 150 ℃ for 10h to obtain NGAs. Dissolving 0.3mmol of sodium molybdate and 0.4mmol of thioacetamide in 20mL of deionized water, and carrying out ultrasonic treatment in an ultrasonic oscillator for 2 hours until the mixture is stirred and dissolved to obtain a first mixed solution. And after no solid particles exist in the solution, NGAs is put into the first mixed solution, stands for 30 minutes and is transferred to a high-pressure reaction kettle, and then is heated for 20 hours at 150 ℃. Remove the MoS2/NGAs. Adding 0.2mmol of ferric nitrate, 0.3mmol of nickel nitrate, 0.3mmol of ammonium fluoride and 0.1mmol of urea into 30ml of deionized water, stirring for 30 minutes, and adding MoS2/NGAs stands for 20 minutes to obtain a second mixed solution; then transferring the mixture into a hydrothermal kettle to react for 12 hours at 120 ℃, cooling the mixture, taking out the mixture to wash the mixture, and drying the mixture overnight in vacuum at 60 ℃ to finally obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
Example 10
The Fe-Ni LDH-MoS of example 9 was added2Grinding the/NGAs hydrogen evolution material, grinding the surface of the glassy carbon electrode by using 0.05 mu m of alumina, removing a residual sample, washing by using ethanol and deionized water, and airing.
(1) 0.5 wt% of Nation solution was prepared with anhydrous methanol. Weighing 5mg of Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is dissolved in 30 mu L of prepared Nation solution and is homogenized under ultrasound for half an hour. Then sucking 12 mu L of the solution on a glassy carbon electrode, and naturally airing to obtain the hydrogen evolution glassy carbon electrode.
(2) Preparing 1.0M potassium hydroxide solution as an electrocatalytic electrolyte, introducing nitrogen to drive away air, cleaning the electrode surface of the hydrogen evolution glassy carbon electrode by using the 1.0M potassium hydroxide solution, connecting the hydrogen evolution glassy carbon electrode, the Ag/AgCl electrode and the graphite electrode to an electrochemical workstation, and measuring the electrocatalytic hydrogen evolution performance of the electrode material in the electrolyte.
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. Fe-Ni LDH-MoS2The preparation method of the/NGAs hydrogen evolution material is characterized by comprising the following steps:
(1) uniformly mixing the graphene oxide suspension with ethylenediamine, transferring the mixture to a hydrothermal kettle, and carrying out hydrothermal reaction to obtain NGAs;
(2) mixing sodium molybdate, thioacetamide and water uniformly to obtain a first mixed solution;
(3) adding the first mixed solution obtained in the step (2) into a reaction kettle, taking NGAs obtained in the step (1) as a carrier, and obtaining MoS after hydrothermal reaction2/NGAs；
(4) Uniformly mixing ferric nitrate, nickel nitrate, ammonium fluoride, urea and water, and adding the MoS obtained in the step (3)2In the/NGAs, standing to obtain a second mixed solution;
(5) carrying out hydrothermal reaction on the second mixed solution obtained in the step (4) in a transfer reaction kettle, and drying to obtain Fe-Ni LDH-MoS2/NGAs hydrogen evolution materials.
2. A Fe-Ni LDH-MoS as claimed in claim 12The preparation method of the/NGAs hydrogen evolution material is characterized in that in the step (1), the volume ratio of the graphene oxide suspension to the ethylenediamine is 5: 1.
3. a Fe-Ni LDH-MoS as claimed in claim 12The preparation method of the/NGAs hydrogen evolution material is characterized in that in the step (1), the reaction temperature is 150-.
4. A Fe-Ni LDH-MoS as claimed in claim 12The preparation method of the/NGAs hydrogen evolution material is characterized in that in the step (2), the molar ratio of sodium molybdate to thioacetamide is 3: 4; the dosage ratio of the sodium molybdate to the water is 3 mmol: (150- & lt 250- & gt) mL.
5. A Fe-Ni LDH-MoS as claimed in claim 12The preparation method of the/NGAs hydrogen evolution material is characterized in that in the step (3), the reaction temperature is 150-.
6. A Fe-Ni LDH-MoS as claimed in claim 12The preparation method of the/NGAs hydrogen evolution material is characterized in that in the step (4), the dosage ratio of the ferric nitrate, the nickel nitrate, the ammonium fluoride, the urea and the water is 2 mmol: 3 mmol: 3 mmol: 1 mmol: 30 ml.
7. The method for preparing Fe-Ni LDH-MoS2/NGAs hydrogen evolution material as claimed in claim 1, wherein in the step (5), the reaction temperature is 110-150 ℃ and the reaction time is 10-15h in the hydrothermal reaction process.
8. Fe-Ni LDH-MoS prepared by the method of any one of claims 1 to 72/NGAs hydrogen evolution materials.
9. Fe-Ni LDH-MoS as claimed in claim 82Use of/NGAs hydrogen evolution materials, characterized in that the Fe-Ni LDH-MoS2the/NGAs hydrogen evolution material is used for electrocatalytic hydrogen and oxygen evolution reaction.
10. An Fe-Ni LDH-MoS as claimed in claim 92The application of/NGAs hydrogen evolution material is characterized in that Fe-Ni LDH-MoS is added2the/NGAs hydrogen evolution material is uniformly mixed with Nafion solution, then is dripped on a glassy carbon electrode, and is dried to obtain the hydrogen evolution glassy carbon electrode which is used as a working electrode in the electrocatalytic hydrogen evolution reaction.
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