CN109762562A - A kind of CsPbX3@TiO2Nano material and its preparation method and application - Google Patents
A kind of CsPbX3@TiO2Nano material and its preparation method and application Download PDFInfo
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Abstract
The present invention discloses a kind of CsPbX3@TiO2Nano material and its preparation method and application.First by CsX, PbX2It is dissolved in surfactant and n,N-Dimethylformamide solution system, is thermally formed CsPbX3Precursor solution；Then through sol-gel method in metatitanic acid salting liquid, in CsPbX3Surface hydrolysis coats TiOx, obtain CsPbX3@TiOx；It calcines under protection of argon gas, obtains CsPbX3@TiO2Nano material.The CsPbX that the present invention is obvious using " one kettle way " preparation structure, is evenly coated3@TiO2Nano material, and there is good fluorescent stability, material powder energy ambient-temp-stable placement 2 months or more, ultrasound was stablized 60 minutes or more in aqueous solution, can be widely applied to the multiple fields such as solar battery, photocatalysis, display device, laser, light detecting device and biological fluorescent labelling.
Description
Technical field
The present invention relates to nano material synthesis technical fields, and in particular to a kind of CsPbX3@TiO2Nano material and its preparation method
And application.
Background technique
The nanocrystalline CsPbX of full-inorganic perovskite3(X=Cl, Br, I), since its synthesis cost is low, and fluorescence efficiency is up to
90% or more, emit the advantages such as half-peak width and Wavelength tunable, solar battery, photocatalysis, display device, laser,
There is wide application value in the fields such as photodetector and biological fluorescent labelling, especially in solar cell application field, light
Photoelectric transformation efficiency is up to 20% or more.In general, the nanocrystalline preparation of perovskite using high warm injection method (Nano Lett.,
2015,15 (6), 3692-3696), on the one hand, its preparation condition is harsher, if you need to high temperature, heat injection etc., not only greatly increases
Synthesis cost, reduces materials synthesis efficiency, and polar solvent is added during purification, will cause perovskite nanometer
Brilliant aggregation, fluorescence efficiency drastically reduce.Meanwhile there are also problems for the large scale preparation of this method, when progress high-volume conjunction
Cheng Shi, nanocrystalline quality and monodispersity will substantially reduce.On the other hand, the stability of full-inorganic perovskite quantum dot is poor,
When encountering water, perovskite structure can be destroyed, and cause fluorescent quenching.In recent years, perovskite quantum how is efficiently synthesized
Point, and the stability problem in aqueous systems is solved, become its research hotspot applied in each field, in order to improve perovskite
The stability of quantum dot, a large amount of material and method are reported, such as the packet of aluminium oxide, silica, polymer these materials
It covers with certain limitation, never obtains effective solution.
TiO2It is nontoxic, inexpensive, photocatalytic activity is high due to stablizing with physicochemical properties and spectrochemical property, it can be
Normal temperature and pressure work, reaction times are more, and the duration is long, the advantages that being easy to get and the preferred material for becoming photochemical catalyst.
TiO2No doubt it has many good qualities, but there are also limitations.It most significantly, is that a kind of broad stopband that forbidden bandwidth is partly is led
Body, photocatalysis characteristic is only limited to ultraviolet band, and ultraviolet light only accounts for the sub-fraction of sunlight, this directly results in it and inhales to light
Receipts wave-length coverage is narrow, utilization rate is low.In addition, it there are also good electron transport abilities, and with less surface state and in
Between band defect.And calcium titanium ore bed stability is poor, cannot contact with aqueous solution, also limits the range of its application.
How full-inorganic perovskite nanocrystalline CsPbX is developed3@TiO2Nano material improves the report of its stability very
Few, the Weiwei Zheng etc. of Xue Cheng university, the U.S. reports a kind of CsPbX for having synthesized high water stability3@TiO2Nano material
(Adv.Funct.Mater.2017,1704288) synthesizes Cs-OA precursor solution by high temperature oil phase first, then exists
Hot injection method prepares CsPbBr at 170 DEG C3It is nanocrystalline.Then, in butyl titanate/toluene solution, titanium dioxide packet is carried out
It covers, is dried in vacuo to obtain CsPbBr3/TiOxCompound.Argon gas protects 300 DEG C to calcine 5 hours, obtains CsPbBr3/TiO2Composite Nano
Material.CsPbBr prepared by this method3/TiO2With good optical electro-chemistry activity, and in good stability.But its
It is nanocrystalline using high warm injection method to prepare perovskite, experimentation is cumbersome, and condition is relatively harsh, not only considerably increases conjunction
At cost, materials synthesis efficiency is reduced, and polar solvent is added during purification, it is nanocrystalline to will cause perovskite
Aggregation, fluorescence efficiency drastically reduce.Meanwhile there are also problems for the large scale preparation of this method, when carrying out high-volume synthesis,
Nanocrystalline quality and monodispersity will substantially reduce, and be unfavorable for industrialization.
Therefore, a kind of method being simple and efficient is invented to prepare the nanocrystalline CsPbX of high stability full-inorganic perovskite3@TiO2
Nano material can not only simplify operating process, save synthesis cost, improve the water stability of perovskite.Meanwhile to widen
The absorption region of titanium dioxide, in solar battery, photocatalysis, display device, laser, light detecting device and bioluminescence mark
The fields such as note have highly important application prospect.
Summary of the invention
Relative complex for the nanocrystalline preparation process conventional method of full-inorganic perovskite, water stability is poor and light is urged
Change material TiO2The problems such as using the absorption for being limited to ultraviolet light, the primary purpose of the present invention is that providing a kind of CsPbX3@TiO2
Nano material.
Another object of the present invention is to provide above-mentioned CsPbX3@TiO2The preparation method of nano material.
A further object of the present invention is to provide above-mentioned CsPbX3@TiO2Applications to nanostructures.
The present invention is directed to pass through the fusion nanocrystalline CsPbX of full-inorganic perovskite3With the mutual supplement with each other's advantages of titanium dioxide, one is provided
The method that kind is simple and efficient prepares high stability CsPbX3@TiO2Nano material can not only simplify operating process, save and close
At cost, the water stability of perovskite is improved.Meanwhile being the absorption region for widening titanium dioxide, it is expanded in solar-electricity
The fields such as pond, photocatalysis, display device, laser, light detecting device and biological fluorescent labelling application value.
The invention is realized by the following technical scheme:
A kind of CsPbX3@TiO2The preparation method of nano material, comprising the following steps:
(1)CsPbX3The preparation of precursor solution: it takes caesium halide and lead halide to mix first, it is living then to sequentially add surface
Property agent and n,N-Dimethylformamide, reaction is heated in argon atmosphere, that is, the limpid CsPbX of color is prepared3Presoma
Solution；
(2)CsPbX3@TiOxPreparation: take the CsPbX prepared in step (1)3Precursor solution, revolving speed be 500~
Be added in reaction dissolvent under 2000rpm stirring condition, metatitanic acid salting liquid is added after being stirred to react and keep revolving speed be 500~
By rotational speed regulation to 100~200rpm, the reaction was continued after 2000rpm, 5~100s, centrifuged described after reaction
CsPbX3@TiOx；
(3)CsPbX3@TiO2The preparation of nano material: the CsPbX that will be prepared in step (2)3@TiOxIt is dried in vacuum overnight,
It is then ground to powder, calcining obtains the CsPbX under protection of argon gas3@TiO2Nano material.
Preferably, the molal weight ratio of step (1) caesium halide and lead halide is 1:1.
Preferably, step (1) surfactant is the mixture of oleic acid and oleyl amine, and oleic acid: the volume ratio of oleyl amine is
1:2~2:1；It is furthermore preferred that oleic acid: the volume ratio of oleyl amine is 1:1.
Preferably, the mass ratio of the additional amount of surfactant and caesium halide is 5~10:1~5.
Preferably, the mass ratio of the additional amount of n,N-Dimethylformamide and caesium halide is 50~100:1~5.
Preferably, the temperature of step (1) described heating is 90-120 DEG C；It is furthermore preferred that the temperature of the heating is 100
℃。
Preferably, the time of step (1) described reaction is 2~4h；It is furthermore preferred that the time of the reaction is 3h.
Preferably, step (1) caesium halide is one or more of cesium chloride, cesium bromide and cesium iodide, institute
Stating lead halide is one or more of corresponding lead chloride, lead bromide and lead iodide.
Preferably, step (2) reaction dissolvent and CsPbX3The volume ratio of precursor solution is 50~250:1~5.
Preferably, the solvent of step (2) the metatitanic acid salting liquid is identical as the reaction dissolvent.
Preferably, step (2) the metatitanic acid salting liquid and CsPbX3The volume ratio of precursor solution is 5~20:1~5；
Preferably, the concentration of step (2) the metatitanic acid salting liquid is 5mg/mL~50mg/mL；It is furthermore preferred that the metatitanic acid
The concentration of salting liquid is 20mg/mL.
Preferably, the titanate in step (2) the metatitanic acid salting liquid is in butyl titanate, titanium chloride and titanium sulfate
It is one or more kinds of；More preferably butyl titanate.
Preferably, step (2) reaction dissolvent is one of n-hexane, toluene, hexamethylene, normal octane and normal heptane
Or it is two or more；It is furthermore preferred that the reaction dissolvent is n-hexane.
Preferably, the n-hexane have passed through water removal and be dried before being added.
Preferably, step (2) time being stirred to react is 15~30min；It is furthermore preferred that the friendship was stirred to react
Time is 20min.
Preferably, step (2) time that the reaction was continued is 2~4h, more preferably 3h.
Preferably, the revolving speed of step (2) described centrifugation is 2000~10000rpm.
Preferably, the time of step (2) described centrifugation is 5~30min.
Preferably, step (3) the vacuum drying temperature is 40~80 DEG C；More preferably 60 DEG C.
Preferably, the temperature of step (3) described calcining is 200~600 DEG C；More preferably 450 DEG C.
Preferably, the time of step (3) described calcining is 2~4h；More preferably 3h.
Above-mentioned CsPbX3@TiO2The CsPbX that the preparation method of nano material is prepared3@TiO2Nanocrystalline material.
Above-mentioned CsPbX3@TiO2Nano material is in solar battery, photocatalysis, display device, laser, light detecting device
With the application in biological fluorescent labelling.
Reaction mechanism of the invention are as follows: first by CsX (caesium halide), PbX2(lead halide) is added to oleic acid, oleyl amine and N,
In dinethylformamide solution system, heating reaction forms precursor solution；It is then cooled to which room temperature, takes appropriate presoma
Solution is added in reaction dissolvent, forms CsPbX3It is nanocrystalline, reaction a period of time, certain density metatitanic acid salting liquid is added,
By sol-gel method in CsPbX3Surface hydrolysis coats TiOx, CsPbX is obtained after centrifugation3@TiOxPrecipitating；By what is obtained
CsPbX3@TiOxPrecipitating is dried in vacuum overnight, grind into powder, under protection of argon gas high-temperature calcination, obtains CsPbX3@TiO2It receives
Rice material powder.
The CsPbX that the present invention is prepared3@TiO2Nano material, the CsPbX3(one of X=Cl, Br, I or
Mixed halide) it is that full-inorganic perovskite is nanocrystalline, having a size of 10~50nm, titanium dioxide is with a thickness of 5~100nm.
Compared with prior art, the invention has the following advantages and beneficial effects:
Operation of the present invention is simple, can prepare CsPbX using " one kettle way "3@TiO2Nano material is not necessarily in synthesis process
CsPbX is prepared in organic solution by elder generation3Nanocrystalline, then, centrifuge washing removes extra organic solvent, into row TiO again2
Cladding, the aggregation and fluorescent weakening for avoiding nano particle influence.Meanwhile simplifying experimentation, save the cost is conducive to realize
Batch production.CsPbX3@TiO2Nano material is obvious with structure, is evenly coated, prolonged fluorescent stability, the material powder
Last energy ambient-temp-stable placement 2 months or more, ultrasound was stablized 60 minutes or more in aqueous solution.The CsPbX3@TiO2Nano material can
It is widely used in a variety of necks such as solar battery, photocatalysis, display device, laser, light detecting device and biological fluorescent labelling
Domain.
Detailed description of the invention
Fig. 1 is CsPbX of the present invention3@TiO2The preparation process schematic diagram of nano material.
Fig. 2 is the CsPbBr of Ca-Ti ore type3CsPbBr made from nanocrystalline and embodiment 13@TiO2The transmission of nano material
Electromicroscopic photograph figure, wherein the CsPbBr of (a) corresponding Ca-Ti ore type3It is nanocrystalline, (b) corresponding CsPbBr3@TiO2Nano material.
Fig. 3 is the CsPbBr of Ca-Ti ore type3Nanocrystalline to be centrifuged with acetone precipitation, the relative fluorescence after being scattered in n-hexane is strong
Spend the change curve with washing times.
Fig. 4 is the CsPbBr of Ca-Ti ore type3CsPbBr made from nanocrystalline and embodiment 13@TiO2Nano material is in room temperature
Place the fluorescent stability test curve figure of different time.
Fig. 5 is the CsPbBr of Ca-Ti ore type3CsPbBr made from nanocrystalline and embodiment 13@TiO2Nano material is dispersed in
The relative intensity of fluorescence change curve of different ultrasonic times in water.
Specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in
This:
Embodiment 1
(1)CsPbBr3The preparation of precursor solution: weigh cesium bromide: lead bromide molal weight ratio is 0.5mmol:
0.5mmol, in 25mL three-necked flask, oleic acid is added: oleyl amine volume ratio is the mixture of 0.5mL:0.5mL, then, is added
10mL n,N-Dimethylformamide (DMF) is heated to 100 DEG C under protection of argon gas, reacts 3 hours, it is limpid that color can be obtained
CsPbBr3Precursor solution；
(2)CsPbBr3@TiOxPreparation: take the CsPbBr prepared in 0.3mL step (1)3Precursor solution is in revolving speed
It under 1200rpm, is added rapidly to be removed water in dry 10mL n-hexane, after stirring 15 minutes, dropwise addition 1mL concentration is 20mg/
The hexane solution of the butyl titanate of mL, revolving speed is recalled to 150rpm after 30s, by sol-gel method in CsPbBr3Surface
Hydrolysis cladding TiOx, continue to be stirred to react 2 hours, 5000rpm is centrifuged 10 minutes, obtains CsPbBr3@TiOxPrecipitating；
(3)CsPbBr3@TiO2The preparation of nano material: the full-inorganic calcium nanocrystalline Ti that will be prepared in step (2)
CsPbBr3@TiOxOvernight, grind into powder is protected high-temperature calcination 3 hours in 200 DEG C of argon gas, is obtained for 60 DEG C of precipitating vacuum drying
CsPbBr3@TiO2Nano material.
Embodiment 2
(1)CsPbCl3The preparation of precursor solution: weigh cesium chloride: lead chloride molal weight ratio is 1mmol:1mmol,
In 25mL three-necked flask, oleic acid is added: oleyl amine volume ratio is the mixture of 1.0mL:0.5mL, then, 10mL N, N- is added
Dimethylformamide (DMF) is heated to 100 DEG C under protection of argon gas, reacts 3 hours, the limpid CsPbCl of color can be obtained3
Precursor solution；
(2)CsPbCl3@TiOxPreparation: take the 0.5mL precursor solution prepared in step (1), be 1200rpm in revolving speed
Under, it is added rapidly to be removed water in dry 10mL n-hexane, after stirring 30 minutes, the tetrachloro that 1mL concentration is 40mg/mL is added dropwise
Change titanium/hexane solution, revolving speed is recalled to 150rpm after 30s, by sol-gel method in CsPbCl3Surface hydrolysis cladding
TiOx, continue to be stirred to react 3 hours, 5000rpm is centrifuged 20 minutes, obtains CsPbCl3@TiOxPrecipitating；
(3)CsPbCl3@TiO2The preparation of nano material: the CsPbCl that will be prepared in step (2)3@TiOxPrecipitating, vacuum are dry
Dry 60 DEG C overnight, and grind into powder is protected high-temperature calcination 4 hours in 350 DEG C of argon gas, obtains CsPbCl3@TiO2Nano material.
Embodiment 3
(1)CsPbI3The preparation of precursor solution: weigh cesium iodide: lead iodide molal weight ratio is 1mmol:1mmol, in
In 25mL three-necked flask, oleic acid is added: oleyl amine volume ratio is the mixture of 0.5mL:1mL, then, 10mLN, N- dimethyl is added
Formamide (DMF) is heated to 120 DEG C under protection of argon gas, reacts 2 hours, the limpid CsPbI of color can be obtained3Presoma
Solution；
(2)CsPbI3@TiOxPreparation: take the 0.4mL precursor solution prepared in step (1), be 1200rpm in revolving speed
Under, it is added rapidly to be removed water in dry 10mL toluene, after stirring 30 minutes, the metatitanic acid four that 1mL concentration is 50mg/mL is added dropwise
Butyl ester/toluene solution, revolving speed is recalled to 150rpm after 30s, by sol-gel method in CsPbI3Surface hydrolysis coats TiOx, after
Continuous to be stirred to react 3 hours, 5000rpm is centrifuged 10 minutes, obtains CsPbI3@TiOxPrecipitating；
(3)CsPbI3@TiO2Preparation: the nanocrystalline CsPbI of perovskite that will be prepared in step (2)3@TiOxPrecipitating, vacuum
Dry 80 DEG C overnight, and grind into powder is protected high-temperature calcination 4 hours in 400 DEG C of argon gas, obtains CsPbI3@TiO2Nano material powder
End.
The present invention using transmission electron microscope, Fluorescence Spectrometer respectively to prepared carry out morphology characterization and estimation of stability,
Its concrete outcome is as follows:
(1) morphology characterization
Fig. 1 is CsPbX of the present invention3@TiO2Preparation method schematic diagram.
Fig. 2 is the CsPbBr of Ca-Ti ore type3CsPbBr made from nanocrystalline and embodiment 13@TiO2The transmission of nano material
Electromicroscopic photograph figure, wherein the CsPbBr of (a) corresponding Ca-Ti ore type3It is nanocrystalline, (b) corresponding CsPbBr3@TiO2Nano material.By
Fig. 2 is it follows that CsPbBr3Nanocrystalline is cube structure, size about 20nm；CsPbBr3@TiO2Nano material has obvious
Core-shell structure, the thickness of titanium dioxide is about 15nm.
The CsPbBr of Ca-Ti ore type3Nanocrystalline preparation process is as follows: taking preparation in 1 step of 0.3mL example (1)
CsPbBr3Precursor solution is added rapidly to be removed water in dry 10mL n-hexane in the case where revolving speed is 1200rpm, stirring 15
After minute, the CsPbBr of Ca-Ti ore type can be obtained3Nanocrystal solution.The Ca-Ti ore type for taking 10 μ L to prepare with pipettor
CsPbBr3Nanocrystal solution drips to carbon and supports on film, after room temperature is dried, carries out transmissioning electric mirror test.
(2) estimation of stability
The CsPbBr for the Ca-Ti ore type for taking 5mL to be prepared3Nanocrystal solution be added 5mL acetone demulsification, in 5000rpm from
Heart 10min, remove supernatant, with 5mL n-hexane dispersion be precipitated as the first time wash, then repetitive operation 5mL acetone demulsification,
5000rpm centrifugation 10min, removal supernatant, the dispersion of 5mL n-hexane are precipitated as second of washing, repeat operation as third time
Washing.Initial CsPbBr is surveyed respectively3The fluorescence intensity of nanocrystal solution, and different washing times (for the first time, second, the
Opposite initial soln fluorescence intensity change three times), as a result as shown in Figure 3.By Fig. 3 it follows that with washing times increase
Fluorescence intensity gradually weakens (be initially 100%, after washing first time be 82%, be for the second time 58% and third time is 37%).
Therefore, experimentation can not only be simplified using " one kettle way ", save the cost, meanwhile, it can avoid because repeatedly washing bring fluorescence
Decrease problem.
The CsPbBr for the Ca-Ti ore type for taking 0.05g to be prepared3Powder that nanocrystal solution centrifugal drying obtains, 0.05g
The CsPbBr that 1 step of embodiment (3) is prepared3@TiO2Nano material powder is investigated place different time at 25 DEG C respectively
The fluorescence intensity change of (1,3,7,14,30,45 and 60 day).The result of investigation is as shown in figure 4, available by Fig. 4: perovskite
The CsPbBr of type3The decline of manocrystalline powders fluorescence is obvious, is quenched substantially after 30 days, relative intensity of fluorescence is only 6%；And
CsPbBr3@TiO2Nano material powder relative intensity of fluorescence in 60 days is basicly stable, maintains 90% or more.
The CsPbBr for the Ca-Ti ore type for taking 0.02g to be prepared3Manocrystalline powders and 0.02g CsPbBr3@TiO2Nanometer material
Feed powder end, both comparisons are distributed in 5mL deionized water respectively, (power 100W) ultrasound different time under ultrasound condition
Change in fluorescence situation after (1,5,10,15,20,30,45 and 60min), experimental result are as shown in Figure 5.Experiment shows with super
The extension of sound time, the CsPbBr of Ca-Ti ore type3The relative intensity of fluorescence of manocrystalline powders is quenched seriously, is only at 15 minutes
4%, it is quenched completely after twenty minutes；And CsPbBr3@TiO2Nano material powder fluorescent is relatively stable, stablizes in 60 minutes 90%
More than.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of CsPbX3@TiO2The preparation method of nano material, which comprises the following steps:
(1)CsPbX3The preparation of precursor solution: it takes caesium halide and lead halide to mix first, then sequentially adds surfactant
And n,N-Dimethylformamide, reaction is heated in argon atmosphere, that is, CsPbX is prepared3Precursor solution；
(2)CsPbX3@TiOxPreparation: take the CsPbX prepared in step (1)3Precursor solution, revolving speed be 500~
Be added in reaction dissolvent under 2000rpm stirring condition, metatitanic acid salting liquid is added after being stirred to react and keep revolving speed be 500~
By rotational speed regulation to 100~200rpm, the reaction was continued after 2000rpm, 5~100s, centrifuged described after reaction
CsPbX3@TiOx；
(3)CsPbX3@TiO2The preparation of nano material: the CsPbX that will be prepared in step (2)3@TiOxIt is dried in vacuum overnight, then
Grind into powder, calcining obtains the CsPbX under protection of argon gas3@TiO2Nano material.
2. CsPbX according to claim 13@TiO2The preparation method of nano material, which is characterized in that step (1) is described
The molal weight of caesium halide and lead halide ratio is 1:1；
Step (1) surfactant is the mixture of oleic acid and oleyl amine, and oleic acid: the volume ratio of oleyl amine is 1:2~2:1.
3. CsPbX according to claim 23@TiO2The preparation method of nano material, which is characterized in that step (1) is described
The additional amount of surfactant and the mass ratio of caesium halide are 5~10:1~5.
4. described in any item CsPbX according to claim 1~33@TiO2The preparation method of nano material, which is characterized in that step
Suddenly the mass ratio of the additional amount of (1) described n,N-Dimethylformamide and caesium halide is 50~100:1~5.
5. described in any item CsPbX according to claim 1~33@TiO2The preparation method of nano material, which is characterized in that step
Suddenly the temperature of (1) described heating is 90~120 DEG C；The time of step (1) described reaction is 2~4h.
6. described in any item CsPbX according to claim 1~33@TiO2The preparation method of nano material, which is characterized in that step
Suddenly (2) described reaction dissolvent and CsPbX3The volume ratio of precursor solution is 50~250:1~5；
Step (2) the metatitanic acid salting liquid and CsPbX3The volume ratio of precursor solution is 5~20:1~5；
The solvent of step (2) the metatitanic acid salting liquid is identical as the reaction dissolvent；
The concentration of step (2) the metatitanic acid salting liquid is 5mg/mL~50mg/mL.
7. described in any item CsPbX according to claim 1~33@TiO2The preparation method of nano material, which is characterized in that step
Suddenly (1) described caesium halide is one or more of cesium chloride, cesium bromide and cesium iodide, the lead halide be lead chloride,
One or more of lead bromide and lead iodide；
Titanate in step (2) the metatitanic acid salting liquid is one or both of butyl titanate, titanium chloride and titanium sulfate
More than；
Step (2) reaction dissolvent is one or more of n-hexane, toluene, hexamethylene, normal octane and normal heptane.
8. described in any item CsPbX according to claim 1~33@TiO2The preparation method of nano material, which is characterized in that step
Suddenly (2) described time being stirred to react is 15~30min；
Step (2) time that the reaction was continued is 2~4h；
The revolving speed of step (2) described centrifugation is 2000~10000rpm；
The time of step (2) described centrifugation is 5~30min；
Step (3) the vacuum drying temperature is 40~80 DEG C；
The temperature of step (3) described calcining is 200~600 DEG C；
The time of step (3) described calcining is 2~4h.
9. CsPbX according to any one of claims 1 to 83@TiO2The CsPbX that the preparation method of nano material is prepared3@
TiO2Nano material.
10. CsPbX as claimed in claim 93@TiO2Nano material solar battery, photocatalysis, display device, laser,
Application in light detecting device and biological fluorescent labelling.
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| CN115784301A (en) * | 2023-02-10 | 2023-03-14 | 武汉理工大学 | CsPbBr 3 @TiO 2 Core-shell heterojunction, preparation method and application thereof |
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| CN110743592A (en) * | 2019-10-25 | 2020-02-04 | 天津理工大学 | Perovskite photocatalyst and preparation method and application thereof |
| CN110743592B (en) * | 2019-10-25 | 2022-09-13 | 天津理工大学 | Perovskite photocatalyst and preparation method and application thereof |
| CN110975894B (en) * | 2019-12-18 | 2023-03-14 | 河南理工大学 | Visible light response type efficient and stable nano CsPbBr 3 /TiO 2 Composite photocatalyst and preparation method thereof |
| CN110975894A (en) * | 2019-12-18 | 2020-04-10 | 河南理工大学 | Visible light response type efficient and stable nano CsPbBr3/TiO2Composite photocatalyst and preparation method thereof |
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| CN112808282A (en) * | 2021-01-20 | 2021-05-18 | 河南大学 | Cesium-lead-bromine perovskite @ silicon dioxide hollow mesoporous spherical core-shell structure, and preparation method and application thereof |
| CN114163997A (en) * | 2021-12-06 | 2022-03-11 | 上海交通大学 | Semiconductor composite luminescent material, preparation method and luminescent device |
| CN114890463A (en) * | 2022-06-15 | 2022-08-12 | 重庆邮电大学 | Preparation method of stable perovskite micron crystal with good photocatalytic performance, product and application thereof |
| CN114890463B (en) * | 2022-06-15 | 2023-06-02 | 重庆邮电大学 | Preparation method of perovskite microcrystal with stability and good photocatalytic performance, product and application thereof |
| CN115784301A (en) * | 2023-02-10 | 2023-03-14 | 武汉理工大学 | CsPbBr 3 @TiO 2 Core-shell heterojunction, preparation method and application thereof |
| CN115784301B (en) * | 2023-02-10 | 2023-06-30 | 武汉理工大学 | CsPbBr 3 @TiO 2 Core-shell heterojunction, preparation method and application thereof |
| CN116515482A (en) * | 2023-04-21 | 2023-08-01 | 南昌航空大学 | CsPbX 3 /SnO 2 Preparation method and application of core/shell structure nanocomposite |
| CN116515482B (en) * | 2023-04-21 | 2024-03-26 | 南昌航空大学 | CsPbX 3 /SnO 2 Preparation method and application of core/shell structure nanocomposite |
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