CN117702284A - Method for preparing oxidized perovskite film based on metal oleate precursor - Google Patents
Method for preparing oxidized perovskite film based on metal oleate precursor Download PDFInfo
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- CN117702284A CN117702284A CN202311732232.1A CN202311732232A CN117702284A CN 117702284 A CN117702284 A CN 117702284A CN 202311732232 A CN202311732232 A CN 202311732232A CN 117702284 A CN117702284 A CN 117702284A
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- oleate
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- thin film
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- 229940049964 oleate Drugs 0.000 title claims abstract description 35
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 title claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 22
- 239000002184 metal Substances 0.000 title claims abstract description 22
- 239000002243 precursor Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 13
- -1 rare earth chloride Chemical class 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 235000019441 ethanol Nutrition 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 238000004528 spin coating Methods 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 21
- 239000010409 thin film Substances 0.000 claims description 15
- 229910021645 metal ion Inorganic materials 0.000 claims description 8
- 229910052765 Lutetium Inorganic materials 0.000 claims description 6
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 6
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 5
- 229940096992 potassium oleate Drugs 0.000 claims description 5
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 3
- 238000011403 purification operation Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 241000877463 Lanio Species 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002340 LaNiO3 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001814 protein method Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
-
- 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
- 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
- C30B29/22—Complex oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing an oxidized perovskite film based on a metal oleate precursor, which comprises the following steps of: taking 5mmol of rare earth chloride, 5mmol of rare earth element and 25mmol of oleate, adding 15ml of deionized water, 20ml of absolute ethyl alcohol and 35ml of normal hexane into a round-bottomed flask of 100ml, condensing and refluxing for 4 hours at 70 ℃, and then standing and naturally cooling to room temperature; pouring the upper reaction layer solution into a separating funnel, washing and purifying with a mixed solution of water and ethanol, and sealing and preserving the upper reaction layer solution at 4 ℃ for later use to obtain a reaction solution; taking 20-100 ml of the solution, and spin-coating the solution on a substrate under the parameters of 2000-5000 rpm and 20-50 s; placing the substrate spin-coated with the solution A in a tube furnace at a heating rate of 1-10 ℃/min, and naturally cooling after heating at 450-900 ℃ to obtain the oxidized perovskite film with smooth, compact and uniform surface. The invention is suitable for wide popularization and use.
Description
Technical Field
The invention belongs to the technical preparation field of metal oxide perovskite film materials, and mainly relates to an oxidized perovskite film with smooth, compact and uniform surface, large grain size and high crystallization quality, which is prepared by in-situ integration based on a metal oleate precursor.
Background
Currently, the search for efficient, stable, inexpensive, environmentally friendly energy conversion materials has become critical to alleviating the traditional energy crisis and solving environmental problems. Wherein, the oxidized perovskite material is generally expressed by ABX3 because of the unique crystal structure, the A site is alkaline earth or rare earth ion, the B site is transition metal ion, the X site is O2-ion, and three atoms form a cubic crystal system crystal structure. The crystal structure leads to the oxidation perovskite material having excellent chemical stability, unique semiconductor band gap and excellent spectral absorption characteristics, thereby having large-scale application in the fields of photocatalysis, fuel cells, chemical sensors, magnetic materials, wastewater treatment adsorbents, environmental remediation, energy conversion and the like. However, the perovskite prepared by the conventional method has small specific surface area, poor film quality and poor conductivity of part of perovskite at normal temperature, so that the catalytic activity and the like of the perovskite are limited.
The existing methods for preparing perovskite oxide include direct synthesis method, hydrothermal method, protein method, combustion method, coprecipitation method, nanoparticle method, sputtering method, pulse laser deposition method or sol-gel method. These methods generally require preferential preparation of oxidized perovskite powders, dissolution and dispersion of the material with a suitable solvent, spin coating of the dispersed solution, and high temperature calcination. However, the perovskite prepared by the traditional methods has small specific surface area, more crystal defects on the surface of the film, poor film quality and poor conductivity of part of perovskite at normal temperature, so that the catalytic activity of the perovskite is reduced, and further application of the film in various fields is limited.
Disclosure of Invention
In order to solve the technical problems, the invention adopts the basic conception of the technical scheme that:
a method for preparing an oxidized perovskite thin film based on a metal oleate precursor, comprising the following method steps:
s1: taking 5mmol of rare earth chloride, 5mmol of rare earth element and 25mmol of oleate, adding 15ml of deionized water, 20ml of absolute ethyl alcohol and 35ml of normal hexane into a round-bottomed flask of 100ml, condensing and refluxing for 4 hours at 70 ℃, and then standing and naturally cooling to room temperature;
s2: pouring the upper reaction layer solution into a separating funnel, washing and purifying for several times by using a mixed solution of water and ethanol, and sealing and preserving the upper reaction layer solution at 4 ℃ for later use to obtain a reaction solution A;
s3, taking 20-100 ml of the solution A, and spin-coating the solution on a substrate under the parameters of 2000-5000 rpm and 20-50S;
s4, placing the substrate spin-coated with the solution A in a tube furnace at a heating rate of 1-10 ℃/min, and naturally cooling the substrate after the heating temperature is 450-900 ℃, thereby obtaining the oxidized perovskite film with smooth, compact and uniform surface.
As a preferred embodiment of the present invention, the rare earth elements comprise yttrium, lutetium, and elements between yttrium atomic number and lutetium atomic number, and the rare earth chlorides include, but are not limited to, lacl3.6h O, feCl 3.6h2o, and the like.
In a preferred embodiment of the present invention, the metal element in the oleate contains any of Co, ni, fe, mn, cu and the like.
As a preferred embodiment of the present invention, the oleate contains metal ions and oleate ions inside, the molar ratio of the metal ions to oleate ions is 1:2 or 1:3, and the ratio varies according to the valence state of the metal ions.
As a preferred embodiment of the present invention, the oleate salts include, but are not limited to, sodium oleate, potassium oleate, and the like.
As a preferred embodiment of the invention, the volume ratio of water to ethanol during the purification operation is 1:10.
As a preferred embodiment of the present invention, the substrate includes, but is not limited to, FTO or ITO, a glass sheet, a quartz sheet, etc., and the substrate surface is coated with the solution a to form a thin film and then calcined at a high temperature.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method is simple and convenient, the operation is easy, and the prepared perovskite film is smooth, compact and uniform and can be controlled in thickness.
2. The surface of the prepared perovskite film is smooth, compact and uniform, the grain size is large, and the perovskite film has high crystallization quality.
3. The prepared perovskite film has better catalytic activity and degradation capability for dye.
4. The preparation method can reduce the interface defect density and improve the crystallinity and the grain size of perovskite crystals.
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
In the drawings:
FIG. 1 is a flow chart of a method for preparing an oxidized perovskite thin film based on a metal oleate precursor;
FIG. 2 is a schematic illustration of LaNiO prepared in preparing oxidized perovskite thin films based on metal oleate precursors 3 An XRD pattern of (b);
FIG. 3 is a LaNiO prepared in preparing an oxidized perovskite film based on a metal oleate precursor 3 SEM images of (a);
FIG. 4 is a LaNiO prepared in preparing an oxidized perovskite film based on a metal oleate precursor 3 XPS graph of (2);
FIG. 5 is a LaCoO prepared in preparing an oxidized perovskite film based on a metal oleate precursor 3 An XRD pattern of (b);
FIG. 6 is a LaCoO prepared in preparing an oxidized perovskite film based on a metal oleate precursor 3 SEM images of (a);
FIG. 7 is a LaCoO prepared in preparing an oxidized perovskite film based on a metal oleate precursor 3 Is a XPS graph of (C).
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and the following embodiments are used to illustrate the present invention.
Embodiment one:
as shown in fig. 1 to 4:
the preparation method of the LaNiO3 perovskite film comprises the following steps:
(1) The synthesis method of the La/Ni oleate precursor comprises the following steps:
5mmol of LaCl was weighed separately 3 ·6H 2 O (or 5mmol of La (NO) 3 ) 3 ·6H 2 O), 5mmol of NiCl 2 ·6H 2 O (or 5mmol Ni (NO) 3 ) 2 ·6H 2 O). Then 25mmol sodium oleate (or equimolar potassium oleate) and 15ml H are weighed 2 O, 20mL of absolute ethanol, 35mL of n-hexane are placed in a 100mL round bottom flask, and the mixture is condensed, refluxed and stirred for 4 hours at 70 ℃. After the reaction is finished, adding a water/ethanol mixed solution (volume ratio is 10:1), and repeatedly washing for a plurality of times until the lower layer solution is clarified. 1ml of the upper layer solution is taken for quantification, the molar concentration of the obtained product is calculated, and the upper layer solution is collected and stored in a sealed manner at 4 ℃.
(2) Preparation of LaNiO 3 Perovskite thin film:
0.5mmol of the upper layer solution is taken, and then 35mL of solution A is taken on a spin coater at 5000rpm for 30s to spin on an FTO substrate. Placing the FTO spin-coated with the upper layer solution in a tube furnace at a heating rate of 1 ℃/min, heating to 600 ℃ and preserving heat for 2 hours, and naturally cooling to obtain the perovskite film.
Embodiment two:
the difference from this embodiment based on the above embodiment is that:
as shown in figures 5 to 7 of the drawings,
(1) The synthesis method of the La/Co oleate precursor comprises the following steps:
5mmol of LaCl was weighed separately 3 ·6H 2 O (or 5mmol of La (NO) 3 ) 3 ·6H 2 O), weigh 5mmol of CoCl 2 ·6H 2 O (or 5mmol Co (NO) 3 ) 2 ·6H 2 O). Then 25mmol sodium oleate (or equimolar potassium oleate) and 15ml H are weighed 2 O, 20mL absolute ethanol, 35mL n-hexane in a 100mL round bottom flask. Condensing, refluxing and stirring at 70 ℃ for reaction for 4 hours. After the reaction is finished, adding a water/ethanol mixed solution (volume ratio is 10:1), and repeatedly washing for a plurality of times until the lower layer solution is clarified. 1ml of the upper layer solution is taken for quantification, the molar concentration of the obtained product is calculated, and the upper layer solution is collected and stored in a sealed manner at 4 ℃.
(2) Preparation of LaCoO 3 Perovskite thin film:
0.5mmol of the above upper layer solution was taken, and then 35mL of solution A was spin-coated onto the FTO on a spin coater at 5000rpm for 30 s. Placing the FTO spin-coated with the upper layer solution in a tube furnace at a heating rate of 1 ℃/min, and preserving the temperature at 600 ℃ for 2 hours to obtain the perovskite film.
Embodiment III:
the difference from this embodiment based on the above embodiment is that:
in this arrangement, the rare earth elements include yttrium, lutetium, and elements between yttrium atomic numbers and lutetium atomic numbers, and the rare earth chlorides include, but are not limited to, laCl3.6H O, feCl 3.6H2O, and the like.
In this embodiment, the metal element in the oleate contains any of Co, ni, fe, mn, cu and the like.
In the setting, the oleate contains metal ions and oleate ions, the molar ratio of the metal ions to the oleate ions is 1:2 or 1:3, and the ratio is changed according to the valence state of the metal ions.
In this arrangement, oleates include, but are not limited to, sodium oleate, potassium oleate, and the like.
In this setting, the volume ratio of water to ethanol was 1:10 during the purification operation.
In this arrangement, the substrate includes, but is not limited to, FTO or ITO, glass flakes, quartz flakes, etc., and the substrate surface is coated with solution a to form a thin film, which is then calcined at high temperature.
Claims (7)
1. A method for preparing an oxidized perovskite thin film based on a metal oleate precursor, comprising the following method steps:
s1: taking 5mmol of rare earth chloride, 5mmol of rare earth element and 25mmol of oleate, adding 15ml of deionized water, 20ml of absolute ethyl alcohol and 35ml of normal hexane into a round-bottomed flask of 100ml, condensing and refluxing for 4 hours at 70 ℃, and then standing and naturally cooling to room temperature;
s2: pouring the upper reaction layer solution into a separating funnel, washing and purifying for several times by using a mixed solution of water and ethanol, and sealing and preserving the upper reaction layer solution at 4 ℃ for later use to obtain a reaction solution A;
s3, taking 20-100 ml of the solution A, and spin-coating the solution on a substrate under the parameters of 2000-5000 rpm and 20-50S;
s4, placing the substrate spin-coated with the solution A in a tube furnace at a heating rate of 1-10 ℃/min, and naturally cooling the substrate after the heating temperature is 450-900 ℃, thereby obtaining the oxidized perovskite film with smooth, compact and uniform surface.
2. A method of preparing an oxidized perovskite thin film based on a metal oleate precursor according to claim 1 wherein the rare earth element comprises yttrium, lutetium and elements between yttrium atomic number and lutetium atomic number, the rare earth chlorides including but not limited to LaCl 3 ·6H 2 O、FeCl 3 ·6H 2 O, etc.
3. The method for preparing an oxidized perovskite thin film based on a metal oleate precursor according to claim 1, wherein the metal element in the oleate contains any one of Co, ni, fe, mn, cu and the like.
4. The method for preparing an oxidized perovskite thin film based on a metal oleate precursor according to claim 1, wherein the oleate contains metal ions and oleate ions in a molar ratio of 1:2 or 1:3, and the ratio varies according to the valence state of the metal ions.
5. A method of preparing an oxidized perovskite thin film based on a metal oleate precursor according to claim 1 wherein the oleate salt includes, but is not limited to, sodium oleate, potassium oleate, and the like.
6. The method of preparing an oxidized perovskite thin film based on metal oleate precursors according to claim 1, wherein the volume ratio of water and ethanol during the purification operation is 1:10.
7. A method of preparing an oxidized perovskite thin film based on a metal oleate precursor according to claim 1 wherein the substrate includes but is not limited to FTO or ITO, glass flakes, quartz flakes, etc., and the thin film is formed after the substrate surface is coated with solution a and calcined at high temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311732232.1A CN117702284A (en) | 2023-12-16 | 2023-12-16 | Method for preparing oxidized perovskite film based on metal oleate precursor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311732232.1A CN117702284A (en) | 2023-12-16 | 2023-12-16 | Method for preparing oxidized perovskite film based on metal oleate precursor |
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| Publication Number | Publication Date |
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| CN117702284A true CN117702284A (en) | 2024-03-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202311732232.1A Pending CN117702284A (en) | 2023-12-16 | 2023-12-16 | Method for preparing oxidized perovskite film based on metal oleate precursor |
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| Country | Link |
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- 2023-12-16 CN CN202311732232.1A patent/CN117702284A/en active Pending
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