CN110876946B - MoS 2 -RGO-NiO @ Ni foam composite photoelectrocatalysis hydrogen evolution material and preparation method thereof - Google Patents
MoS 2 -RGO-NiO @ Ni foam composite photoelectrocatalysis hydrogen evolution material and preparation method thereof Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 46
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000006260 foam Substances 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000463 material Substances 0.000 title abstract description 10
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 title description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000003618 dip coating Methods 0.000 claims abstract description 9
- 229910021382 natural graphite Inorganic materials 0.000 claims abstract description 7
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 6
- 239000005078 molybdenum compound Substances 0.000 claims abstract description 5
- 150000002752 molybdenum compounds Chemical class 0.000 claims abstract description 5
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 5
- 239000007800 oxidant agent Substances 0.000 claims abstract description 5
- 150000003464 sulfur compounds Chemical class 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims abstract description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 50
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 50
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- -1 polytetrafluoroethylene Polymers 0.000 claims description 12
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- UCGFRIAOVLXVKL-UHFFFAOYSA-N benzylthiourea Chemical compound NC(=S)NCC1=CC=CC=C1 UCGFRIAOVLXVKL-UHFFFAOYSA-N 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- KQJQICVXLJTWQD-UHFFFAOYSA-N N-Methylthiourea Chemical compound CNC(N)=S KQJQICVXLJTWQD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008118 PEG 6000 Substances 0.000 claims description 3
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 claims description 3
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- PVTGORQEZYKPDK-UHFFFAOYSA-N ethenylthiourea Chemical compound NC(=S)NC=C PVTGORQEZYKPDK-UHFFFAOYSA-N 0.000 claims description 3
- PDDXOPNEMCREGN-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum;hydrate Chemical compound O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O PDDXOPNEMCREGN-UHFFFAOYSA-N 0.000 claims description 3
- 229920000136 polysorbate Polymers 0.000 claims description 3
- 229950008882 polysorbate Drugs 0.000 claims description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229920002535 Polyethylene Glycol 1500 Polymers 0.000 claims description 2
- 229920002594 Polyethylene Glycol 8000 Polymers 0.000 claims description 2
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 125000005456 glyceride group Chemical group 0.000 claims description 2
- 229910052961 molybdenite Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- 229920002523 polyethylene Glycol 1000 Polymers 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000005187 foaming Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 229910021389 graphene Inorganic materials 0.000 description 13
- 239000002202 Polyethylene glycol Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 7
- 239000010411 electrocatalyst Substances 0.000 description 7
- 238000011056 performance test Methods 0.000 description 7
- 238000012546 transfer Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- RBORURQQJIQWBS-QVRNUERCSA-N (4ar,6r,7r,7as)-6-(6-amino-8-bromopurin-9-yl)-2-hydroxy-2-sulfanylidene-4a,6,7,7a-tetrahydro-4h-furo[3,2-d][1,3,2]dioxaphosphinin-7-ol Chemical compound C([C@H]1O2)OP(O)(=S)O[C@H]1[C@@H](O)[C@@H]2N1C(N=CN=C2N)=C2N=C1Br RBORURQQJIQWBS-QVRNUERCSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 230000036561 sun exposure Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
- 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
- B01J35/39—Photocatalytic properties
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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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or 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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Abstract
The invention discloses a method for preparing MoS by a sol dip-coating method 2 the-RGO-NiO @ Ni foam hydrogen evolution material and the preparation method thereof specifically comprise the following steps: (1) dissolving molybdenum compound, sulfur compound and nonionic surfactant in a weight ratio of (2-10): (4-12):1 in deionized water, and carrying out hydrothermal treatment at 140- 2 (ii) a (2) Processing natural graphite powder by an improved Hummer method to prepare RGO; (3) soaking foamed nickel in a solution with the concentration of 0.2-1.0M and containing an oxidant for 20-50min to obtain NiO @ Ni; (4) the prepared MoS 2 Dispersing RGO in PEG solution to obtain suspension sol solution; (5) and soaking, lifting and drying the NiO @ Ni in the suspension sol solution for many times, and carrying out temperature programming roasting and heat preservation under the atmosphere protection to obtain the three-dimensional porous foam nickel-based photoelectrocatalysis hydrogen evolution composite material.
Description
Technical Field
The invention relates to a method for preparing MoS by a sol dip coating method 2 an-RGO-NiO @ Ni foam hydrogen evolution composite material and a preparation method thereof, in particular to a method for pre-oxidizing foam nickel to obtain nickel-based nickel oxide and preparing newly prepared MoS 2 And dispersing RGO in a PEG solution to obtain a suspension sol solution, performing multiple times of dipping, lifting, drying, performing temperature programming roasting under the atmosphere protection, performing heat preservation in a reducing atmosphere, and naturally cooling to obtain the material, wherein the prepared material shows excellent performance of producing hydrogen by decomposing water through photoelectrocatalysis.
Background
For the development of renewable and clean energy sources, in particular hydrogen (H) 2 ) New technologies of energy to replace traditional fossil fuels, technologists have made many efforts. Photocatalytic/electrocatalytic Hydrogen Evolution (HER) is considered a promising hydrogen production strategy. Although noble metals (Pt, Pd, Rh, etc.) can be effective HER catalysts, they are costly and scarceSeverely hampering its practical application. Therefore, there is an urgent need to find alternative catalysts that are efficient, low cost and environmentally friendly.
Among numerous hydrogen production methods, the hydrogen production by water electrolysis has a long history, long industrialization time, high product purity, no pollution, rich and renewable raw materials, and no carbon emission in the production and use processes, and is a mature large-scale hydrogen production technology. At present, research aiming at the water electrolysis hydrogen production technology mainly focuses on exploring and synthesizing (photo) electrocatalyst materials, and hydrogen evolution overvoltage is reduced by using (photo) electrocatalysts, so that energy consumption and production cost can be reduced. Therefore, a key factor affecting large-scale industrial application of hydrogen production by water electrolysis is the hydrogen evolution catalyst. As is well known, Pt has excellent properties such as high catalytic activity, low overpotential, small Tafel slope, and good stability as a hydrogen evolution electrode, and is the most deeply studied electrode material. However, the Pt group, as a noble metal, is low in abundance in the earth's crust and exhibits considerable scarcity, limiting its wide application in the electrolytic water industry. Therefore, the electrode active material with high development efficiency, low manufacturing cost, high abundance, low overpotential and stable operation replaces a noble metal catalyst, and is a research hotspot of hydrogen evolution reaction.
More recently, transition metals and their related compounds, including oxides, nitrides, phosphides, carbides and sulfides, have been extensively studied and proven to be potential catalysts for HER. Among these compounds, molybdenum disulfide (MoS) having a layered structure 2 ) Have proven to be excellent alternatives to noble metal electrocatalysts. However, the accumulation and agglomeration of the molybdenum disulfide layer reduces its active sites and conductivity, which is detrimental to the hydrogen evolution reaction. To solve these problems, many efforts have been made, and one possible approach is to subject MoS to a stress 2 Nanomaterials associated with highly conductive supports, particularly carbon, such as nanotubes, nanofibres, nanowires, activated carbon, porous carbon, g-C 3 N 4 Graphene, etc. For example, the Li subject group will MoS 2 Coupled with N-doped carbon nanotubes to enhance HER activity. Lai subject group prepared nitrogen-doped carbon nanofiber/MoS with high HER efficiency 2 A nanocomposite material. Liu subject group in waterReduced Graphene Oxide (RGO) is used in the thermal process, and CoS can be well distributed 2 /MoS 2 And the electrical conductivity is improved. In addition, the prepared electrocatalyst needs to be supported on an electrically conductive substrate. The three-dimensional porous nickel foam with rich content and good conductivity is widely used as the framework support of the water decomposition electrocatalyst. Electrocatalysts are typically deposited on a substrate by a drip method, however, drip of conventional electrocatalysts on a substrate presents a peeling problem that reduces the electrocatalytic performance.
In view of all the above factors, it is of great interest to prepare an effective HER system with more exposed active sites and a close interaction between the active catalyst particles and the matrix. In this context, graphene, MoS is considered 2 And foam nickel to prepare a composite material, the composite material is mixed with pure foam nickel, NiO @ Ni and MoS 2 the-NiO @ Ni samples should exhibit superior HER performance compared to the active MoS 2 Good dispersion with conductive graphene and MoS 2 The intimate interfacial contact between graphene and nickel foam has a positive and synergistic electrocatalytic decomposition effect on water to produce hydrogen.
Disclosure of Invention
The invention aims to provide a graphene-based Metal Oxide Semiconductor (MOS) prepared from graphene and MoS 2 And polyethylene glycol (PEG) to form a sol, which is coated on the pre-oxidized nickel foam to form a sol containing MoS 2 The RGO and in-situ NiO foam Ni-based composite material and the preparation method thereof solve the problems of too high hydrogen evolution overpotential, poor material circulation stability and the like of the conventional electrocatalytic hydrogen production material.
In order to solve the technical problem, the NiO @ Ni foam is obtained by oxidizing foam nickel in situ. Preparing RGO by treating natural graphite powder with improved Hummer method, and synthesizing MoS by hydrothermal method 2 And then obtaining MoS by sol-assisted dip coating 2 -RGO-NiO @ Ni composite. Compared with the reported preparation method, the synthesis process has unique characteristics, and the optimal composite material prepared by adopting the sol-assisted dip coating method is 10mA/cm 2 Only 150 mV of low overpotential is needed, and the Tafel slope is 80 mV/dec; HER activity was further enhanced under simulated solar irradiation. The specific technical proposal comprises thatAnd (5) next step.
(1) Dissolving a molybdenum compound, a sulfur compound and a nonionic surfactant in a weight ratio of (2-10): 4-12):1 in 120mL of deionized water under continuous stirring, transferring the mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal treatment at 140- 2 Washing with deionized water, centrifuging, and vacuum drying.
(2) RGO is prepared by treating natural graphite powder with improved Hummer method.
(3) Dissolving PEG surfactant in hot deionized water, and adding MoS obtained in step (1) 2 Dispersing the RGO obtained in the step (2) in a PEG solution, performing ultrasonic treatment for 30min to form stable suspension sol, and adding the stable suspension sol into 100mL of deionized water according to the mass ratio of W PEG :W MoS2 :W RGO =10:(0.1-1.0):(0.02-0.2)。
(4) Soaking the foamed nickel in 0.2-1.0M solution containing oxidant for 20-50min to obtain nickel pre-oxide foam (NiO @ Ni).
(5) And (3) immersing the NiO @ Ni obtained in the step (4) into the suspension sol obtained in the step (3) for 1-4 min, then pulling at the speed of 1mm/s, and drying at the temperature of 60 ℃. Repeating the processes of dipping, pulling and drying for 3-8 times.
(6) Placing the product obtained in the step (5) in a tubular furnace, performing temperature programming roasting to 300-600 ℃ under the atmosphere protection, switching to protective gas containing a certain reducing atmosphere, preserving heat for 1-3h, and naturally cooling to room temperature to obtain the MoS with the required load capacity 2 -RGO-NiO @ Ni composite.
On the basis of the scheme, the molybdenum compound in the step (1) is one or a mixture of more of molybdenum acetylacetonate, molybdenum chloride, molybdenum trioxide, dodecamolybdophosphoric acid, ammonium phosphomolybdate and sodium phosphomolybdate; the sulfur compound is one or a mixture of more of thiourea, vinyl thiourea, methyl isothiourea and benzylthiourea; the nonionic surfactant is one or more of fatty glyceride, sorbitan fatty acid, polysorbate and polyoxyethylene.
On the basis of the scheme, the PEG in the step (3) is one or a mixture of more of PEG1000, PEG1500, PEG2000, PEG4000, PEG6000 and PEG 8000.
On the basis of the scheme, the oxidant in the step (4) is HNO 3 、H 2 SO 4 、KMnO 4 、H 2 O 2、 KClO 3 、KClO 4 One or more of the above-mentioned materials.
On the basis of the scheme, the protective gas in the step (6) is one or a mixture of several of argon, helium, nitrogen and carbon dioxide; the reducing atmosphere is prepared by adding 0.5-5 vol% of H into protective gas 2 CO and SO 2 One or more of them.
On the basis of the scheme, the sample obtained in the step (6) is characterized, and the diffraction peak of the sample is consistent with the standard pattern of hexagonal molybdenum disulfide (JCPDS card number 37-1492) as can be seen from the enlarged image of the upper left corner of the XRD pattern (figure 1). The sample had stronger diffraction peaks at 44.8 °, 52.2 ° and 76.8 °, due to the (111), (200) and (220) crystal planes of cubic metallic nickel (JCPDS card number 04-0850), respectively. The foam nickel after preoxidation has weak diffraction peaks at 37.2 degrees, 43.3 degrees and 62.9 degrees, which are matched with the hexagon of NiO (JCPDS card number 44-1159), and the NiO is formed on the surface of the foam nickel. By further coating with MoS 2 The NiO diffraction peak disappears after the composite material is formed by the NiO and the graphene, and is due to MoS 2 And graphene coverage. The morphology and the nanostructure of different foam nickel-based samples were characterized by SEM, TEM and HRTEM analyses, indicating that the Ni foam had been pre-oxidized and covered with a thin film consisting of NiO nanoparticles, MoS on the surface of the pre-oxidized nickel foam 2 The particles are stacked and agglomerated with each other (fig. 2). As is clear from FIG. 3, MoS 2 The nano-sheets are well loaded and dispersed on the graphene micro-sheets, and the distinguishable lattice spacing (0.62 nm) corresponds to MoS 2 (002) van der Waals planes.
On the basis of the scheme, the product obtained in the step (6)The composite material is subjected to electrochemical performance test through an electrochemical workstation, and the composite electrode material shows good HER performance under the optimal condition, wherein the HER performance is 10mA/cm 2 The overpotential under current of (1) is 150 mV (FIG. 4), which is significantly less than the overpotential of pure nickel foam (204 mV), NiO @ Ni overpotential (194 mV), MoS 2 -NiO @ Ni overpotential (169 mV); tafel slope of 80mv/dec (FIG. 5), significantly less than pure nickel foam, NiO @ Ni and MoS 2 Tafel slope of NiO @ Ni (169, 167 and 135mV/dec, respectively); the charge transfer resistance (Rct) was 15.14 Ω (FIG. 6), which was significantly less than NiO @ Ni and MoS 2 Rct values for-NiO @ Ni (32.17 and 23.17 Ω, respectively). And after the sample is subjected to long-time cycle experiments, graphene oxide is converted into graphene, but the HER performance stability is good. MoS was observed under simulated sun exposure 2 The HER performance of the-RGO-NiO @ Ni electrode is further improved, and the sample also has certain photocatalytic performance. MoS 2 The excellent HER performance of the-RGO-NiO @ Ni electrode is due to the MoS 2 The RGO-NiO is combined with a three-dimensional porous foam nickel substrate, has higher active specific surface area, can expose more active centers and improves the contact and diffusion of electrolyte ions. At the same time, high-activity MoS 2 The good distribution of the catalyst on the conductive graphene can effectively improve the charge transfer rate.
Drawings
FIG. 1 foam Ni, NiO @ Ni and MoS 2 XRD pattern of the-RGO-NiO @ Ni samples.
Figure 2 SEM image of the composite material.
Figure 3 HRTEM of composite material.
FIG. 4 Pt/C, foam Ni, NiO @ Ni, MoS 2 -NiO @ Ni and MoS 2 Comparative overpotential plot for the-G-NiO @ Ni samples.
FIG. 5 Pt/C, foam Ni, NiO @ Ni, MoS 2 -NiO @ Ni and MoS 2 Tafel slope comparison plot for the-G-NiO @ Ni samples.
FIG. 6 foam Ni, NiO @ Ni, MoS 2 -NiO @ Ni and MoS 2 Comparative plot of charge transfer resistance (Rct) for the-G-NiO @ Ni samples.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are provided only for illustrating the present invention and are not to be construed as limiting the present invention.
Example 1
(1) Under the condition of continuous stirring, dissolving dodecamolybdophosphoric acid, methylisothiourea and polysorbate in a weight ratio of 5:6:1 in 120mL of deionized water, transferring the mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal treatment at 180 ℃ for 24 hours, and obtaining MoS 2 Washing with deionized water, centrifuging, and vacuum drying. (2) RGO is prepared by treating natural graphite powder with a modified Hummer process. (3) Adding 18g of PEG4000 into 100mL of deionized water, heating to dissolve, and adding the MoS obtained in the step (1) 2 0.4g of RGO obtained in step (2) and 0.05g of RGO were sequentially dispersed in a PEG solution and sonicated for 30min to form a suspension sol. (4) And soaking the foamed nickel in a nitric acid solution with the concentration of 0.2M for 30min to obtain the pre-oxidized NiO @ Ni. (5) And (3) immersing the NiO @ Ni obtained in the step (4) into the suspension sol obtained in the step (3) for 2 min, then pulling at the speed of 1mm/s, and drying at the temperature of 60 ℃. The dipping, pulling and drying processes were repeated 4 times. (6) Putting the product obtained in the step (5) into a tubular furnace, heating to 400 ℃ at a heating rate of 3 ℃/mim under the protection of nitrogen, then switching to an atmosphere containing 3% of hydrogen and 97 nitrogen, preserving heat for 2h, and naturally cooling to room temperature to obtain the MoS with the required load capacity 2 -RGO-NiO @ Ni composite. (7) Performing a photoelectrocatalysis hydrogen evolution performance test on the composite material obtained in the step (6) under the irradiation of an electrochemical workstation and a xenon lamp, wherein the photoelectrocatalysis hydrogen evolution performance test is performed on the composite material in an alkaline electrolyte (1M KOH, the pH value is 13.7) and the current density is 10mA/cm 2 And then, obtaining data such as hydrogen evolution overpotential, Tafel slope value, charge transfer resistance (Rct), photoelectrocatalysis hydrogen production performance and the like.
Example 2
(1) Dissolving ammonium molybdate, thiourea and fatty acid glyceride in a weight ratio of 4:7:1 in 120mL of deionized water under continuous stirring, transferring the mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, performing hydrothermal treatment for 30 h at 160 ℃, and obtaining MoS 2 Washing with deionized water and centrifugingDrying in air for use. (2) RGO is prepared by treating natural graphite powder with a modified Hummer process. (3) Adding 16g PEG6000 into 100mL deionized water, heating to dissolve, and adding the MoS obtained in step (1) 2 0.3g of RGO obtained in step (2) and 0.06g of RGO were sequentially dispersed in a PEG solution and sonicated for 30min to form a suspension sol. (4) And soaking the foamed nickel in a hydrogen peroxide solution with the concentration of 0.8M for 50min to obtain the pre-oxidized NiO @ Ni. (5) And (3) immersing the NiO @ Ni obtained in the step (4) into the suspension sol obtained in the step (3) for 1 min, then pulling at the speed of 1mm/s, and drying at the temperature of 60 ℃. The dipping, pulling and drying processes were repeated 5 times. (6) Putting the product obtained in the step (5) into a tube furnace, heating to 300 ℃ at a heating rate of 4 ℃/mim under the protection of helium, then switching to an atmosphere containing 2% hydrogen and 98 helium, preserving the heat for 90min, and naturally cooling to room temperature to obtain the MoS with the required load capacity 2 -RGO-NiO @ Ni composite. (7) Performing a photoelectrocatalysis hydrogen evolution performance test on the composite material obtained in the step (6) under the irradiation of an electrochemical workstation and a xenon lamp, wherein the photoelectrocatalysis hydrogen evolution performance test is performed on the composite material in an alkaline electrolyte (1M KOH, the pH value is 13.7) and the current density is 10mA/cm 2 And then, obtaining data such as hydrogen evolution overpotential, Tafel slope value, charge transfer resistance (Rct), photoelectrocatalysis hydrogen production performance and the like.
Example 3
(1) Dissolving sodium molybdate, vinyl thiourea and fatty acid sorbitan in a weight ratio of 6:8:1 in 120mL of deionized water under continuous stirring, transferring the mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal treatment for 26 h at 170 ℃, and obtaining MoS 2 Washing with deionized water, centrifuging, and vacuum drying. (2) RGO is prepared by treating natural graphite powder with a modified Hummer process. (3) Adding 20g PEG2000 into 100mL deionized water, heating to dissolve, and adding MoS obtained in step (1) 2 0.5g of RGO obtained in step (2) and 0.07g of RGO were sequentially dispersed in a PEG solution and sonicated for 30min to form a suspension sol. (4) And soaking the foamed nickel in a potassium permanganate solution with the concentration of 0.5M for 40min to obtain the pre-oxidized NiO @ Ni. (5) Immersing the NiO @ Ni obtained in the step (4) into the suspended sol obtained in the step (3) for 3 min, and thenThen, the resultant was pulled at a rate of 1mm/s and dried at 60 ℃. The dipping, pulling and drying processes were repeated 5 times. (6) Putting the product obtained in the step (5) into a tubular furnace, heating to 500 ℃ at a heating rate of 5 ℃/mim under the protection of argon atmosphere, then switching to an argon atmosphere containing 5% of hydrogen and 95%, preserving heat for 3h, and naturally cooling to room temperature to obtain the MoS with the required load capacity 2 -RGO-NiO @ Ni composite. (7) Performing a photoelectrocatalysis hydrogen evolution performance test on the composite material obtained in the step (6) under the irradiation of an electrochemical workstation and a xenon lamp, wherein the photoelectrocatalysis hydrogen evolution performance test is performed on the composite material in an alkaline electrolyte (1M KOH, the pH value is 13.7) and the current density is 10mA/cm 2 And then, obtaining data such as hydrogen evolution overpotential, Tafel slope value, charge transfer resistance (Rct), photoelectrocatalysis hydrogen production performance and the like.
Claims (6)
1. MoS prepared by sol dip-coating method 2 A method for preparing a foam hydrogen evolution composite material of-RGO-NiO @ Ni, in particular to a method for pre-oxidizing foam nickel to obtain nickel-based nickel oxide and preparing MoS 2 The preparation method comprises the following steps of dispersing RGO in a PEG solution to obtain a suspension sol solution, carrying out multiple times of dipping, lifting and drying, carrying out temperature programming roasting under the atmosphere protection, carrying out heat preservation under a reducing atmosphere, and then naturally cooling to obtain the excellent hydrogen production composite material by photoelectrocatalysis water decomposition, and is characterized by comprising the following steps:
(1) dissolving a molybdenum compound, a sulfur compound and a nonionic surfactant in a weight ratio of (2-10): 4-12):1 in 120mL of deionized water under continuous stirring, transferring the mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal treatment at 140- 2 Washing with deionized water, centrifuging, and vacuum drying;
(2) RGO is prepared by processing natural graphite powder by an improved Hummer method;
(3) dissolving PEG surfactant in hot deionized water, and adding MoS obtained in step (1) 2 Dispersing the RGO obtained in the step (2) in a PEG solution, performing ultrasonic treatment for 30min to form stable suspension sol, wherein the mass ratio of three substances in 100mL of deionized water is W PEG :W MoS2 :W RGO =10:(0.1-1.0):(0.02-0.2)；
(4) Soaking the foamed nickel in a solution with the concentration of 0.2-1.0M and containing an oxidant for 20-50min to obtain pre-oxidized nickel foam (NiO @ Ni);
(5) immersing NiO @ Ni obtained in the step (4) into the suspension sol obtained in the step (3) for 1-4 min, then pulling at the speed of 1mm/s, and drying at the temperature of 60 ℃, and repeating the processes of immersing, pulling and drying for 3-8 times;
(6) placing the product obtained in the step (5) in a tubular furnace, performing temperature programming roasting to 300-600 ℃ under the atmosphere protection, switching to protective gas containing a certain reducing atmosphere, preserving heat for 1-3h, and naturally cooling to room temperature to obtain MoS with required load capacity 2 -RGO-NiO @ Ni composite.
2. MoS prepared by sol dip coating method according to claim 1 2 -RGO-NiO @ Ni method of foaming hydrogen evolving composite material, characterized in that: the molybdenum compound in the step (1) is one or a mixture of more of molybdenum acetylacetonate, molybdenum chloride, molybdenum trioxide, dodecamolybdophosphoric acid, ammonium phosphomolybdate and sodium phosphomolybdate; the sulfur compound is one or a mixture of more of thiourea, vinyl thiourea, methyl isothiourea and benzylthiourea; the nonionic surfactant is one or more of fatty glyceride, sorbitan fatty acid, polysorbate and polyoxyethylene.
3. MoS prepared by sol dip coating method according to claim 1 2 The method for preparing the-RGO-NiO @ Ni hydrogen evolution foam composite material comprises the step (3), wherein the PEG is one or a mixture of PEG1000, PEG1500, PEG2000, PEG4000, PEG6000 and PEG 8000.
4. MoS prepared by sol dip coating method according to claim 1 2 -RGO-NiO @ Ni foam hydrogen evolution composite material, step (4) the oxidizing agent is HNO 3 、H 2 SO 4 、KMnO 4 、H 2 O 2 、KClO 3 、KClO 4 One or more ofA mixture of (a).
5. MoS prepared by sol dip coating method according to claim 1 2 The RGO-NiO @ Ni foam hydrogen evolution composite material is prepared by the method, wherein the protective gas in the step (6) is one or a mixture of argon, helium, nitrogen and carbon dioxide; the reducing atmosphere is prepared by adding 0.5-5 vol% of H into protective gas 2 CO and SO 2 One or more of the above gases.
6. MoS obtainable by the preparation process according to any one of claims 1 to 5 2 the-RGO-NiO @ Ni foam hydrogen evolution composite material shows good performance of water hydrogen evolution by photoelectrocatalysis decomposition and catalytic stability by testing electrochemical performance and hydrogen production performance under the irradiation of an electrochemical workstation and a xenon lamp.
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