CN107381625B - A kind of preparation method that the water-soluble CsPbX3 perovskite of high stability is nanocrystalline - Google Patents
A kind of preparation method that the water-soluble CsPbX3 perovskite of high stability is nanocrystalline Download PDFInfo
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Abstract
A kind of water-soluble CsPbX of high stability of the invention3The nanocrystalline preparation method of perovskite belongs to the technical field of semiconductor nano material preparation.The invention firstly uses exchange of solvent methods soluble polymer particles are dispersed in hexane solvent be centrifuged to obtain again polymer microballoon precipitating, then will be dispersed in the CsPbX in toluene and hexane mixed solvent3Perovskite is nanocrystalline to be mixed 24 hours with the polymer microballoon precipitating, and the polymer particle of the nanocrystalline load of perovskite is obtained by centrifugation.The perovskite of Polymer-supported prepared by the present invention is nanocrystalline can not only to be dispersed in aqueous solution, the stability with higher under the conditions of different pH, by preparing different perovskite particles, fluorescence is obtained in visual field, the water soluble nanometer particles of high-efficiency fluorescence quantum efficiency, in bio-imaging, the fields such as display have huge application value.
Description
Technical field
The invention belongs to semiconductor nano material preparation technical fields, are related to a kind of water-soluble CsPbX of high stability3
The nanocrystalline synthetic method of (X=Cl, Br, I) perovskite.
Background technique
After semiconductor material is mutually gradually decrease to certain critical dimension (1~20 nanometer) from body, the fluctuation of carrier
Become significant, movement will be limited, and lead to the increase of kinetic energy, and corresponding electronic structure becomes quasi- point from the consecutive level structure of body
What is split is discontinuous, this phenomenon is referred to as quantum size effect.Relatively common semi-conductor nano particles, that is, quantum dot mainly has II-
VI, III-V and group IV-VI.The quantum dot of these types all very abides by quantum size effect, and property is presented with size and advised
The variation of rule property, such as absorption and launch wavelength change with change in size.Therefore, semiconductor nano illumination, display, swash
The fields such as light device and biological fluorescent labelling suffer from highly important application.
In recent years, the nanocrystalline especially halide perovskite of perovskite it is nanocrystalline because its brilliant charge transport properties with
And good chemical controllability, so that its is shown one's talent in the application of solar battery, LED, laser and photodetector, especially
It is in area of solar cell, photoelectric conversion efficiency can reach 20%.Currently, the nanocrystalline synthesis of perovskite focuses primarily upon
Organic-inorganic mixed type perovskite is nanocrystalline, and method substantially uses highly polar DMF or DMSO to go to prepare calcium as solvent
Titanium ore is nanocrystalline, and recently, pure inorganic halogen lead caesium perovskite is nanocrystalline to be prepared out for the first time, and Kovalenko group is using heat
Injection method has been successfully prepared the CsPbBr of 3.8~11.8nm3Perovskite nanometer blocks, and the nanocrystalline fluorescent quantum of its preparation
Efficiency can reach 90%.The perovskite that Xie group is not only successfully prepared small size with one-step method is nanocrystalline, but also can be
Room temperature prepares the nanocrystalline of single size.It obtains nanocrystalline brilliant with the assemble nanometer similar with single particle emission peak.Currently, not
Pipe is the synthesis of organic or inorganic perovskite nanometer, all uses organic phase preparation method.And the perovskite obtained is nanocrystalline
It must be dispersed in nonpolar solvent.It is current research shows that: a nanocrystalline distinguishing feature of perovskite is to polar reagent
It is very sensitive, such as acetone, methanol and ethyl alcohol even water can decompose perovskite.Even chloroform solvent, small size
It is nanocrystalline also unstable.Thus, solar battery is such as prepared in the subsequent application aspect of perovskite, stability is to face at present
Sixty-four dollar question especially prepares the one of the nanocrystalline preparation of water-soluble perovskite or perovskite Syntheses field
A challenge.
In conclusion the organic and inorganic perovskite prepared at present is nanocrystalline to have unstability, especially in polar solvent
Under the conditions of, it is nanocrystalline to decompose.The nanocrystalline stability of perovskite is improved, water-soluble calcium titanium ore technology is especially prepared and needs
Innovation.Therefore, freshly prepared water solubility CsPbX is established3The nanocrystalline method of (X=Cl, Br, I) perovskite, for perovskite nanometer
Brilliant and associated materials application field is of great significance to.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the problems, such as that background technique exists, provide and a kind of prepare high stability
Water-soluble CsPbX3The nanocrystalline new method of (X=Cl, Br, I) perovskite.
Technical problem of the invention solves by the following technical programs:
A kind of water-soluble CsPbX of high stability3The nanocrystalline preparation method of perovskite, will be water-soluble using exchange of solvent method
Property polymer microballoon be added in ethyl alcohol, ultrasound 30 minutes further dispersion obtain homogeneous phase solution, be then centrifuged, will be precipitated
Redisperse rear ultrasound 2 hours into hexane, then be centrifuged to obtain polymer microballoon precipitating；It then will be dispersed in toluene and hexane mixing
CsPbX in solvent3Perovskite is nanocrystalline to be mixed 24 hours with the polymer microballoon precipitating, obtains perovskite by centrifugation
The polymer particle of nanocrystalline load is finally dispersed to obtain water-soluble calcium titanium ore nanoparticle in aqueous solution；Wherein X is derived from
Cl, Br or I.
The polymer microballoon includes polyethylene, polyvinyl chloride, polypropylene, polystyrene, polymethyl methacrylate,
Acrylic nitrile-butadiene-styrene, polyamide or epoxy resin, for size between 0.1 to 10 microns, surface is that sulfonate radical is repaired
Decorations, it can be dispersed in aqueous solution, which can be bought by commercialization.
The CsPbX3Preferably 4~12 nanometers of the nanocrystalline size of perovskite.
Preferred 1:1~20 of the volume ratio of toluene and hexane in the toluene and hexane mixed solvent.
The CsPbX3The nanocrystalline preparation of perovskite belongs to the prior art, prepares CsPbX using one-step method3(X=
Cl, Br, I) perovskite is nanocrystalline, and by regulating and controlling nanocrystalline size and composition, preparation launch wavelength is received at 400-700 nanometers
Meter Jing, nanocrystalline size range are 4-12 nanometers.
Core of the invention is to be mixed by the way of gradually exchange of solvent by hydrophobic nanocrystalline and polymer particle
It closes, the nanocrystalline mode gradually spread of hydrophobic perovskite enters polymer microballoon, to obtain water-soluble calcium titanium ore nanometer
Particle, specific experiment mechanism are as shown in Figure 1.
This new synthetic method proposed by the invention, finally by the CsPbX of synthesis3(X=Cl, Br, I) perovskite
It is nanocrystalline to be dispersed in water, it absorbs and entire visible range is covered in transmitting.
The utility model has the advantages that
1, water solubility CsPbX prepared by the present invention3Perovskite is nanocrystalline sufficiently stable, is dispersed in polar solvent water,
And pH quantum dot fluorescence intensity in 1 to 14 ranges does not change.
2, operation of the present invention is simply adjustable, by regulating and controlling nanocrystalline size and composition, can get different fluorescence emission wavelengths
Water-solubility nanocrystalline.
Detailed description of the invention:
Fig. 1 is that the present invention prepares the nanocrystalline mechanism choice of water-soluble calcium titanium ore.
Fig. 2 is the nanocrystalline photo in the UV lamp of water-soluble calcium titanium ore of polystyrene microsphere cladding.
Fig. 3 is the nanocrystalline fluorescence spectrum changed over time under the conditions of 1 pH of water-soluble calcium titanium ore.
Fig. 4 is the nanocrystalline fluorescence spectrum changed over time under the conditions of 7 pH of water-soluble calcium titanium ore.
Fig. 5 is the nanocrystalline fluorescence spectrum changed over time under the conditions of 14 pH of water-soluble calcium titanium ore.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing.
Wherein the attached figures are only used for illustrative purposes and cannot be understood as limitating the patent.
Embodiment 1:
Firstly, 10mL ethyl alcohol is added in 0.01g (1mL) water-soluble polystyrene microsphere (size is at 0.1~10 micron)
In, further disperse to obtain homogeneous phase solution within ultrasound 30 minutes, be then centrifuged, ultrasound after precipitating is re-dispersed into hexane
2 hours, solution is centrifuged again to obtain polystyrene microsphere precipitating.
Then by the 5mL CsPbBr of preparation3(perovskite containing 0.001mmol is nanocrystalline, diameter for perovskite nanocrystal solution
In 4~12nm, solvent is the toluene and ethane of volume ratio 1:10) it is added in precipitate of polystyrene, then ultrasound 1 hour is stirred
It mixes 24 hours.Solution is centrifuged to obtain perovskite and polystyrene compound particle.It is molten that the particle of acquisition is re-dispersed into hexane
In liquid, by precipitating, redisperse obtains perovskite supported polystyrene particle into hexane.Finally again by the product of preparation
It is distributed in water, it is nanocrystalline to obtain water-soluble perovskite.The experiment mechanism choice of specific experiment process as shown in Figure 1.
Embodiment 2:
Firstly, 10mL ethyl alcohol is added in 0.01g (1mL) water-soluble polystyrene microsphere (size is at 0.1~10 micron)
In, further disperse to obtain homogeneous phase solution within ultrasound 30 minutes, be then centrifuged, ultrasound after precipitating is re-dispersed into hexane
2 hours.Solution is centrifuged again to obtain polystyrene microsphere precipitating.
Then by the 5mL CsPbBr of preparation3(perovskite containing 0.002mmol is nanocrystalline, diameter for perovskite nanocrystal solution
In 4~12nm, solvent is the toluene and ethane of volume ratio 1:4) it is added in precipitate of polystyrene, then ultrasound 1 hour stirs
24 hours.Finally solution is centrifuged to obtain perovskite and polystyrene compound particle.It is molten that the grain of acquisition is re-dispersed into hexane
In liquid, by precipitating, redisperse obtains perovskite supported polystyrene particle into hexane.Finally again by the product of preparation
It is distributed in water, obtains that water-soluble perovskite is nanocrystalline, and fluorescence photo is shown in Fig. 2.The reality of specific experiment process as shown in Figure 1
Test mechanism choice.
Embodiment 3:
Firstly, 0.02g (1mL) water-soluble poly (methyl methacrylate) micro-sphere (size is at 0.1~10 micron) is added
In 10mL ethyl alcohol, further disperses to obtain homogeneous phase solution within ultrasound 30 minutes, be then centrifuged, precipitating is re-dispersed into hexane
In after ultrasound 2 hours.Solution is centrifuged again to obtain poly (methyl methacrylate) micro-sphere precipitating.
Then by the 5mL CsPb (Br/Cl) of preparation3Perovskite nanocrystal solution (perovskite containing 0.001mmol is nanocrystalline,
For diameter in 4~12nm, solvent is the toluene and ethane of volume ratio 1:4) it is added in polymethyl methacrylate precipitating, ultrasound 1 is small
When, then under agitation 24 hours.Solution is centrifuged to obtain perovskite and polymethyl methacrylate compound particle.It will obtain
The grain obtained is re-dispersed into hexane solution, and by precipitating, redisperse obtains perovskite supported polymethyl into hexane
Sour methyl esters particle.Finally the product of preparation is re-dispersed into water, it is nanocrystalline to obtain water-soluble perovskite.Specific experiment mistake
The experiment mechanism choice of journey as shown in Figure 1.
Embodiment 4:
Firstly, 10mL ethyl alcohol is added in 0.01g (1mL) water-soluble polychlorostyrene acetylene microballoon (size is at 0.1~10 micron)
In, further disperse to obtain homogeneous phase solution within ultrasound 30 minutes, be then centrifuged, ultrasound after precipitating is re-dispersed into hexane
2 hours.Solution is centrifuged again to obtain polychlorostyrene acetylene microballoon precipitating.
Then by the 5mL CsPb (Br/I) of preparation3Perovskite nanocrystal solution (perovskite containing 0.001mmol is nanocrystalline,
For diameter in 4~12nm, solvent is the toluene and ethane of volume ratio 1:1) it is added in polychlorostyrene acetylene precipitating, ultrasound 1 hour, then
24 hours under agitation.Solution is centrifuged to obtain perovskite and polychlorostyrene acetylene compound particle, the grain of acquisition is dispersed again
Into hexane solution, by precipitating, redisperse obtains perovskite supported polychlorostyrene acetylene particle into hexane.Finally by preparation
Product is re-dispersed into water, and it is nanocrystalline to obtain water-soluble perovskite.The experiment mechanism of specific experiment process as shown in Figure 1
Figure.
Embodiment 5:
Firstly, by 0.04g (1mL) water-soluble acrylonitrile-butadiene-styrene copolymer microballoon, (size is 0.1~10
Micron) it is added in 10mL ethyl alcohol, further disperse to obtain homogeneous phase solution within ultrasound 30 minutes, be then centrifuged, will be precipitated again
Ultrasound 2 hours after being distributed in hexane.Solution is centrifuged again to obtain acrylonitrile-butadiene-styrene copolymer microballoon precipitating.
Then by the 5mL CsPbI of preparation3(perovskite containing 0.001mmol is nanocrystalline, and diameter exists for perovskite nanocrystal solution
4~12nm, solvent are the toluene and ethane of volume ratio 1:10) it is added in acrylonitrile-butadiene-styrene copolymer precipitating,
Ultrasound 1 hour, then under agitation 24 hours.Finally solution is centrifuged to obtain perovskite and acrylonitrile-butadiene-benzene second
Alkene copolymer compound particle.The grain of acquisition is re-dispersed into hexane solution, by precipitating, redisperse is final into hexane to be obtained
To perovskite supported acrylonitrile-butadiene-styrene copolymer particle.Finally the product of preparation is re-dispersed into water,
It is nanocrystalline to obtain water-soluble perovskite.The experiment mechanism choice of specific experiment process as shown in Figure 1.
Embodiment 6:
Firstly, 10mL ethyl alcohol is added in 0.02g (1mL) water-soluble epoxide resin microballoon (size is at 0.1~10 micron)
In, further disperse to obtain homogeneous phase solution within ultrasound 30 minutes, be then centrifuged, ultrasound after precipitating is re-dispersed into hexane
2 hours.Solution is centrifuged again to obtain epoxide resin microballoon precipitating.
Then by the 5mL CsPbBr of preparation3(perovskite containing 0.002mmol is nanocrystalline, diameter for perovskite nanocrystal solution
In 4~12nm, solvent is the toluene and ethane of volume ratio 1:20) it is added in epoxy resin precipitating, then ultrasound 1 hour exists
Stirring condition lower 24 hours.Solution is centrifuged to obtain perovskite and epoxy resin compound particle.The grain of acquisition is re-dispersed into
In hexane solution, by precipitating, redisperse obtains perovskite supported epoxy resin particle into hexane.Finally by the production of preparation
Object is re-dispersed into water, and it is nanocrystalline to obtain water-soluble perovskite.The experiment mechanism choice of specific experiment process as shown in Figure 1.
Embodiment 7:
The nanocrystalline stability test of the water-soluble calcium titanium ore of polystyrene microsphere cladding.
The water-soluble calcium titanium ore of polystyrene microsphere cladding in embodiment 2 nanocrystalline is distributed to pH 1, pH 7 respectively
In the aqueous solution of pH 14, then section monitors its fluorescence spectrum in different times respectively, and specific spectrum change process is shown in Fig. 3
~Fig. 5 can be seen that its nanocrystalline fluorescence intensity of the water-soluble calcium titanium ore coated is basically unchanged by Fig. 3~Fig. 5, indicate that it has
Good stability.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (3)
1. a kind of water-soluble CsPbX of high stability3The nanocrystalline preparation method of perovskite, will be water-soluble using exchange of solvent method
Polymer microballoon is added in ethyl alcohol, is further dispersed to obtain homogeneous phase solution within ultrasound 30 minutes, is then centrifuged, will be precipitated again
Ultrasound 2 hours after being distributed in hexane, then be centrifuged to obtain polymer microballoon precipitating；It then will be dispersed in toluene and hexane mixing be molten
CsPbX in agent3Perovskite is nanocrystalline to be mixed 24 hours with the polymer microballoon precipitating, is obtained perovskite by centrifugation and is received
The polymer particle of the brilliant load of rice, is finally dispersed to obtain water-soluble calcium titanium ore nanoparticle in aqueous solution；Wherein X be derived from Cl,
Br or I；The volume ratio of toluene and hexane is 1:1~20 in the toluene and hexane mixed solvent.
2. a kind of water-soluble CsPbX of high stability according to claim 13The nanocrystalline preparation method of perovskite, it is special
Sign is, the polymer microballoon is polyethylene, polyvinyl chloride, polypropylene, polystyrene, and polymethyl methacrylate gathers
Acrylonitrile-butadiene-styrene (ABS), polyamide or epoxy resin, for size between 0.1 to 10 microns, surface is sulfonate radical modification
's.
3. a kind of water-soluble CsPbX of high stability according to claim 1 or 23The nanocrystalline preparation method of perovskite,
It is characterized in that, the CsPbX3The nanocrystalline size of perovskite is 4~12 nanometers.
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| CN113444514B (en) * | 2021-06-17 | 2022-12-23 | 上海大学 | Hydrophobic perovskite-polymer composite material and preparation method thereof |
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| CN114958367B (en) * | 2022-06-09 | 2023-06-06 | 南京工业大学 | Preparation and biological imaging application of water-soluble lead halide perovskite nanocrystalline |
| CN115161011B (en) * | 2022-07-20 | 2024-03-01 | 上海电力大学 | High-stability perovskite phase CsPbI 3 Nanocrystalline and preparation method thereof |
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