CN114890463B - Preparation method of perovskite microcrystal with stability and good photocatalytic performance, product and application thereof - Google Patents
Preparation method of perovskite microcrystal with stability and good photocatalytic performance, product and application thereof Download PDFInfo
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- 239000013081 microcrystal Substances 0.000 title claims abstract description 61
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 49
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims abstract description 16
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims abstract description 16
- UBZYKBZMAMTNKW-UHFFFAOYSA-J titanium tetrabromide Chemical compound Br[Ti](Br)(Br)Br UBZYKBZMAMTNKW-UHFFFAOYSA-J 0.000 claims abstract description 16
- 238000007146 photocatalysis Methods 0.000 claims abstract description 15
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000009975 flexible effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 2
- 229910000042 hydrogen bromide Inorganic materials 0.000 claims 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims 2
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 229910001507 metal halide Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 150000005309 metal halides Chemical class 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 halide metal halide Chemical class 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/002—Compounds containing, besides titanium, two or more other elements, with the exception of oxygen or hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention relates to a preparation method of perovskite microcrystal with stability and good photocatalytic performance, a product and application thereof, and belongs to the technical field of perovskite microcrystal preparation. The invention discloses a preparation method of perovskite microcrystal with stable and good photocatalysis performance, which mainly uses cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl), titanium tetrachloride (TiCl) 4 ) Preparation of perovskite micro-crystals (Cs) by taking hydrogen bromide (HBr) and hydrogen chloride (HCl) as raw materials 2 TiCl 3 Br 3 ). The preparation method of the invention is simple, easy to operate, low in equipment requirement, low in cost and energy consumption, and suitable for expanded production. The perovskite microcrystal (Cs) with stable and good photocatalysis performance prepared by the invention 2 TiCl 3 Br 3 ) Has better photocatalytic performance and good stability, and has great application potential in the field of photocatalysis.
Description
Technical Field
The invention belongs to the technical field of perovskite microcrystal preparation, and relates to a preparation method of perovskite microcrystal with stability and good photocatalytic performance, a product and application thereof.
Background
The original metal halide is CaTiO 3 Belonging to the oxide of cubic crystal system, developed by Russian scientist PaveloskiNow, the name of the metal halide is Perovskite, which is named after the last name. The structure of the metal halides is generally measured by the silver chloride printing method of Kelvin Luo Ding, most of which are ABX 3 The cubic space group is in a cubic crystal form. Substances similar to the crystal structure of metal halides are hereinafter referred to collectively as metal halides.
The lead halide metal halide material is a novel inorganic functional material and has wide application prospect in the fields of photoelectric detection, light-emitting diodes, micro lasers and the like with excellent optical and electrical properties. But its application is limited due to the environmental unfriendly lead element and its poor stability.
Therefore, in order to improve the side effects of lead element in the existing lead halide metal halide materials, more and more students have been interested in the study of lead-free metal halide nanomaterials in recent years.
Disclosure of Invention
Accordingly, one of the objects of the present invention is to provide a method for preparing perovskite micro-crystals with stable and good photocatalytic performance; the second object of the present invention is to provide a perovskite micro crystal which is stable and has good photocatalytic performance; the third object of the invention is to provide a stable perovskite micro crystal with good photocatalysis performance, which is applied in the photocatalysis field.
In order to achieve the above purpose, the present invention provides the following technical solutions:
1. a method for preparing perovskite micro-crystals with stable and good photocatalysis performance, which comprises the following steps:
(1) Cesium bromide (CsBr), titanium tetrabromide (TiBr) 4 ) And cesium chloride (CsCl) are added to a catalyst containing titanium tetrachloride (TiCl) 4 ) Heating hydrogen bromide (HBr) and hydrogen chloride (HCl) in a closed container to 100 ℃ in a glove box, and stirring to uniformly mix the materials;
(2) Cooling the mixture uniformly mixed in the step (1) to room temperature, centrifuging to remove a precipitate obtained by supernatant fluid, and drying to form powder;
(3) Annealing the powder of step (2)The perovskite micro-crystal Cs with stable and luminous property and flexible characteristic can be obtained 2 TiCl 3 Br 3 。
Preferably, in step (1), the cesium bromide (CsBr) or titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl) and titanium tetrachloride (TiCl) 4 ) The molar ratio of (2) is 5:3:5:3.
Preferably, in step (1), the titanium tetrachloride (TiCl 4 ) The molar volume ratio of hydrogen bromide (HBr) to hydrogen chloride (HCl) was 1.2:4:4, mmol: ml.
Preferably, in step (1), the stirring time is 10 hours or more.
Preferably, in the step (2), the rotational speed of the centrifugation is 9000-10000rpm and the time is 5-10min.
Preferably, in step (2), the drying is at 60-100 ℃ for 24-48 hours.
Preferably, in the step (3), the annealing is performed in an annealing apparatus at 100-120 ℃ for 30-60min.
2. The perovskite micro-crystal Cs with stable and luminous property and flexible property prepared by the preparation method 2 TiCl 3 Br 3 。
3. The perovskite micro-crystal Cs with the stability and the good photocatalysis performance 2 TiCl 3 Br 3 Application in the field of photocatalysis.
The invention has the beneficial effects that: the invention discloses a preparation method of perovskite microcrystal with stable and good photocatalysis performance, which mainly uses cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl), titanium tetrachloride (TiCl) 4 ) Preparation of perovskite micro-crystals (Cs) by taking hydrogen bromide (HBr) and hydrogen chloride (HCl) as raw materials 2 TiCl 3 Br 3 ). The preparation method of the invention is simple, easy to operate, low in equipment requirement, low in cost and energy consumption, and suitable for expanded production. The perovskite microcrystal (Cs) with stable and luminous property and flexible characteristic prepared by the invention 2 TiCl 3 Br 3 ) Has better photocatalytic performance and good stability, and has great application potential in the field of photocatalysis。
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objects and other advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the specification.
Drawings
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in the following preferred detail with reference to the accompanying drawings, in which:
FIG. 1 is a graph showing the stable and luminescent perovskite micro-crystals (Cs) having flexibility characteristics prepared in example 1 2 TiCl 3 Br 3 Microcrystals);
FIG. 2 is a graph showing the stable and luminescent perovskite crystallites (Cs) having flexibility characteristics prepared in example 1 2 TiCl 3 Br 3 Microcrystal), wherein a is X-ray photoelectron spectrum total spectrum, b is Cs element spectrum, c is Ti element spectrum, d is Cl element spectrum, e is Br element spectrum;
FIG. 3 is a graph showing the stable and luminescent perovskite micro-crystals (Cs) having flexibility characteristics prepared in example 1 2 TiCl 3 Br 3 Microcrystal), wherein a is an ultraviolet-visible light absorption spectrum, and b is a Tauc plot curve;
FIG. 4 is a graph showing the stable and luminescent perovskite micro-crystals (Cs) having flexibility characteristics prepared in example 1 2 TiCl 3 Br 3 Microcrystals), wherein a is the XRD pattern of the freshly prepared Cs2TiCl3Br3 microcrystals (initial) and Cs2TiCl3Br3 microcrystals with 3h illumination; b is the XRD pattern of freshly prepared Cs2TiCl3Br3 micro-crystals (initial), cs2TiCl3Br3 micro-crystals after 120h of heat preservation at 100 ℃ and Cs2TiCl3Br3 micro-crystals after 120h of irradiation of 365nm ultraviolet lamp (exposure un der 365nm UV light for 120hours);
FIG. 5 is a perovskite micro-scale with flexible properties for stable luminescence prepared in example 1Rice crystal (Cs) 2 TiCl 3 Br 3 Microcrystals), where a is the CO yield plot and b is the CO yield plot.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be noted that the illustrations provided in the following embodiments merely illustrate the basic idea of the present invention by way of illustration, and the following embodiments and features in the embodiments may be combined with each other without conflict.
Example 1
Stable perovskite microcrystal (Cs) with good photocatalytic performance 2 TiCl 3 Br 3 Microcrystals) whose XRD is shown in fig. 1, a specific preparation method comprises the steps of:
(1) Cesium bromide (CsBr), titanium tetrabromide (TiBr) 4 ) And cesium chloride (CsCl) are added to a catalyst containing titanium tetrachloride (TiCl) 4 ) Hydrogen bromide (HBr) and hydrogen chloride (HCl) (wherein cesium bromide (CsBr), titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl) and titanium tetrachloride (TiCl) 4 ) In a molar ratio of 5:3:5:3), heating to 100 ℃ in a glove box, and stirring for 10 hours to uniformly mix the materials;
(2) Cooling the mixture uniformly mixed in the step (1) to room temperature, centrifuging at 10000rpm for 5min to remove supernatant to obtain precipitate, and drying at 80 ℃ for 24h to form powder;
(3) Treating the powder in step (2) in an annealing instrument at 100deg.C for 30min to obtain stable perovskite microcrystal (Cs) with good photocatalytic performance 2 TiCl 3 Br 3 Micro-crystals).
The stable perovskite microcrystals (Cs) with good photocatalytic performance prepared in example 1 were subjected to 2 TiCl 3 Br 3 The micrometer crystal) is detected by an X-ray photoelectron spectroscopy instrument (XPS), and X-ray photoelectron spectroscopy is shown in figure 2, wherein a is X-ray photoelectron spectroscopy total spectrum, b is Cs element spectroscopy, c is Ti element spectroscopy, d is Cl element spectroscopy, and e is Br element spectroscopy. As can be seen from FIG. 2, the stable perovskite microcrystals (Cs) with good photocatalytic performance prepared in example 1 2 TiCl 3 Br 3 Microcrystals) do contain Cs, ti, cl, br elements.
The stable perovskite microcrystals (Cs) with good photocatalytic performance prepared in example 1 were subjected to 2 TiCl 3 Br 3 Microcrystals) were subjected to ultraviolet-visible light absorption spectrum (Abs) analysis, the results of which are shown in fig. 3, where a is the ultraviolet-visible absorption spectrum and b is the Tauc plot. As can be seen from FIG. 3, cs 2 TiCl 3 Br 3 The micron crystal has a wider light absorption range reaching 600nm, and the valence band position of the material accords with the photocatalytic band gap range at 2.27eV, so the two points can indicate Cs 2 TiCl 3 Br 3 The microcrystal has good photocatalysis performance.
The stable perovskite microcrystals (Cs) with good photocatalytic performance prepared in example 1 were subjected to the following steps 2 TiCl 3 Br 3 Microcrystal) is subjected to X-ray powder diffraction tests under different conditions, as shown in fig. 4, wherein a is the comparison of XRD patterns of Cs2TiCl3Br3 microcrystal after 3 hours of illumination and the freshly prepared Cs2TiCl3Br3 microcrystal; b is a comparison of XRD patterns of freshly prepared Cs2TiCl3Br3 micro-crystals (initial), cs2TiCl3Br3 micro-crystals after 120h incubation at 100 ℃ C., for 120hours at 100 ℃ C., and Cs2TiCl3Br3 micro-crystals after 120h irradiation with 365nm ultraviolet lamp (exposure under 365nm UV light for 120hours). As can be seen from FIG. 4, cs prepared in example 1 of the present invention 2 TiCl 3 Br 3 The microcrystals have good light, heat and air stability.
To better verify the perovskite crystallites (Cs) of the present invention 2 TiCl 3 Br 3 Microcrystals), the stable perovskite micro-particles with good photocatalytic properties prepared in example 1 were tested firstRice crystal (Cs) 2 TiCl 3 Br 3 Microcrystals) and the test method is as follows: 3mg Cs 2 TiCl 3 Br 3 The microcrystals are added into a test tube filled with 1ml toluene and then subjected to ultrasonic treatment for 10min to make Cs 2 TiCl 3 Br 3 The microcrystalline powder is completely dissolved in toluene solution, and the resulting solution is then dropped onto a previously prepared glass sheet, the glass sheet is placed on a drying station and dried at 60℃, and the toluene is evaporated by dropping the solution to leave Cs at last 2 TiCl 3 Br 3 The microcrystals remained on the glass sheet, the above operation was repeated until the solution in the test tube was dropped, and then the prepared sample was put in a photocatalytic test instrument for 3 hours for photocatalytic performance test, and the results are shown in fig. 5, where a is a CO yield graph and b is a CO yield line graph. As can be seen from FIG. 5, cs 2 TiCl 3 Br 3 The amount of carbon dioxide by the photocatalytic reduction of the microcrystals is considerable, the reduction amount of 3 hours is close to 9000, and a line diagram shows Cs 2 TiCl 3 Br 3 The linearity of the reduction of carbon dioxide by the microcrystals is good.
In summary, the invention discloses a preparation method of perovskite microcrystal with stable and good photocatalysis performance, which mainly uses cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl), titanium tetrachloride (TiCl) 4 ) Preparation of perovskite micro-crystals (Cs) by taking hydrogen bromide (HBr) and hydrogen chloride (HCl) as raw materials 2 TiCl 3 Br 3 ). The preparation method of the invention is simple, easy to operate, low in equipment requirement, low in cost and energy consumption, and suitable for expanded production. The perovskite microcrystal (Cs) with stable and good photocatalysis performance prepared by the invention 2 TiCl 3 Br 3 ) Has better photocatalytic performance and good stability, and has great application potential in the field of photocatalysis.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the claims of the present invention.
Claims (7)
1. A preparation method of perovskite microcrystals with stability and good photocatalytic performance, which is characterized by comprising the following steps:
(1) Adding cesium bromide, titanium tetrabromide and cesium chloride into a closed container containing titanium tetrachloride, hydrogen bromide and hydrogen chloride, heating to 100 ℃ in a glove box, and stirring to uniformly mix the materials;
(2) Cooling the mixture uniformly mixed in the step (1) to room temperature, centrifuging to remove a precipitate obtained by supernatant fluid, and drying to form powder;
(3) Annealing the powder in the step (2) to obtain stable and luminous perovskite micro-crystal Cs with flexible characteristics 2 TiCl 3 Br 3 ；
In the step (1), the molar ratio of cesium bromide to titanium tetrabromide to cesium chloride to titanium tetrachloride is 5:3:5:3, and the molar volume ratio of titanium tetrachloride to hydrogen bromide to hydrogen chloride is 1.2:4:4, and mmol: mL.
2. The method according to claim 1, wherein in the step (1), the stirring time is 10 hours or longer.
3. The method according to claim 1, wherein in the step (2), the centrifugal rotation speed is 9000 to 10000rpm and the time is 5 to 10min.
4. The method according to claim 1, wherein in the step (2), the drying is performed at 60 ℃ to 100 ℃ for 24 to 48 hours.
5. The method according to claim 1, wherein in the step (3), the annealing is performed in an annealing apparatus at 100 ℃ to 120 ℃ for 30 to 60 minutes.
6. The perovskite micro-crystalline Cs with good photocatalytic performance and stable and prepared by the preparation method according to any one of claims 1-5 2 TiCl 3 Br 3 。
7. The stable, well-photocatalytic perovskite microcrystalline Cs of claim 6 2 TiCl 3 Br 3 Application in the field of photocatalysis.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012161716A (en) * | 2011-02-04 | 2012-08-30 | Sumitomo Chemical Co Ltd | Method for producing supported ruthenium oxide, and method for producing chlorine |
| WO2017110217A1 (en) * | 2015-12-22 | 2017-06-29 | 富士フイルム株式会社 | Photocatalyst electrode and artificial photosynthesis module |
| CN109762562A (en) * | 2019-02-20 | 2019-05-17 | 暨南大学 | A kind of CsPbX3@TiO2Nano material and its preparation method and application |
| CN113517364A (en) * | 2021-06-23 | 2021-10-19 | 上海应用技术大学 | Method for preparing lead-free double perovskite film by adopting printing method and application |
| CN113975946A (en) * | 2021-10-29 | 2022-01-28 | 重庆邮电大学 | Method for converting carbon dioxide by synergy of plasma and photocatalyst |
| CN114130410A (en) * | 2021-10-29 | 2022-03-04 | 盐城工学院 | Bismuth iron titanium oxyhalide photocatalytic material and preparation method and application thereof |
| CN114751447A (en) * | 2022-04-13 | 2022-07-15 | 滨州裕能化工有限公司 | Cs2TiBr6Method for preparing powder |
| CN115350716A (en) * | 2022-05-23 | 2022-11-18 | 重庆邮电大学 | Perovskite composite material photocatalyst and preparation method and application thereof |
-
2022
- 2022-06-15 CN CN202210678789.0A patent/CN114890463B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012161716A (en) * | 2011-02-04 | 2012-08-30 | Sumitomo Chemical Co Ltd | Method for producing supported ruthenium oxide, and method for producing chlorine |
| WO2017110217A1 (en) * | 2015-12-22 | 2017-06-29 | 富士フイルム株式会社 | Photocatalyst electrode and artificial photosynthesis module |
| CN109762562A (en) * | 2019-02-20 | 2019-05-17 | 暨南大学 | A kind of CsPbX3@TiO2Nano material and its preparation method and application |
| CN113517364A (en) * | 2021-06-23 | 2021-10-19 | 上海应用技术大学 | Method for preparing lead-free double perovskite film by adopting printing method and application |
| CN113975946A (en) * | 2021-10-29 | 2022-01-28 | 重庆邮电大学 | Method for converting carbon dioxide by synergy of plasma and photocatalyst |
| CN114130410A (en) * | 2021-10-29 | 2022-03-04 | 盐城工学院 | Bismuth iron titanium oxyhalide photocatalytic material and preparation method and application thereof |
| CN114751447A (en) * | 2022-04-13 | 2022-07-15 | 滨州裕能化工有限公司 | Cs2TiBr6Method for preparing powder |
| CN115350716A (en) * | 2022-05-23 | 2022-11-18 | 重庆邮电大学 | Perovskite composite material photocatalyst and preparation method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| A first-principles study on the optoelectronic properties of mixed-halide double perovskites Cs2TiI6-xBrx;Diwen Liu et al.;《New J. Chem.》;第44卷;第13613-13618页 * |
| A Review on Cs-Based Pb-Free Double Halide Perovskites: From Theoretical and Experimental Studies to Doping and Applications;Fatemeh Heidari Gourji et al.;《Molecules》;第26卷;第1-45页 * |
| Novelty All-Inorganic Titanium-Based Halide Perovskite for Highly Efficient Photocatalytic CO2 Conversion;Jinchen Zhou et al.;《small》;第1-8页 * |
| 全无机铯铅卤化物钙钛矿基光催化剂性能研究进展;张春艳等;《电子元件与材料》;第41卷(第6期);第560-573页 * |
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