CN114369818A - Preparation method of metal compound nanosheet single crystal array film - Google Patents
Preparation method of metal compound nanosheet single crystal array film Download PDFInfo
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- CN114369818A CN114369818A CN202111538090.6A CN202111538090A CN114369818A CN 114369818 A CN114369818 A CN 114369818A CN 202111538090 A CN202111538090 A CN 202111538090A CN 114369818 A CN114369818 A CN 114369818A
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- single crystal
- metal
- crystal array
- array film
- metal compound
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 99
- 239000013078 crystal Substances 0.000 title claims abstract description 75
- 150000002736 metal compounds Chemical class 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 50
- 239000002184 metal Substances 0.000 claims abstract description 50
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000758 substrate Substances 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 15
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 150000004820 halides Chemical class 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052796 boron Inorganic materials 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 150000004767 nitrides Chemical class 0.000 claims abstract description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 8
- 239000011574 phosphorus Substances 0.000 claims abstract description 8
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 8
- 239000011593 sulfur Substances 0.000 claims abstract description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- -1 halide salts Chemical class 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 12
- 229910052736 halogen Inorganic materials 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 4
- 239000005922 Phosphane Substances 0.000 claims description 4
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 229910000085 borane Inorganic materials 0.000 claims description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 4
- 229910000064 phosphane Inorganic materials 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 3
- 229910052976 metal sulfide Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 230000008929 regeneration Effects 0.000 claims 1
- 238000011069 regeneration method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 17
- 238000003860 storage Methods 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 6
- 238000007789 sealing Methods 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 57
- 238000002441 X-ray diffraction Methods 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000000862 absorption spectrum Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 229940112669 cuprous oxide Drugs 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
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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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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/02—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/68—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous solutions with pH between 6 and 8
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention relates to the field of photoelectric conversion and storage, in particular to a preparation method of a metal compound nanosheet single crystal array film. Taking a metal substrate or a substrate with a metal coating deposited on the surface as a precursor, suspending the precursor above a mixed solution of ethylene glycol containing halide and water, sealing the precursor in a reaction kettle, putting the reaction kettle into an oven for heating treatment, taking out the substrate after cooling to room temperature, washing the substrate with deionized water and drying to obtain a metal oxide nanosheet single crystal array film supported by the substrate; and further carrying out heat treatment in an atmosphere of one or more of nitrogen, sulfur, phosphorus, carbon and boron elements to obtain the metal nitride, sulfide, phosphide, carbide and boride supported by the matrix and the metal compound nanosheet single crystal array film doped with different elements. Therefore, the method provides abundant material storage and a simple preparation method for constructing a high-efficiency photoelectric conversion and storage device based on the metal compound nanosheet single crystal array film.
Description
Technical Field
The invention relates to the field of photoelectric conversion and storage, in particular to a preparation method of a metal compound nanosheet single crystal array film.
Background
The two-dimensional material has unique physicochemical properties in the aspect of electronic structure (for example, the transition from indirect band gap to direct band gap and from metal to semiconductor), and also has unique characteristics in the aspects of optical absorption, carrier transmission, adsorption of molecules and ions and the like, and in addition, has structural advantages of high specific surface area, more reactive active sites and the like. These properties make the two-dimensional materials promising as active components for solar-driven photocatalytic systems. To this end, in addition to graphene, a number of two-dimensional materials have been used to construct various photocatalysts and photoelectrodes that significantly improve solar conversion efficiency and/or exhibit some unique characteristics. Meanwhile, the nano sheets vertically arranged have strong light collecting capacity and good appearance, and provide good conditions for further preparation of a heterostructure, so that the nano sheet has great application potential in the aspect of solar energy conversion. Meanwhile, the two-dimensional nano material has the property similar to that of graphene, has high efficiency and cycle performance for rechargeable lithium ion batteries, and the three-dimensional conductive substrate assembled by the two-dimensional structure has great advantages in the aspects of energy storage and sensors, so that the two-dimensional material has good application value and commercial value. However, the two-dimensional material (the two-dimensional material in the form of powder) growing on the substrate ex situ also has disadvantages, namely, a large amount of photogenerated carriers are compounded at the interface between the material and the substrate and the grain boundary between the material and the material, the time and the process cost of the experiment are increased, and thirdly, most of the synthesized nano sheets are modified on the surface of the electrode to be used as a photoelectrode or an electron transmission layer of a solar cell and are randomly oriented, so that the transmission of the photogenerated carriers is not facilitated, the large amount of the grain boundary is generated, the reduction of quantum efficiency (serious compounding) is caused, the photoelectrochemical activity of the material is greatly reduced, the photoelectric conversion efficiency is directly influenced, and the needs of subsequent industrialization and the commercial application are limited. Meanwhile, the two-dimensional material in the form of powder is difficult to recover from the aqueous solution after participating in the photocatalytic reaction, and secondary pollution is possibly caused. Currently, controllable synthesis preparation of two-dimensional materials is widely researched, and controllable preparation of substrate-supported metal compound nanosheet single crystal arrays is still challenging, and a simple method for batch preparation is lacked, so that how to grow metal oxide nanosheet single crystal array thin films on a substrate through a simple and universal method is very necessary in the fields of photoelectrochemistry, energy storage and sensors.
Disclosure of Invention
The invention aims to provide a preparation method of a metal compound nanosheet single crystal array film, which realizes in-situ growth of various metal compound nanosheet single crystal array film materials on a substrate and provides rich material storage and a simple preparation method for constructing a high-efficiency photoelectric conversion and storage device based on the metal compound nanosheet single crystal array film.
The technical scheme of the invention is as follows:
a preparation method of a metal compound nanosheet single crystal array film comprises the steps of taking a metal substrate or a substrate with a metal coating deposited on the surface as a precursor, suspending the precursor above a mixed solution of ethylene glycol containing halide and water, sealing the precursor in a reaction kettle, putting the reaction kettle into an oven for heating treatment, taking out the substrate after cooling to room temperature, washing with deionized water and drying to obtain a metal oxide nanosheet single crystal array film supported by the substrate; or further carrying out heat treatment in an atmosphere containing one or more of nitrogen, sulfur, phosphorus, carbon and boron elements to obtain the metal nitride, sulfide, phosphide, carbide and boride supported by the matrix and the metal compound nanosheet single crystal array film doped with different elements.
The precursor of the preparation method of the metal compound nanosheet single crystal array film is a metal or alloy substrate in various forms and a substrate with metal or alloy coatings deposited on various surfaces.
The preparation method of the metal compound nanosheet single crystal array film comprises the steps of adding a mixed solution of ethylene glycol and water containing halide, wherein the mass ratio of the water to the ethylene glycol is 0-0.5, the molar concentration of the halide is 1 mM-1000 mM, the halide comprises various halide salts or halogen acids, the halide salts are NaF, KF or NaCl, and the halogen acids are HF, HCl or HBr.
According to the preparation method of the metal compound nanosheet single crystal array film, the heating treatment temperature of the oven is 80-220 ℃, and the heating treatment time is 0.5-24 h.
According to the preparation method of the metal compound nanosheet single crystal array film, the atmosphere containing nitrogen, sulfur, phosphorus, carbon and boron elements is one or more of mixed gas of nitrogen, ammonia gas, hydrogen sulfide, methane, acetylene, carbon monoxide, carbon dioxide, sulfur dioxide, phosphane and borane gas.
The preparation method of the metal compound nanosheet single crystal array film has the advantages that the atmosphere heat treatment temperature is 150-1200 ℃, and the heat treatment time is 15 min-180 h.
According to the preparation method of the metal compound nanosheet single crystal array film, the thickness of a single metal compound nanosheet is 1 nm-200 nm, the length distribution range of the single metal compound nanosheet is 100 nm-5 microns, and the width distribution range of the single metal compound nanosheet is 100 nm-5 microns.
According to the preparation method of the metal compound nanosheet single crystal array film, the thickness distribution range of the metal compound nanosheet single crystal array film is 20 nm-10 microns.
The preparation method of the metal compound nanosheet single crystal array film comprises the step of preparing a metal compound from one or more than two of metal oxide, heterogeneous element doped metal oxide, metal nitride, metal sulfide, metal carbide, metal phosphide and metal boride.
According to the preparation method of the metal compound nanosheet single crystal array film, after the metal oxide nanosheet single crystal array film is obtained through atmosphere heat treatment, in the process of regenerating other metal compounds, the nanosheet is converted from nonporous to porous due to the difference of density, and the pore size distribution range of the nanosheet is 1 nm-100 nm.
The design idea of the invention is as follows:
for a chemical reaction, the reactions occur at solid-solid interface, solid-liquid interface, solid-gas interface, so that the properties and morphology of the final product of the substrate are greatly different. The gas-phase hydrothermal method is a new method for forming metal compound thin film nanostructures on a corresponding metal substrate, and the most obvious difference between the process and the liquid-phase hydrothermal process is that due to mass transport limitations in a thin liquid-phase reaction zone on the metal substrate, dissolution and structure formation are highly localized on the metal substrate. However, the conventional gas-phase hydrothermal method has a large saturated vapor pressure, so that the longitudinal etching rate of the halogen ions to the substrate is very high, the effect of the halogen ions as a morphology regulator cannot be shown, and the product mainly shows a one-dimensional characteristic structure. And a gas-phase solvothermal method is constructed by using high-boiling-point organic solvents such as ethylene glycol and the like, so that the saturated vapor pressure of the reaction can be effectively reduced, the etching rate of halogen to the substrate can be effectively reduced, and the possibility is provided for the halogen to be effectively adsorbed on certain crystal faces of the material, so that the growth of metal in the plane dimension of adsorbing halogen ions is limited, the growth is not limited in the etching dimension vertical to the metal substrate and the plane dimension without halogen adsorption, and a two-dimensional nanosheet structure can be obtained.
The invention has the advantages and beneficial effects that:
1. the invention relates to a preparation method of a metal compound nanosheet single crystal array film, which provides rich material storage and a simple preparation method for constructing a high-efficiency photoelectric conversion and storage device based on the metal compound nanosheet single crystal array film.
2. The invention adopts a synthesis method which is environment-friendly and simple in steps, and is beneficial to large-scale production.
3. The precursor adopted by the invention is a substrate with various metal (alloy) substrates or a substrate with metal (or alloy) coatings deposited on the surface, and has rich resources and easy storage, preparation and use.
Drawings
FIG. 1. the resulting TiO2The horizontal coordinate of the XRD pattern of the nano-sheet single crystal array film is diffraction angle 2 theta (degree), and the vertical coordinate is diffraction peak intensity (a.u.).
FIG. 2. the resulting TiO2Scanning Electron Microscope (SEM) picture of the nano-sheet single crystal array film.
FIG. 3. the resulting TiO2And (3) a cross-section SEM photo of the nano-sheet single crystal array film.
FIG. 4. the resulting TiO2The ultraviolet-visible absorption spectrum of the nanosheet single crystal array film has the abscissa representing the wavelength (nm) and the ordinate representing the absorption intensity (a.u.).
FIG. 5 shows the XRD spectrum of the porous TiN nano sheet single crystal array film, the abscissa is the diffraction angle 2 theta (degree), and the ordinate is the diffraction peak intensity (a.u.).
FIG. 6 is an SEM photograph of the porous TiN nano sheet single crystal array film.
FIG. 7. the resulting Cu2The horizontal coordinate of the XRD spectrum of the O nanosheet single crystal array film is diffraction angle 2 theta (degree), and the vertical coordinate of the XRD spectrum is diffraction peak intensity (a.u ℃).
FIG. 8. the resulting Cu2And (4) SEM (scanning electron microscope) picture of the O nano sheet single crystal array film.
FIG. 9. the resulting Cu2The X-ray-visible absorption spectrum of the O nanosheet single crystal array film has the abscissa representing the wavelength (nm) and the ordinate representing the absorption intensity (a.u.).
FIG. 10. WO obtained3The horizontal coordinate of the XRD pattern of the nano-sheet single crystal array film is diffraction angle 2 theta (degree), and the vertical coordinate is diffraction peak intensity (a.u.).
FIG. 11. WO obtained3SEM photograph of nano-sheet single crystal array film.
FIG. 12. WO obtained3And (3) a cross-section SEM photo of the nano-sheet single crystal array film.
Detailed Description
In the specific implementation process, a metal substrate (or a substrate with a metal coating deposited on the surface) is used as a precursor, the precursor is suspended above a mixed solution of ethylene glycol and water containing halide with a certain concentration, the mixed solution is sealed in a reaction kettle, the reaction kettle is placed in an oven for heating treatment for a certain time, the substrate is taken out after being cooled to room temperature, the substrate is cleaned by deionized water and dried to obtain a metal oxide nanosheet single crystal array film supported by the substrate, and further the substrate is subjected to heat treatment in an atmosphere containing elements such as nitrogen, sulfur, phosphorus, carbon, boron and the like to obtain metal nitride, sulfide, phosphide, carbide, boride and metal compound nanosheet single crystal array films doped with different elements and supported by the substrate. Wherein, specific characterized in that:
1. the precursor is a metal (or alloy) substrate with various forms and a substrate with various surface deposition metal (or alloy) coatings.
2. In the mixed solution of water and glycol, the mass ratio of water to glycol is 0-0.5, and the preferred mass ratio is 0-0.15.
3. In the glycol solution containing the halide with a certain concentration, the molar concentration of the halide is 1 mM-1000 mM, and preferably 40-350 mM.
4. The halide includes various halide salts (e.g., NaF, KF, NaCl, etc.) and hydrohalic acids (e.g., HF, HCl, HBr, etc.), with HF, HCl, and NaF being preferred.
5. The heating temperature of the oven is 80-220 ℃, preferably 120-180 ℃, and the heating time is 0.5-24 h, preferably 5-10 h.
6. The atmosphere containing nitrogen, sulfur, phosphorus, carbon, boron and other elements is one or a mixture of several of nitrogen, ammonia, hydrogen sulfide, methane, acetylene, carbon monoxide, carbon dioxide, sulfur dioxide, phosphane and borane gases, and preferably ammonia, hydrogen sulfide, methane, borane and phosphane.
7. The atmosphere treatment temperature is 150-1200 ℃, preferably 400-700 ℃, and the treatment time is 15 min-180 h, preferably 0.5-3.0 h.
8. The thickness of the single metal compound nano-sheet is 1 nm-200 nm, the length distribution range of the single nano-sheet is 100 nm-5 μm, preferably 200 nm-1 μm, and the width distribution range is 100 nm-5 μm, preferably 200 nm-1 μm.
9. The thickness distribution range of the nano-sheet single crystal array film is 20 nm-10 μm, preferably 200 nm-1 μm.
10. The metal compound comprises metal oxide, heterogeneous element doped metal oxide, metal nitride, metal sulfide, metal carbide, metal phosphide, metal boride and the composite compound.
11. In the process of generating other metal compounds after the metal oxide nanosheet single crystal array film is treated in the atmosphere, the nanosheets are converted from non-porous to porous due to density difference, and the pore size distribution range is 1 nm-100 nm, preferably 1 nm-20 nm.
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Example 1
A commercial metal titanium foil is adopted, 10mL of ethylene glycol is firstly measured, then 60mM of hydrofluoric acid is added, after uniform stirring, the solution is transferred into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, a sample holder is placed, and then the metal titanium foil is placed on the sample holder. Sealing the reaction kettle, putting the reaction kettle into an oven, heating for 7 hours at 150 ℃, taking out a reaction sample, cleaning the reaction sample by deionized water and ethanol, and drying the reaction sample by nitrogen to obtain TiO2A nano-sheet single crystal array film. As shown in FIG. 1, the resulting TiO2The XRD pattern of the nano-sheet single crystal array film only has characteristic peaks of metallic titanium and anatase titanium oxide. As shown in FIG. 2, the resulting TiO2SEM photograph of nano sheet monocrystal array film, nano sheet plane size 400nm and thickness 6 nm. As shown in FIG. 3, the resulting TiO2The cross section SEM photograph of the nano-sheet single crystal array film has the thickness of 0.5 mu m. As shown in FIG. 4, TiO2The ultraviolet-visible absorption spectrum of the nano-sheet single crystal array film has an absorption cut-off edge of 420 nm.
Example 2
With the use of a commercial metallic titanium foil,firstly, 10mL of ethylene glycol is measured, then 60mM of hydrofluoric acid is added, after uniform stirring, the solution is transferred into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, a sample support is placed, and then a metal titanium foil is placed on the sample support. Sealing the reaction kettle, putting the reaction kettle into an oven, heating for 7 hours at 150 ℃, taking out a reaction sample, cleaning the reaction sample by deionized water and ethanol, and drying the reaction sample by nitrogen to obtain TiO2A nano-sheet single crystal array film. And treating for 2 hours at 700 ℃ in ammonia atmosphere to obtain the porous TiN nano sheet monocrystal array film. As shown in FIG. 5, the XRD pattern of the obtained porous TiN nano sheet single crystal array film only has the characteristic peaks of metal titanium and titanium nitride, and the strong XRD diffraction peak shows that the film has very high crystallinity. As shown in FIG. 6, in the SEM photograph of the porous TiN nano sheet single crystal array film, the plane size of the nano sheet is 400nm, the thickness of the nano sheet is 6nm, the nano sheet is in a pore structure, and the pore size range is 1-10 nm.
Example 3
A commercial metal copper foil is adopted, 10mL of ethylene glycol is firstly measured, then 60mM of hydrofluoric acid is added, after uniform stirring, the solution is transferred into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, a sample holder is placed, and then the metal copper foil is placed on the sample holder. Sealing the reaction kettle, putting the reaction kettle into an oven, heating for 7 hours at 140 ℃, taking out a reaction sample, cleaning the reaction sample by using deionized water and ethanol, and drying the reaction sample by using nitrogen to obtain the Cu-Cu alloy2O nano-sheet single crystal array film. As shown in FIG. 7, the resulting Cu2An XRD (X-ray diffraction) spectrum of the O nanosheet single crystal array film only has characteristic peaks of metal copper and cuprous oxide. As shown in FIG. 8, the obtained Cu2An SEM photo of the O nano-sheet single crystal array film, wherein the plane size of the nano-sheet is 250nm, and the thickness of the nano-sheet is 5 nm. As shown in FIG. 9, Cu2The O nano sheet single crystal array film has ultraviolet-visible absorption spectrum, and the absorption edge extends to 600 nm.
Example 4
A commercial metal tungsten wire mesh is adopted, 10mL of ethylene glycol is firstly measured, then 60mM of hydrofluoric acid is added, after uniform stirring, the solution is transferred into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, a sample holder is placed, and then the metal tungsten wire mesh is placed on the sample holder. After the reaction kettle is sealedPutting the mixture into an oven for heating treatment at 180 ℃ for 7h, taking out a reaction sample, washing the reaction sample by using deionized water and ethanol, and drying the reaction sample by using nitrogen to obtain WO3A nano-sheet single crystal array film. WO obtained as shown in FIG. 103And (3) XRD (X-ray diffraction) pattern of the nano-sheet single crystal array film. WO obtained as shown in FIG. 113SEM photograph of nano sheet monocrystal array film, the size of the nano sheet is about 1 micron and the thickness is 80 nm. WO obtained as shown in FIG. 123The cross section SEM photograph of the nano-sheet single crystal array film has the thickness of 0.75 mu m.
The example results show that the metal oxide nanosheet single crystal array film supported by the substrate can be obtained by using a metal substrate (or a substrate with a metal coating deposited on the surface) as a precursor and performing heat treatment in an atmosphere generated by a mixed solution of ethylene glycol and water containing halide with a certain concentration, and further the metal nitride, sulfide, phosphide, carbide, boride and metal compound nanosheet single crystal array film doped with different elements supported by the substrate can be obtained by performing heat treatment in an atmosphere containing elements such as nitrogen, sulfur, phosphorus, carbon, boron and the like.
Claims (10)
1. A preparation method of a metal compound nanosheet single crystal array film is characterized in that a metal substrate or a substrate with a metal coating deposited on the surface is taken as a precursor, the precursor is suspended above a mixed solution of ethylene glycol containing halide and water, the mixed solution is sealed in a reaction kettle, the reaction kettle is placed in an oven for heating treatment, the substrate is taken out after being cooled to room temperature, and the substrate is washed by deionized water and dried to obtain a metal oxide nanosheet single crystal array film supported by the substrate; or further carrying out heat treatment in an atmosphere containing one or more of nitrogen, sulfur, phosphorus, carbon and boron elements to obtain the metal nitride, sulfide, phosphide, carbide and boride supported by the matrix and the metal compound nanosheet single crystal array film doped with different elements.
2. The method for preparing the metal compound nanosheet single crystal array film as defined in claim 1, wherein the precursor is a metal or alloy substrate of various forms and a substrate with various surface-deposited metal or alloy coatings.
3. The method for preparing a metal compound nanosheet single crystal array film according to claim 1, wherein in the mixed solution of ethylene glycol and water containing a halide, the mass ratio of water to ethylene glycol is 0-0.5, the molar concentration of the halide is 1 mM-1000 mM, the halide comprises various halide salts or halogen acids, the halide salts are NaF, KF or NaCl, and the halogen acids are HF, HCl or HBr.
4. The preparation method of the metal compound nanosheet single crystal array film as defined in claim 1, wherein the oven heat treatment temperature is 80-220 ℃ and the heat treatment time is 0.5-24 h.
5. The method for preparing a metal compound nanosheet single crystal array film according to claim 1, wherein the atmosphere containing nitrogen, sulfur, phosphorus, carbon and boron is one or a mixture of two or more of nitrogen, ammonia, hydrogen sulfide, methane, acetylene, carbon monoxide, carbon dioxide, sulfur dioxide, phosphane and borane.
6. The preparation method of the metal compound nanosheet single crystal array film as defined in claim 5, wherein the atmospheric heat treatment temperature is 150-1200 ℃ and the heat treatment time is 15 min-180 h.
7. The method for preparing a metal compound nanosheet single crystal array film according to claim 1, wherein the thickness of a single metal compound nanosheet is 1nm to 200nm, the length distribution range of the single metal compound nanosheet is 100nm to 5 μm, and the width distribution range is 100nm to 5 μm.
8. The method for preparing a metal compound nanosheet single crystal array film as defined in claim 1, wherein the thickness distribution of the metal compound nanosheet single crystal array film is within the range of 20nm to 10 μm.
9. A method for preparing a metal compound nanosheet single crystal array film as recited in claim 1, wherein the metal compound comprises one or more of a metal oxide, a heteroelement-doped metal oxide, a metal nitride, a metal sulfide, a metal carbide, a metal phosphide and a metal boride.
10. The preparation method of the metal compound nanosheet single crystal array film as defined in claim 1, wherein after the metal oxide nanosheet single crystal array film is obtained by atmospheric heat treatment, the nanosheets are converted from non-porous to porous due to density differences during regeneration of other metal compounds, and the range of pore size distribution is 1nm to 100 nm.
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