CN114890463A - Preparation method of stable perovskite micron crystal with good photocatalytic performance, product and application thereof - Google Patents
Preparation method of stable perovskite micron crystal with good photocatalytic performance, product and application thereof Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 44
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 49
- 239000013081 microcrystal Substances 0.000 claims abstract description 19
- 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
- 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
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000000137 annealing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000007146 photocatalysis Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 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
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000001228 spectrum Methods 0.000 description 10
- 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 9
- 150000005309 metal halides Chemical class 0.000 description 9
- 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 8
- 238000004020 luminiscence type Methods 0.000 description 6
- 239000002159 nanocrystal Substances 0.000 description 6
- 239000000463 material Substances 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
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000031700 light absorption 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
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000010200 validation analysis 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 a perovskite micron crystal which is stable and has good photocatalytic performance, a product and application thereof, belonging to the technical field of perovskite micron crystal preparation. The invention discloses a preparation method of perovskite micro-crystal with stability and good photocatalytic performance, which mainly uses cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl), titanium tetrachloride (TiCl) 4 ) Preparation of perovskite micron crystal (Cs) by using hydrogen bromide (HBr) and hydrogen chloride (HCl) as raw materials 2 TiCl 3 Br 3 ). The preparation method is simple, easy to operate, low in equipment requirement, low in cost and energy consumption, and suitable for expanded production. The perovskite micron crystal (Cs) prepared by the method is stable and has good photocatalytic performance 2 TiCl 3 Br 3 ) Has better photocatalytic performance and stability, and is in the field of photocatalysisShowing great application potential.
Description
Technical Field
The invention belongs to the technical field of perovskite micron crystal preparation, and relates to a preparation method of perovskite micron crystal which is stable and has good photocatalytic performance, and a product and application thereof.
Background
The original metal halide is CaTiO 3 Oxides of the cubic crystal system, discovered by the russian scientist perofski, and named after his last name, the metal halide is known under the english name Perovskite. The structure of the metal halide can be generally measured by a collotype silver chloride photographic method, and most of the metal halide is ABX 3 The cubic space group is formed into a cubic crystal form. Materials that resemble the crystal structure of metal halides are later referred to collectively as metal halides.
The lead halogenated 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 unfriendliness of lead element and its poor stability.
Therefore, in order to improve the side effect of lead element in the existing lead halogenated metal halide material, more and more researchers in recent years are interested in the research of lead-free metal halide nano material.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a perovskite microcrystalline with good stability and photocatalytic performance; the second purpose of the invention is to provide a perovskite micron crystal which is stable and has good photocatalytic performance; the invention also aims to provide application of the perovskite micron crystal which is stable and has good photocatalytic performance in the field of photocatalysis.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a preparation method of a perovskite microcrystal with stability and good photocatalytic performance comprises the following steps:
(1) cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) And cesium chloride (CsCl) is added to a solution containing titanium tetrachloride (TiCl) 4 ) Heating hydrogen bromide (HBr) and hydrogen chloride (HCl) in a sealed container to 100 deg.C in a glove box, and stirring to mix well;
(2) cooling the uniformly mixed mixture in the step (1) to room temperature, centrifuging to remove a precipitate obtained from the supernatant, and drying to form powder;
(3) annealing the powder in the step (2) to obtain the perovskite micron crystal Cs which is stable, luminous and flexible 2 TiCl 3 Br 3 。
Preferably, in the step (1), the cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl) and titanium tetrachloride (TiCl) 4 ) In a molar ratio of 5:3:5: 3.
Preferably, in the 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: ml.
Preferably, in the step (1), the stirring time is 10 hours or more.
Preferably, in the step (2), the rotation speed of the centrifugation is 9000-10000rpm, and the time is 5-10 min.
Preferably, in the step (2), the drying is carried out at 60-100 ℃ for 24-48 h.
Preferably, in the step (3), the annealing is carried out in an annealing instrument at 100-120 ℃ for 30-60 min.
2. The perovskite micron crystal Cs which is stable, luminous and flexible is prepared by the preparation method 2 TiCl 3 Br 3 。
3. The perovskite micron crystal Cs with stability and good photocatalytic 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 micro-crystal with stability and good photocatalytic performance, which mainly uses cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl), titanium tetrachloride (TiCl) 4 ) Preparation of perovskite micron crystal (Cs) by using hydrogen bromide (HBr) and hydrogen chloride (HCl) as raw materials 2 TiCl 3 Br 3 ). The preparation method is simple, easy to operate, low in equipment requirement, low in cost and energy consumption, and suitable for expanded production. The prepared product is stablePerovskite micron crystal (Cs) with fixed light and luminescence and flexible characteristic 2 TiCl 3 Br 3 ) Has better photocatalytic performance and good stability, and shows 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 objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 shows perovskite micro-crystals (Cs) with stable and flexible luminescence characteristics prepared in example 1 2 TiCl 3 Br 3 Microcrystalline) XRD pattern;
FIG. 2 shows the perovskite micro-crystals (Cs) with stable and flexible luminescence characteristics prepared in example 1 2 TiCl 3 Br 3 Micron crystal), wherein a is the total spectrum of the X-ray photoelectron spectrum, b is the spectrum of Cs element, c is the spectrum of Ti element, d is the spectrum of Cl element, and e is the spectrum of Br element;
FIG. 3 shows perovskite nanocrystals (Cs) with stable luminescence and flexible characteristics prepared in example 1 2 TiCl 3 Br 3 Micron crystal), wherein a is the ultraviolet-visible absorption spectrum and b is a Tauc plot;
FIG. 4 shows perovskite nanocrystals (Cs) with stable luminescence and flexible characteristics prepared in example 1 2 TiCl 3 Br 3 Micron crystal) under different conditions, wherein a is the XRD pattern of the Cs2TiCl3Br3 micron crystal (initial) which is just prepared and the Cs2TiCl3Br3 micron crystal which is irradiated for 3 h; b is Cs2TiCl3Br3 micron crystal (initial) as prepared, Cs2TiCl3Br3 micron crystal (heating at 100 deg.C for 120hours) after heat preservation at 100 deg.C, and 1 irradiation at 365nm ultraviolet lampXRD pattern of Cs2TiCl3Br3 micron crystal (exposure under 365nm UV light for 120hours) after 20 h;
FIG. 5 shows perovskite nanocrystals (Cs) with stable luminescence and flexible characteristics prepared in example 1 2 TiCl 3 Br 3 Microcrystals) where a is a CO yield plot and b is a CO yield line plot.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.
Example 1
Stable perovskite micron crystal (Cs) with good photocatalytic performance 2 TiCl 3 Br 3 Micron crystal), the XRD of which is shown in figure 1, and the specific preparation method comprises the following steps:
(1) cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) And cesium chloride (CsCl) is added to a solution containing titanium tetrachloride (TiCl) 4 ) Hydrogen bromide (HBr) and hydrogen chloride (HCl) (cesium bromide (CsBr), titanium tetrabromide (TiBr) among others 4 ) Cesium chloride (CsCl) and titanium tetrachloride (TiCl) 4 ) Heating to 100 ℃ in a glove box in a closed container with the molar ratio of 5:3:5:3), and stirring for 10 hours to uniformly mix;
(2) cooling the uniformly mixed mixture 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 the step (2) in an annealing instrument at 100 ℃ for 30min to obtain the perovskite micron crystal (Cs) with stability and good photocatalytic performance 2 TiCl 3 Br 3 Microcrystalline).
The perovskite micro crystal (Cs) with good photocatalytic performance and stability prepared in the example 1 2 TiCl 3 Br 3 Microcrystal) is detected by an X-ray photoelectron spectroscopy instrument (XPS) to obtain an X-ray photoelectron spectrum as shown in FIG. 2, wherein a is an X-ray photoelectron spectrum total spectrum, b is a Cs element spectrum, c is a Ti element spectrum, d is a Cl element spectrum, and e is a Br element spectrum. As can be seen from FIG. 2, the perovskite microcrystals (Cs) prepared in example 1, which are stable and have good photocatalytic properties 2 TiCl 3 Br 3 Micron crystal) contains three elements of Cs, Ti, Cl and Br.
The perovskite micro crystal (Cs) with good photocatalytic performance and stability prepared in the example 1 2 TiCl 3 Br 3 Microcrystals) were subjected to ultraviolet-visible absorption spectroscopy (Abs) analysis, and the results are shown in fig. 3, in which a is an ultraviolet-visible absorption spectrum and b is a Tauc plot. As can be seen from FIG. 3, Cs 2 TiCl 3 Br 3 The micron crystal has a wide light absorption range reaching 600nm, the valence band position of the material at 2.27eV accords with the photocatalytic band gap range, so the Cs can be indicated 2 TiCl 3 Br 3 The micron crystal has good photocatalytic performance.
The perovskite micro crystal (Cs) with good photocatalytic performance and stability prepared in the example 1 2 TiCl 3 Br 3 Micron crystal) after different conditions, as shown in fig. 4, wherein a is the comparison of XRD patterns of Cs2TiCl3Br3 micron crystal after Cs2TiCl3Br3 micron crystal is illuminated for 3h and Cs2TiCl3Br3 micron crystal which is just prepared; b is a comparison of XRD patterns of as-prepared Cs2TiCl3Br3 nanocrystals (initial), Cs2TiCl3Br3 nanocrystals after incubation for 120h at 100 ℃ (heating at 100 ℃ for 120hours), and Cs2TiCl3Br3 nanocrystals after 120h irradiation with a 365nm UV lamp (exposure under 365 UV light for 120 hours). As can be seen from FIG. 4, Cs produced in example 1 of the present invention 2 TiCl 3 Br 3 The microcrystals have good light, heat and air stability.
To is coming toBetter validation of the perovskite microcrystals (Cs) of the invention 2 TiCl 3 Br 3 Microcrystals) prepared in example 1, perovskite microcrystals (Cs) having stable, good photocatalytic properties prepared in example 1 were first tested 2 TiCl 3 Br 3 Micron crystal), the test method is as follows: 3mg of Cs 2 TiCl 3 Br 3 Adding the micrometer crystals into a test tube containing 1ml of toluene, and performing ultrasonication for 10min to obtain Cs 2 TiCl 3 Br 3 Dissolving the micron crystal powder in toluene solution completely, dropping the obtained solution on a glass sheet prepared in advance, drying the glass sheet at 60 deg.C on a drying table, dropping the solution to evaporate toluene and remove Cs 2 TiCl 3 Br 3 The micro-crystals remained on the glass plate, the above operation was repeated until the solution in the test tube was dropped off, and then the prepared sample was placed in a photocatalytic testing apparatus to perform a photocatalytic performance test for 3 hours, with the results shown in fig. 5, in which 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 reduced by the micron-sized crystal photocatalysis is quite considerable, the amount of 3h reduction is close to 9000, and the line graph shows that Cs is 2 TiCl 3 Br 3 The linearity of the microcrystalline reduced carbon dioxide is good.
In conclusion, the invention discloses a preparation method of perovskite micro-crystal with stability and good photocatalytic performance, which mainly uses cesium bromide (CsBr) and titanium tetrabromide (TiBr) 4 ) Cesium chloride (CsCl), titanium tetrachloride (TiCl) 4 ) Preparation of perovskite micron crystal (Cs) by using hydrogen bromide (HBr) and hydrogen chloride (HCl) as raw materials 2 TiCl 3 Br 3 ). The preparation method is simple, easy to operate, low in equipment requirement, low in cost and energy consumption, and suitable for expanded production. The perovskite micron crystal (Cs) prepared by the method is stable and has good photocatalytic performance 2 TiCl 3 Br 3 ) Has better photocatalytic performance and good stability, and shows great application potential in the field of photocatalysis.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (9)
1. A preparation method of perovskite micro-crystal with stability and good photocatalytic performance 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;
(2) cooling the uniformly mixed mixture in the step (1) to room temperature, centrifuging to remove a precipitate obtained from the supernatant, and drying to form powder;
(3) annealing the powder in the step (2) to obtain the perovskite micron crystal Cs which is stable, luminous and flexible 2 TiCl 3 Br 3 。
2. The production method according to claim 1, wherein in the step (1), the molar ratio of cesium bromide, titanium tetrabromide, cesium chloride and titanium tetrachloride is 5:3:5: 3.
3. The production method according to claim 1, wherein in the step (1), the molar volume ratio of titanium tetrachloride to hydrogen bromide to hydrogen chloride is 1.2:4:4, mmol: ml: ml.
4. The process according to claim 1, wherein the stirring is carried out for 10 hours or more in the step (1).
5. The method as claimed in claim 1, wherein in the step (2), the rotation speed of the centrifugation is 9000-10000rpm for 5-10 min.
6. The method according to claim 1, wherein in the step (2), the drying is performed at 60 ℃ to 100 ℃ for 24 to 48 hours.
7. The method according to claim 1, wherein in the step (3), the annealing is performed in an annealing apparatus at 100-120 ℃ for 30-60 min.
8. Stable, luminescent and flexible perovskite micron crystal Cs prepared by the preparation method according to any one of claims 1 to 7 2 TiCl 3 Br 3 。
9. The stable, good photocatalytic perovskite microcrystalline Cs of claim 8 2 TiCl 3 Br 3 Application in the field of photocatalysis.
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