CN115432740B - Preparation method of high-entropy oxide nanoparticle monolayer superlattice - Google Patents
Preparation method of high-entropy oxide nanoparticle monolayer superlattice Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 87
- 239000002356 single layer Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 83
- 229910052751 metal Inorganic materials 0.000 claims abstract description 57
- 239000002184 metal Substances 0.000 claims abstract description 56
- 239000002243 precursor Substances 0.000 claims abstract description 55
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 49
- 229940049964 oleate Drugs 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- 239000008367 deionised water Substances 0.000 claims description 36
- 229910021641 deionized water Inorganic materials 0.000 claims description 36
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 32
- 238000004108 freeze drying Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 16
- 239000012295 chemical reaction liquid Substances 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 239000010410 layer Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 16
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 11
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 10
- 238000011065 in-situ storage Methods 0.000 claims description 9
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims description 9
- 235000002597 Solanum melongena Nutrition 0.000 claims description 8
- 244000061458 Solanum melongena Species 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 239000012044 organic layer Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000010025 steaming Methods 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000011592 zinc chloride Substances 0.000 claims description 8
- 235000005074 zinc chloride Nutrition 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims description 5
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 229960001939 zinc chloride Drugs 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 229910000314 transition metal oxide Inorganic materials 0.000 abstract description 27
- 230000008569 process Effects 0.000 abstract description 5
- 150000002739 metals Chemical class 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 230000001808 coupling effect Effects 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- -1 iron cobalt manganese zinc cadmium Chemical compound 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- LJAOOBNHPFKCDR-UHFFFAOYSA-K chromium(3+) trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3] LJAOOBNHPFKCDR-UHFFFAOYSA-K 0.000 description 2
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910007570 Zn-Al Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to the technical field of inorganic materials, in particular to a preparation method of a high-entropy oxide nanoparticle monolayer superlattice. The method mainly aims at the problem that the high-entropy oxide nano-particle monolayer superlattice is limited by the number or the type of metal components in the process of preparing the high-entropy oxide nano-particle monolayer superlattice, and provides the following technical scheme: step one: preparing an inorganic salt template; step two: preparing a polybasic oleate precursor; step three: preparing inorganic salt coated high-entropy oxide nanoparticle superlattice; step four: preparation of high entropy oxide nanoparticle superlattice. The synthesis method is simple, the cost of raw materials is low, the mass preparation can be realized, the limitation of the number or the types of metal components is avoided, the method can be expanded to transition metal oxide nano particles with single-element to five-element different metal components, and the synergistic coupling effect between multiple metals is effectively exerted.
Description
Technical Field
The invention relates to the technical field of inorganic materials, in particular to a preparation method of a high-entropy oxide nanoparticle monolayer superlattice.
Background
Hydrogen is a new energy source for replacing traditional fossil fuel because of clean and renewable characteristics, and effectively solves the increasingly serious environmental problem caused by the excessive use of the traditional fossil fuel. The water electrolysis technology is a very environment-friendly hydrogen production technology which is currently known, and hydrogen and oxygen with high purity are obtained through hydrogen evolution and oxygen evolution reactions respectively occurring at a cathode and an anode. However, the overall kinetics process is slow due to the four proton coupling electron transfer process existing in the oxygen evolution reaction process, and the electrolysis efficiency is greatly limited. The known noble metal catalysts such as iridium dioxide and ruthenium dioxide can effectively reduce the overpotential required by the reaction, but the problems of low self-reserve, high cost, poor durability and the like prevent the noble metal catalysts from being applied to large scale in actual production. Therefore, the search for non-noble metal catalyst materials with low cost, high activity and high stability is the key point of current research.
Among non-noble metal catalysts, transition metal oxides are considered to be promising low-cost catalysts due to their low cost, abundant reserves, and the like, and have received extensive attention from researchers in recent years. Further research shows that the electronic structure of the metal can be optimized by introducing a plurality of different metal components to increase the diversity of the chemical composition of the catalyst, which is favorable for exerting the synergistic effect among multiple metals, effectively reducing the reaction energy barrier and improving the catalytic activity, and the catalyst is defined as a high-entropy compound when more than five metal elements exist in the system. On the other hand, the nano structure of the catalyst material can also have a great influence on the catalytic performance, the two-dimensional structure can effectively increase the specific surface area of the catalyst, the full exposure of active sites is facilitated, the mass transfer process in the catalytic reaction is greatly promoted, and the nano structure is often used as an important idea for the structural design of the catalyst. In view of this, we propose a method for preparing a high entropy oxide nanoparticle monolayer superlattice.
Disclosure of Invention
The invention aims to provide a preparation method of a high-entropy oxide nano-particle monolayer superlattice, aiming at the problem that the metal component number or the type of the high-entropy oxide nano-particle monolayer superlattice is limited in the preparation process of the high-entropy oxide nano-particle monolayer superlattice in the background art.
The technical scheme of the invention is as follows: the preparation method of the high-entropy oxide nanoparticle monolayer superlattice comprises the following specific steps:
step one: preparing an inorganic salt template; dissolving inorganic salt in deionized water, and stirring under ultrasound until inorganic salt crystals are completely dissolved to obtain a clear and transparent solution. The solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: preparing a polybasic oleate precursor; sequentially adding five metal salt precursors into the three-neck flask, and continuously adding a proper amount of deionized water to completely dissolve the metal salt; sequentially adding ethanol, sodium oleate and n-hexane, and reacting for 4 hours at a reflux state of 70 ℃; after the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding deionized water to remove unreacted metal salt precursor and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer water layer, repeating the operation for 3-5 times, transferring an upper organic layer to an eggplant type bottle, separating out a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is the polybasic oleate precursor;
step three: preparing inorganic salt coated high-entropy oxide nanoparticle superlattice; dissolving the polybasic oleate precursor obtained in the step two in normal hexane in a glass bottle to obtain brown polybasic oleate precursor solution, fully mixing the solution with the inorganic salt template obtained in the step one, and then calcining at a high temperature in a nitrogen atmosphere to enable the polybasic oleate precursor to be pyrolyzed in situ to form corresponding high-entropy oxide nano particles, thus obtaining the high-entropy oxide nano particle superlattice coated on the surface of the inorganic salt;
step four: preparing a superlattice of high-entropy oxide nano particles; and (3) dissolving the high-entropy oxide nanoparticle superlattice coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by using water washing, and repeating for 3 times to obtain the self-supporting single-layer high-entropy oxide nanoparticle superlattice.
Preferably, the inorganic salt in the first step is one or more of sodium chloride, potassium chloride and magnesium chloride.
Preferably, the mass ratio of the inorganic salt and deionized water in the first step is about 1:3.
Preferably, the five metal inorganic salt precursors in the second step are: ferric chloride hexahydrate, cobalt chloride hexahydrate, manganese chloride tetrahydrate, zinc chloride, aluminum chloride hexahydrate, ferric chloride hexahydrate, cobalt chloride hexahydrate, manganese chloride tetrahydrate, zinc chloride, aluminum chloride hexahydrate in a molar ratio of 1:1:1:1:1.
Preferably, in the second step, the volume ratio of deionized water, ethanol and n-hexane is 1:1:2.
Preferably, in the third step, the mass ratio of the polybasic oleate precursor to the inorganic salt template is 1:20.
Preferably, the high-temperature calcination temperature in the third step is 400 ℃, the calcination time is 120 minutes, and the temperature rising rate is 2 ℃/min.
Preferably, the five metal inorganic salt precursors specifically include the following components in parts by weight: 2.2-10.8g of ferric chloride hexahydrate, 0-4.7g of cobalt chloride hexahydrate, 0-2.6g of manganese chloride tetrahydrate, 0-1.36g of zinc chloride and 0-2.1g of aluminum chloride hexahydrate.
Compared with the prior art, the invention has the following beneficial technical effects:
1. according to the preparation method, the inorganic salt is used as a two-dimensional lamellar structure template, so that the precursor of the multi-element metal oleate is pyrolyzed into a single-layer high-entropy oxide nano-particle superlattice in situ in the inorganic salt template, and the high-entropy oxide nano-particles with different components and composition numbers can be obtained by changing the composition of the multi-element metal oleate; when the catalyst is used as a catalyst for the electrocatalytic oxygen evolution reaction, the synergistic effect among various different metals can be exerted due to the complexity of element composition, and the obviously improved catalytic activity is shown; meanwhile, a single-layer superlattice structure formed by high-entropy oxide nano particles is designed and synthesized, so that the specific surface area of the material can be effectively increased, the full exposure of surface active sites is facilitated, the collective effect different from that of single particles is exerted, and the reactivity and the stability are further obviously improved;
2. in the process of synthesizing the multielement metal oleate serving as a precursor for forming nano particles, the method is not limited by the number or types of metal components, can be expanded into transition metal oxide nano particles with single to five-membered different metal components, effectively exerts the synergistic coupling effect between the multiple metals, and in addition, the superlattice structure of the single-layer nano particles can effectively increase the specific surface area of the material, is beneficial to the full exposure of surface active sites, exerts the collective effect different from single particles, and shows the catalytic activity exceeding that of ruthenium dioxide serving as a commercial catalyst for the electrocatalytic oxygen evolution reaction;
3. in conclusion, the synthesis method is simple, the raw material cost is low, and mass preparation can be realized.
Drawings
FIG. 1 is a scanning electron microscope photograph of a superlattice of single-layer high-entropy oxide nanoparticles prepared in accordance with an embodiment of the invention;
FIG. 2 is a transmission electron micrograph of a superlattice of single-layer high-entropy oxide nanoparticles prepared in accordance with an embodiment of the invention;
FIG. 3 is a spectral plane scan of a superlattice of single-layer high-entropy oxide nanoparticles prepared in accordance with an embodiment of the invention;
FIG. 4 is a powder diffraction pattern of a superlattice of single-layer high-entropy oxide nanoparticles prepared in accordance with an embodiment of the invention;
FIG. 5 is a linear sweep voltammogram of a single layer high entropy oxide nanoparticle superlattice prepared in accordance with an embodiment of the invention;
fig. 6 is a constant voltage polarization curve of a single-layer high entropy oxide nanoparticle superlattice prepared in accordance with an embodiment of the invention.
Detailed Description
The technical scheme of the invention is further described below with reference to the attached drawings and specific embodiments.
Example 1
As shown in fig. 1-6, the preparation method of the high-entropy oxide nanoparticle single-layer superlattice provided by the invention comprises the following steps:
step one: 60g of inorganic salt is taken and dissolved in 200mL of deionized water, and the solution is stirred under ultrasonic until the inorganic salt crystals are completely dissolved, thus obtaining a clear and transparent solution. The solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: and (3) synthesizing Fe-Co-Mn-Zn-Al multi-element metal oleate. To a three-necked flask, 2.2g of ferric chloride hexahydrate, 1.9g of cobalt chloride hexahydrate, 1.6g of manganese chloride tetrahydrate, 1.1g of zinc chloride, 2.1g of chromium chloride hexahydrate were sequentially added, and 60mL of deionized water was further added to completely dissolve the metal salt. 60mL of ethanol, 36.5g of sodium oleate and 120mL of n-hexane were then added in this order and reacted at 70℃under reflux for 4 hours. After the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding a proper amount of deionized water to remove unreacted metal salt precursors and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer of water, repeating the operation for 3-5 times, transferring an upper layer of organic layer to an eggplant type bottle, separating a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is the polybasic oleate precursors;
step three: dissolving 2g of the polybasic oleate precursor obtained in the step II in 5mL of n-hexane in a glass bottle to obtain brown polybasic oleate precursor solution, fully mixing the solution with 20g of the inorganic salt template obtained in the step I, and calcining at 400 ℃ under nitrogen atmosphere to enable the polybasic oleate precursor to be subjected to in-situ pyrolysis to form corresponding high-entropy oxide nano particles, thus obtaining a superlattice of the high-entropy oxide nano particles coated on the surface of the inorganic salt;
step four: and (3) dissolving the high-entropy oxide nanoparticle superlattice coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by using water washing, and repeating for 3 times to obtain the self-supporting single-layer high-entropy oxide nanoparticle superlattice.
In this embodiment, as can be seen from fig. 1, the superlattice size of the obtained single-layer high-entropy oxide nanoparticle is about 2-5 μm;
as can be seen in conjunction with fig. 2, the particle size of the high entropy oxide nanoparticles is about 7nm;
as can be seen from fig. 3, the five elements of iron, cobalt, manganese, zinc, aluminum are uniformly distributed in the superlattice material of the single layer;
as can be seen from fig. 4, the crystallinity slightly decreases due to the introduction of the multi-elements, representing a mixed phase of five oxides;
the test was performed in 1m koh solution, and as can be seen from fig. 5, the catalyst had an overpotential of 290mV at a current density of 10, and the performance was significantly better than the commercial ruthenium dioxide catalyst;
as can be seen from fig. 6, after 20 hours of testing under constant voltage conditions, no significant decay of current occurred, demonstrating good cycling stability of the catalyst.
Example two
The invention provides a preparation method of a high-entropy oxide nanoparticle monolayer superlattice, which comprises the following steps:
step one: preparation of inorganic salt template: dissolving 60g of inorganic salt in 200mL of deionized water, and stirring under ultrasound until inorganic salt crystals are completely dissolved to obtain a clear and transparent solution; the solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: synthesis of monobasic metal oleate: 10.8g of ferric chloride hexahydrate is sequentially added into the three-necked flask, and 60mL of deionized water is added to completely dissolve the metal salt; then 60mL of ethanol, 36.5g of sodium oleate and 120mL of n-hexane are sequentially added, and the mixture is reacted for 4 hours at the reflux state of 70 ℃; after the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding a proper amount of deionized water to remove unreacted metal salt precursors and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer of water, repeating the operation for 3-5 times, transferring an upper organic layer to an eggplant type bottle, separating a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is a monobasic oleate precursor;
step three: preparation of inorganic salt coated unitary transition metal oxide nanoparticle superlattice: dissolving 2g of the monobasic metal oleate precursor obtained in the step II in 5mL of n-hexane in a glass bottle to obtain brown monobasic metal oleate precursor solution, fully mixing the solution with 20g of the inorganic salt template obtained in the step I, and calcining at 400 ℃ under nitrogen atmosphere to enable the monobasic metal oleate precursor to be pyrolyzed in situ to form corresponding monobasic transition metal oxide nano particles, thus obtaining a superlattice of the monobasic transition metal oxide nano particles coated on the surface of the inorganic salt;
step four: preparation of a superlattice of single-element transition metal oxide nanoparticles: and (3) dissolving the single-element transition metal oxide nanoparticle superlattice coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by using water washing, and repeating for 3 times to obtain the self-supporting single-layer single-element transition metal oxide nanoparticle superlattice.
Example III
The invention provides a preparation method of a high-entropy oxide nanoparticle monolayer superlattice, which comprises the following steps:
step one: preparation of inorganic salt template: dissolving 60g of inorganic salt in 200mL of deionized water, and stirring under ultrasound until inorganic salt crystals are completely dissolved to obtain a clear and transparent solution; the solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: synthesis of binary metal oleate: to a three-necked flask, 5.4g of ferric chloride hexahydrate and 4.7g of cobalt chloride hexahydrate were sequentially added, and 60mL of deionized water was added to completely dissolve the metal salts; then 60mL of ethanol, 36.5g of sodium oleate and 120mL of n-hexane are sequentially added, and the mixture is reacted for 4 hours at the reflux state of 70 ℃; after the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding a proper amount of deionized water to remove unreacted metal salt precursors and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer of water, repeating the operation for 3-5 times, transferring an upper layer of organic layer to an eggplant type bottle, separating a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is a binary oleate precursor;
step three: preparation of inorganic salt coated binary transition metal oxide nanoparticle superlattice: dissolving 2g of binary metal oleate precursor obtained in the step II in 5mL of normal hexane in a glass bottle to obtain brown binary metal oleate precursor solution, fully mixing the brown binary metal oleate precursor solution with 20g of inorganic salt template obtained in the step I, and calcining at 400 ℃ under nitrogen atmosphere to enable the binary metal oleate precursor to be subjected to in-situ pyrolysis to form corresponding binary transition metal oxide nano particles, thus obtaining binary transition metal oxide nano particle superlattice coated on the surface of inorganic salt;
step four: preparation of a superlattice of binary transition metal oxide nanoparticles: and (3) dissolving the binary transition metal oxide nanoparticle superlattice coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by using water washing, and repeating for 3 times to obtain the self-supporting single-layer binary transition metal oxide nanoparticle superlattice.
Example IV
The invention provides a preparation method of a high-entropy oxide nanoparticle monolayer superlattice, which comprises the following steps:
step one: preparation of inorganic salt template: dissolving 60g of inorganic salt in 200mL of deionized water, and stirring under ultrasound until inorganic salt crystals are completely dissolved to obtain a clear and transparent solution; the solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: synthesis of ternary metal oleate: to a three-necked flask, 3.6g of ferric chloride hexahydrate, 3.1g of cobalt chloride hexahydrate and 2.6g of manganese chloride tetrahydrate were sequentially added, and 60mL of deionized water was added to completely dissolve the metal salt; then 60mL of ethanol, 36.5g of sodium oleate and 120mL of n-hexane are sequentially added, and the mixture is reacted for 4 hours at the reflux state of 70 ℃; after the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding a proper amount of deionized water to remove unreacted metal salt precursor and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer of water, repeating the operation for 3-5 times, transferring an upper layer of organic layer to an eggplant type bottle, separating out a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is the ternary oleate precursor;
step three: preparation of inorganic salt coated ternary transition metal oxide nanoparticle superlattice: dissolving 2g of the ternary oleate precursor obtained in the step II in 5mL of n-hexane in a glass bottle to obtain brown ternary oleate precursor solution, fully mixing the brown ternary oleate precursor solution with 20g of the inorganic salt template obtained in the step I, and calcining at 400 ℃ under nitrogen atmosphere to enable the ternary oleate precursor to be pyrolyzed in situ to form corresponding ternary transition metal oxide nano particles, so that ternary transition metal oxide nano-particle superlattice coated on the surface of the inorganic salt can be obtained;
step four: preparation of a superlattice of ternary transition metal oxide nanoparticles: and (3) dissolving the ternary transition metal oxide nanoparticle superlattice coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by using water washing, and repeating for 3 times to obtain the self-supporting ternary transition metal oxide nanoparticle superlattice.
Example five
The invention provides a preparation method of a high-entropy oxide nanoparticle monolayer superlattice, which comprises the following steps:
step one: preparation of inorganic salt template: dissolving 60g of inorganic salt in 200mL of deionized water, and stirring under ultrasound until inorganic salt crystals are completely dissolved to obtain a clear and transparent solution; the solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: synthesis of quaternary metal oleate: to a three-necked flask, 2.7g of ferric chloride hexahydrate, 2.4g of cobalt chloride hexahydrate, 2.0g of manganese chloride tetrahydrate and 1.36g of zinc chloride were sequentially added, and 60mL of deionized water was added to completely dissolve the metal salt; then 60mL of ethanol, 36.5g of sodium oleate and 120mL of n-hexane are sequentially added, and the mixture is reacted for 4 hours at the reflux state of 70 ℃; after the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding a proper amount of deionized water to remove unreacted metal salt precursors and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer of water, repeating the operation for 3-5 times, transferring an upper layer of organic layer to an eggplant type bottle, separating a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is the quaternary oleate precursors;
step three: preparation of inorganic salt coated quaternary transition metal oxide nanoparticle superlattice: dissolving 2g of quaternary metal oleate precursor obtained in the second step in 5mL of normal hexane in a glass bottle to obtain brown quaternary metal oleate precursor solution, fully mixing the brown quaternary metal oleate precursor solution with 20g of inorganic salt template obtained in the first step, and calcining at 400 ℃ under nitrogen atmosphere to enable the quaternary metal oleate precursor to be pyrolyzed in situ to form corresponding quaternary transition metal oxide nano particles, thus obtaining quaternary transition metal oxide nano particle superlattice coated on the surface of inorganic salt;
step four: preparation of a quaternary transition metal oxide nanoparticle superlattice: and (3) dissolving the quaternary transition metal oxide nanoparticle superlattice coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by using water washing, and repeating for 3 times to obtain the self-supporting single-layer quaternary transition metal oxide nanoparticle superlattice.
Example six
The invention provides a preparation method of a high-entropy oxide nanoparticle monolayer superlattice, which comprises the following steps:
step one: preparation of inorganic salt template: dissolving 60g of inorganic salt in 200mL of deionized water, and stirring under ultrasound until inorganic salt crystals are completely dissolved to obtain a clear and transparent solution; the solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: synthesizing iron cobalt manganese zinc cadmium multielement metal oleate: to a three-necked flask, 2.2g of ferric chloride hexahydrate, 1.9g of cobalt chloride hexahydrate, 1.6g of manganese chloride tetrahydrate, 1.1g of zinc chloride, 2.1g of chromium chloride hexahydrate were sequentially added, and 60mL of deionized water was added to completely dissolve the metal salt; then 60mL of ethanol, 36.5g of sodium oleate and 120mL of n-hexane are sequentially added, and the mixture is reacted for 4 hours at the reflux state of 70 ℃; after the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding a proper amount of deionized water to remove unreacted metal salt precursors and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer water layer, repeating the operation for 3-5 times, transferring an upper layer organic layer to an eggplant type bottle, separating a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is the Fe-Co-Mn-Zn-Cd multi-element oleate precursor;
step three: preparation of inorganic salt coated iron-cobalt-manganese-zinc-cadmium oxide nanoparticle superlattice: dissolving 2g of the Fe-Co-Mn-Zn-Cd multi-metal oleic acid precursor obtained in the second step in 5mL of n-hexane to obtain brown Fe-Co-Mn-Zn-Cd multi-metal oleic acid precursor solution, fully mixing with 20g of the inorganic salt template obtained in the first step, and calcining at 400 ℃ under nitrogen atmosphere to enable the Fe-Co-Mn-Zn-Cd multi-metal oleic acid precursor to be subjected to in-situ pyrolysis to form corresponding Fe-Co-Mn-Zn-Cd oxide nano particles, thus obtaining Fe-Co-Mn-Zn-Cd oxide nano particle superlattice coated on the surface of the inorganic salt;
step four: preparing a superlattice of iron-cobalt-manganese-zinc oxide nano particles: and (3) dissolving the superlattice of the iron-cobalt-manganese-zinc-cadmium oxide nano particles coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by water washing, and repeating for 3 times to obtain the self-supporting superlattice of the single-layer iron-cobalt-manganese-zinc-cadmium oxide nano particles.
The above-described embodiments are merely a few preferred embodiments of the present invention, and many alternative modifications and combinations of the above-described embodiments will be apparent to those skilled in the art based on the technical solutions of the present invention and the related teachings of the above-described embodiments.
Claims (7)
1. The preparation method of the high-entropy oxide nanoparticle single-layer superlattice is characterized by comprising the following specific steps of:
step one: preparing an inorganic salt template; dissolving inorganic salt in deionized water, and stirring under ultrasound until inorganic salt crystals are completely dissolved to obtain a clear and transparent solution; the solution is placed in a liquid nitrogen barrel for quick freeze-drying, then is placed in a freeze dryer for further freeze-drying to remove residual moisture, and after the inorganic salt is converted into fluffy white powder from crystal particles, the fluffy white powder is taken out of a freeze drying box and is placed in a drying container for storage for standby;
step two: preparing a polybasic oleate precursor; sequentially adding five metal salt precursors into the three-neck flask, and continuously adding a proper amount of deionized water to completely dissolve the metal salt; sequentially adding ethanol, sodium oleate and n-hexane, and reacting for 4 hours at a reflux state of 70 ℃; after the reaction liquid is cooled to room temperature, transferring the reaction liquid to a separating funnel, adding deionized water to remove unreacted metal salt precursor and sodium oleate, shaking and mixing uniformly, standing and separating to remove a lower layer water layer, repeating the operation for 3-5 times, transferring an upper organic layer to an eggplant type bottle, separating out a low boiling point solvent by using a rotary steaming device, and drying overnight in a vacuum oven to obtain a brown viscous liquid which is the polybasic oleate precursor;
step three: preparing inorganic salt coated high-entropy oxide nanoparticle superlattice; dissolving the polybasic oleate precursor obtained in the step two in normal hexane in a glass bottle to obtain brown polybasic oleate precursor solution, fully mixing the solution with the inorganic salt template obtained in the step one, and then calcining at a high temperature in a nitrogen atmosphere to enable the polybasic oleate precursor to be pyrolyzed in situ to form corresponding high-entropy oxide nano particles, thus obtaining the high-entropy oxide nano particle superlattice coated on the surface of the inorganic salt;
step four: preparing a superlattice of high-entropy oxide nano particles; and (3) dissolving the high-entropy oxide nanoparticle superlattice coated on the surface of the inorganic salt obtained in the step (III) in deionized water, removing the inorganic salt template by using water washing, and repeating for 3 times to obtain the self-supporting single-layer high-entropy oxide nanoparticle superlattice.
2. The method for preparing a single-layer superlattice of high-entropy oxide nanoparticles according to claim 1, wherein the inorganic salt in the first step is one or more of sodium chloride, potassium chloride and magnesium chloride.
3. The method for preparing a single-layer superlattice of high-entropy oxide nanoparticles as defined in claim 1, wherein the mass ratio of inorganic salt to deionized water in the first step is 1:3.
4. The method for preparing a monolayer superlattice of high-entropy oxide nanoparticles as recited in claim 1, wherein the five metal inorganic salt precursors in the second step are: ferric chloride hexahydrate, cobalt chloride hexahydrate, manganese chloride tetrahydrate, zinc chloride, aluminum chloride hexahydrate, ferric chloride hexahydrate, cobalt chloride hexahydrate, manganese chloride tetrahydrate, zinc chloride, aluminum chloride hexahydrate in a molar ratio of 1:1:1:1:1.
5. The method for preparing a single-layer superlattice of high-entropy oxide nanoparticles according to claim 1, wherein in the second step, the volume ratio of deionized water, ethanol and n-hexane is 1:1:2.
6. The method for preparing a single-layer superlattice of high-entropy oxide nano particles according to claim 1, wherein the mass ratio of the polybasic oleate precursor to the inorganic salt template in the third step is 1:20.
7. The method for preparing a single-layer superlattice of high-entropy oxide nanoparticles according to claim 1, wherein the high-temperature calcination temperature in the third step is 400 ℃, the calcination time is 120 minutes, and the heating rate is 2 ℃/min.
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| CN114420953A (en) * | 2021-12-29 | 2022-04-29 | 浙江大学 | Preparation method of silver/high-entropy hydroxide oxide nano composite material |
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| WO2022160474A1 (en) * | 2021-01-28 | 2022-08-04 | 浙江大学 | Highly-conductive a-site high entropy nano metal oxide and preparation method therefor |
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