CN109775750A - A kind of solwution method prepares full-inorganic perovskite CsPbBr3The method and up-conversion luminescent material of nano wire - Google Patents
A kind of solwution method prepares full-inorganic perovskite CsPbBr3The method and up-conversion luminescent material of nano wire Download PDFInfo
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Abstract
The invention discloses a kind of solwution methods to prepare full-inorganic perovskite CsPbBr3The method and up-conversion luminescent material of nano wire, with oleyl amine, oleic acid and octadecylene proportioning concentration are solvent, and lead source and caesium source is added as reactant, it is reacted in the environment of no steam, the nucleation of nano wire is then completed by stages such as heating, heat preservation and coolings, the processes such as grow and grow up, dissolvent residual is removed to, carry out being separated by solid-liquid separation after reaction, prepares full-inorganic perovskite CsPbBr3Nano wire.The method avoids high temperature, time loss, without complicated equipment, therefore it is easy, efficiently, mass production requirement can be met.Conversion and lower Illuminant nanometer material of converting is full-inorganic perovskite CsPbBr in involved green3Nano wire, photoluminescence band is relatively narrow, gained green light purity is high, converts in the green and lower conversion Illuminant nanometer material is suitable for display device, security devices, infrared detector and solar photovoltaic device etc..
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of solwution method prepares full-inorganic perovskite
CsPbBr3The method and up-conversion luminescent material of nano wire.
Background technique
Upper conversion and down-conversion luminescent material are all especially important functional materials, in display field, anti-counterfeit field, biology
Fluorescent marker field all has especially important purposes.Up-conversion luminescence is the sustainable launch wavelength under long wavelength light excitation
Than the light of excitation wave length, it is luminous substantially to belong to a kind of trans- Stokes, and lower conversion is luminous just the opposite with upper conversion,
It is the sustainable launch wavelength light longer than excitation wavelength under the excitation of short wavelength light.In previous research, up-conversion luminescence material
The basis material of material mainly includes fluoride, oxide, sulfur-containing compound, fluorine mainly using rare earth element as research emphasis
Oxide, halide etc..Wherein, the NaYF of hexagonal phase4Basis material is at present in up-conversion luminescence field efficiency highest one
Kind of host material, however, it is necessary to realize that upper conversion shines by the doping of double rare-earth elements and the doping of more rare earth elements.
And down-conversion luminescent material meets Stokes' law, luminescence generated by light effect easy to accomplish, so relatively conventional due to it.
In recent years, upper conversion has been extended to a kind of novel perovskite structure with down-conversion luminescent material.Since Japan
The Miyasaka of the Yokohama Tong Yin university teaches first using halide perovskite material as absorber of light application, all solid state calcium titanium
The development and utilization of mine battery all has received great concern all the time, becomes solar energy materials and up-conversion luminescent material
The hot spot of research.Hu Zhiping et al. is using near-infrared light source (800nm) to CsPbBr3Micro- cube carries out illumination, and sends out
CsPbBr is showed3It can be applied not only to the exploitation of battery, its own is with good up-conversion luminescence effect, CsPbBr3It is positive
Crystallographic system is handed over, Pbnm (62) space group is belonged to, wherein rare earth element is free of, but under the irradiation of near infrared light, CsPbBr3It can
Issue green fluorescence, and stable luminescent property.And Yu Xiaoya et al. utilizes ultraviolet source (400nm) to CsPbBr3Nanometer is vertical
Cube is excited, CsPbBr3Bright green light is released again, shows CsPbBr3With good lower conversion luminescent effect.
These phenomenons successfully cause the concern of domestic and foreign scholars.In addition, about CsPbBr3The reason of luminescence generated by light also always with
To belong to the hot spot of academia's arguement.Therefore research CsPbBr3Up-conversion luminescent material not only has important learning value；And
And it shines also with important potential application.
CsPbX was reported for the first time in 2015 from Kovalenco et al.3Since nanocrystalline body heat injection synthesis, to CsPbBr3
Material preparation research be a hot spot always, be concentrated mainly on by ion exchange, room temperature reprecipitation, Microwave-assisted synthesis,
A variety of methods such as CVD are synthesized.Single-phase CsPbBr is synthesized using solwution method3Nano wire yet there are no the report of document, so, it grinds
Study carefully and develop a kind of single-phase CsPbBr of solwution method synthesis3The technique of nano wire is very urgent.Relevant research not only can be with
Promote single-phase CsPbBr3The basic research of nano material, and this efficient upper conversion can be promoted to send out with lower conversion
Luminescent material display, label, in terms of important application.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing a kind of solution legal system
Standby full-inorganic perovskite CsPbBr3The method and up-conversion luminescent material of nano wire not only obtain high-purity single-phase CsPbBr3It receives
Rice noodles, and relevant optical property is had studied, obtain a kind of new function material of high incidence light.
The invention adopts the following technical scheme:
A kind of solwution method prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, which is characterized in that with Cs2CO3
And PbBr2As reactant, it is added in the high boiling solvent A being mixed by oleyl amine, oleic acid and octadecylene, then in indifferent gas
It heated up, kept the temperature and cooling processing under body protection, completed the nucleation of nano wire, grow and grow up, to after reaction, use
It is separated by solid-liquid separation and removes dissolvent residual, prepare single-phase full-inorganic perovskite CsPbBr3Nano wire.
Specifically, oleic acid, oleyl amine and octadecylene are mixed by the volume ratio of 1:1:2.
Further, heating stirring is carried out to high boiling solvent A, while carries out pumping and heating treatment, continued at least
60min obtains no oxygen without steam reaction environment.
Specifically, the high boiling solvent A of preparation is down to room temperature, in molar ratio (0.05~0.2): 1 is added Cs2CO3With
PbBr2Mixed solution B is obtained, under lasting stirring and inert gas, by mixed solution B temperature reaction, completes nanowire growth,
Then stop heating, reaction system is cooled to room temperature.
Further, warming temperature is 100~120 DEG C, and the reaction time is 30~60min in inert gas.
Further, PbBr2For 1~1.2mmol, Cs2CO3For 0.05~0.24mmol.
Specifically, inert gas is high-purity argon gas or nitrogen.
Specifically, being separated by solid-liquid separation using centrifuge separation, centrifugation rate is 5000~9000r/min；Then hexamethylene is used
Alkane is cleaned.
Specifically, controlling 50~70 DEG C of temperature after being separated by solid-liquid separation, it is orange that acquisition was dried within the time 30~60 minutes
The single-phase full-inorganic perovskite CsPbBr of color3Nano wire.
Another technical solution of the invention is a kind of up-conversion luminescent material, the CsPbBr prepared using the method3It receives
Rice noodles are prepared.
Compared with prior art, the present invention at least has the advantages that
The present invention synthesizes single-phase CsPbBr using solwution method3Nano wire, method is easier, more efficient, safer, harmless,
By being simply vented, heating up, keep the temperature, cooling four-stage can synthesize CsPbBr3Nano wire is of the invention one very big
Advantage is that of avoiding the solid phase procedures of high temperature, time loss, and complicated equipment, to synthesize pure CsPbBr3Nano wire provides
It higher operation accessibility and shorter reaction time, uses oleyl amine, oleic acid and octadecylene for solvent, is a kind of atent solvent
And it is harmless.
Further, the growth for carrying out nano wire without the environment of steam by no oxygen, can be to avoid water in growth course
The destruction of vapour reaches the mesh of in-situ conservation.
Further, used lead salt is lead bromide；Caesium source is cesium carbonate, and the molar ratio of lead bromide and cesium carbonate is 1:
The ratio of (0.05~0.2) may insure final element metering ratio, avoid generating the second phase.
Further, reaction temperature is 100~120 DEG C, does not use pyroreaction, avoids the wasting of resources, when reaction
Between be 30~60min, improve reaction speed, be advantageously implemented batch production.
Further, the protective atmosphere of reaction process is high-purity argon gas or nitrogen, can be effectively protected nano wire, avoid
Nano wire is oxidized or destroys in growth course.
Further, it is separated by solid-liquid separation, can be produced to avoid there is Newly born phase in products therefrom with protecting after reaction
The purity of object, the present invention is for the CsPbBr that makes3Liquid need to only use cyclohexane, not be related to any acid after separation
Journey is washed, to environment without any pollution.
Further, sample is dried, sample volatilization can be avoided to be lost in order to store.
CsPbBr prepared by the present invention3Nano wire is conversion and lower conversion Illuminant nanometer material, luminescence generated by light in green
Bands of a spectrum are relatively narrow, gained green light purity is high, and conversion is suitable for display device, antifake device with lower conversion Illuminant nanometer material in green
Part, infrared detector and solar photovoltaic device.
In conclusion the invention avoids high temperature, time loss, without complicated equipment, therefore it is easy, efficiently, it can expire
Sufficient mass production requirement.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is the XRD spectrum of embodiment 1；
Fig. 2 is the up-conversion luminescence map of embodiment 1；
Fig. 3 is the luminous map of lower conversion of embodiment 1；
Fig. 4 is the absorption map of embodiment 1；
Fig. 5 is the XRD spectrum of embodiment 2；
Fig. 6 is the up-conversion luminescence map of embodiment 2；
Fig. 7 is the luminous map of lower conversion of embodiment 2；
Fig. 8 is the XRD spectrum of embodiment 3.
Specific embodiment
The present invention provides a kind of solwution methods to prepare full-inorganic perovskite CsPbBr3The method of nano wire, with oleyl amine, oleic acid
It is high boiling solvent A with octadecylene mixed liquor, and by PbBr2With Cs2CO3As reactant, carried out under the protection of inert gas
Reaction, then by exhaust, heating, heat preservation and cooling four-stage, to after reaction, remove organic substance residues, preparation is obtained
Obtain full-inorganic perovskite CsPbBr3Nano wire.
A kind of solwution method of the present invention prepares full-inorganic perovskite CsPbBr3The method of nano wire, comprising the following steps:
S1, oleyl amine, oleic acid and octadecylene are mixed into high boiling solvent A with the volume ratio of 1:1:2；
S2, heating stirring is carried out to high boiling solvent A, while carries out pumping process, by heating, so that the oxygen in solvent
Gas and steam are sufficiently pumped, this process continues 60 minutes, to obtain reaction environment of the no oxygen without steam；
It is cooled to room temperature after the completion of S3, step S2, a certain proportion of Cs is added2CO3And PbBr2Mixed solution B is obtained,
Under lasting stirring and protective atmosphere, mixed solution B is warming up to certain temperature and is reacted, completed through reaction after a period of time
Nanowire growth, then stops heating, and reaction system is cooled to room temperature；
PbBr2For 1~1.2mmol, Cs2CO3For 0.05~0.24mmol；PbBr2And Cs2CO3Molar ratio range be 1:
(0.05~0.2), reaction temperature are 100~120 DEG C, and the reaction time is 30~60min, and protective atmosphere is high-purity argon gas or nitrogen
Gas.
S4, by centrifuge separation, centrifugation rate be 5000~9000r/min；It is cleaned with hexamethylene, outwells solution,
It realizes and is separated by solid-liquid separation, be dried in drying box, drying temperature is 50~70 DEG C, and the time is 30~60 minutes, is obtained orange
The product of color, as target product.
The full-inorganic perovskite CsPbBr prepared using the method for the present invention3For pure phase nanometer linear structure, photoluminescence spectrum
With relatively narrow, gained green light purity is high, suitable for display device, security devices, infrared detector and solar photovoltaic device.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being described and shown in usually here in attached drawing is real
The component for applying example can be arranged and be designed by a variety of different configurations.Therefore, below to the present invention provided in the accompanying drawings
The detailed description of embodiment be not intended to limit the range of claimed invention, but be merely representative of of the invention selected
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
Firstly, injecting 2mL oleyl amine, 2mL oleic acid and 4mL octadecylene are mixed into high boiling solvent A in bis- mouthfuls of bottles of 50mL；
Then, heating stirring is carried out to high boiling solvent A, is evacuated, while by being warming up to 100 DEG C, keeping the temperature 60min.Repeatedly into
Line number time gas washing is to obtain environment of the no oxygen without steam；Then, 1mmol PbBr is added2With 0.1mmol Cs2CO3, make
PbBr2: Cs2CO3Molar ratio be 1:0.1.Under lasting stirring and protective atmosphere, 100 DEG C are warming up to, heat preservation 60min completion is received
Nanowire growth, then stops heating, and reaction system is cooled to room temperature；Finally, using ring by centrifuge separation at 5000r/min
Hexane cleans 3 times, outwells solution, obtains orange-yellow powder, as target product in 50 DEG C of drying 60min.
Fig. 1 is the monocrystalline CsPbBr that is grown according to embodiment 13The X-ray diffraction spectrum of nano wire, free from admixture peak go out
It is existing, illustrate that product is for pure CsPbBr3。
It in wavelength 980nm laser is excitaton source, the luminescent properties of acquisition, test wavelength range 200 that Fig. 2, which is embodiment 1,
~900nm, the peak PL after laser excitation are located at 550nm or so, and half-peak breadth is about 14nm, have good monochromaticjty.
It in wavelength 365nm laser is excitaton source, the luminescent properties of acquisition, test wavelength range 200 that Fig. 3, which is embodiment 1,
~900nm, the peak PL after laser excitation are located at 531nm or so, and half-peak breadth is about 16nm, have good monochromaticjty.
Fig. 4 is the absorption spectrogram of embodiment 1, and absorption peak is located at 520nm or so, corresponding with the peak position PL.
Embodiment 2
Firstly, injecting 4mL oleyl amine, 4mL oleic acid and 8mL octadecylene are mixed into high boiling solvent A in bis- mouthfuls of bottles of 50mL；
Then, heating stirring and pumping are carried out to high boiling solvent A, while by being warming up to 100 DEG C, keeps the temperature 60min, number is repeated
Secondary gas washing is to obtain environment of the no oxygen without steam；Then, 1mmol PbBr is added2With 0.05mmol Cs2CO3, make PbBr2:
Cs2CO3Molar ratio be 1:0.05.Under lasting stirring and protective atmosphere, 120 DEG C are warming up to, heat preservation 30min completes nano wire
Growth, then stops heating, and reaction system is cooled to room temperature；Finally, using hexamethylene by centrifuge separation at 9000r/min
Cleaning 3 times, outwells solution, obtains orange-yellow powder, as target product in 70 DEG C of drying 30min.
Fig. 5 is the monocrystalline CsPbBr grown by embodiment 23The X-ray diffraction spectrum of nano wire, PbBr2: Cs2CO3For
1:0.05, free from admixture peak occur, and illustrate that product is for pure CsPbBr3。
It in wavelength 980nm laser is excitaton source, the luminescent properties of acquisition, test wavelength range 200 that Fig. 6, which is embodiment 1,
~900nm, the peak PL after laser excitation are located at 551nm or so, and half-peak breadth is about 12nm.
It in wavelength 365nm laser is excitaton source, the luminescent properties of acquisition, test wavelength range 200 that Fig. 7, which is embodiment 1,
~900nm, the peak PL after laser excitation are located at 552nm or so, and half-peak breadth is about 18nm, have good monochromaticjty.
Embodiment 3
Firstly, injecting 3mL oleyl amine, 3mL oleic acid and 6mL octadecylene are mixed into high boiling solvent A in bis- mouthfuls of bottles of 50mL；
Then, heating stirring and pumping are carried out to high boiling solvent A, while by being warming up to 120 DEG C, keeps the temperature 30min, number is repeated
Secondary gas washing is to obtain environment of the no oxygen without steam；Then, 1.2mmol PbBr is added2With 0.24mmol Cs2CO3, make
PbBr2: Cs2CO3Molar ratio be 1:0.2.Under lasting stirring and protective atmosphere, 110 DEG C are warming up to, heat preservation 40min completion is received
Nanowire growth, then stops heating, and reaction system is cooled to room temperature；Finally, using ring by centrifuge separation at 7000r/min
Hexane cleans 3 times, outwells solution, obtains orange-yellow powder, as target product in 60 DEG C of drying 40min.
Fig. 8 is the monocrystalline CsPbBr grown by embodiment 33The X-ray diffraction spectrum of nano wire, PbBr2: Cs2CO3For
1:0.2, free from admixture peak occur, and illustrate that product is for pure CsPbBr3。
Above 3 embodiments, have finally all obtained the CsPbBr of pure phase3Nano wire reacts preset condition, institute by changing
Product pattern, purity etc. all do not change, it was demonstrated that the feasibility of the above implementation condition.Technique of the present invention
Method is easier, more efficient, safer, harmless, by being simply vented, heating up, keeps the temperature, cooling four-stage can synthesize
CsPbBr3Nano wire avoids high temperature and time loss.
1-dimention nano wire material is a kind of novel photovoltaic material, has good optical absorption characteristics, Light-Emitting Diode,
Display device and the photovoltaic property aspect for improving solar battery have potential application.University Copenhagen Denmark Bohr grinds
Study carefully Robert Feidenhansl et al. by being furtherd investigate to a variety of nanometers of filamentary materials, discovery uses nano wire
Manufactured LED only needs to utilize few outside resources, so that it may provide more as bright light source.Currently, GaN nano wire
LED and InGaN nanowire LED has been prepared out, and is had received widespread attention.And full-inorganic perovskite CsPbBr3
The appearance of nano wire provides a new direction for the development of one-dimensional nano line LED.
The method of the present invention main characteristics are the formula rate being added by raw material, can obtain the CsPbBr of pure phase3Change
Close object.Relative to Cs4PbBr6Deng the compound of other stoicheiometries, CsPbBr3Compound is a kind of multifunctional material, existing excellent
Different upper conversion performance also has particularly preferred lower conversion luminescent properties.Upper transformational provided by the present invention and lower conversion shine
Spectrogram has very narrow bandwidth, is a kind of especially excellent luminescence feature close to monochrome, will show neck in green emitting
The fields such as domain and anti-fake mark tool plays a very important role.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. a kind of solwution method prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, which is characterized in that with Cs2CO3With
PbBr2As reactant, it is added in the high boiling solvent A being mixed by oleyl amine, oleic acid and octadecylene, then in inert gas
It heated up, kept the temperature and cooling processing under protection, completed the nucleation of nano wire, grow and grow up, to after reaction, using solid
Liquid is separated off dissolvent residual, prepares single-phase full-inorganic perovskite CsPbBr3Nano wire.
2. solwution method according to claim 1 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, feature
It is, oleic acid, oleyl amine and octadecylene are mixed by the volume ratio of 1:1:2.
3. solwution method according to claim 1 or 2 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, it is special
Sign is, carries out heating stirring to high boiling solvent A, while carrying out pumping and heating treatment, continues at least 60min and obtains anaerobic
Gas is without steam reaction environment.
4. solwution method according to claim 1 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, feature
It is, the high boiling solvent A of preparation is down to room temperature, in molar ratio (0.05~0.2): 1 is added Cs2CO3And PbBr2It is mixed
Solution B is closed, is stirred lasting under inert gas, by mixed solution B temperature reaction, is completed nanowire growth, then stop adding
Heat, reaction system are cooled to room temperature.
5. solwution method according to claim 1 or 4 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, it is special
Sign is that warming temperature is 100~120 DEG C, and the reaction time is 30~60min in inert gas.
6. solwution method according to claim 5 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, feature
It is, PbBr2For 1~1.2mmol, Cs2CO3For 0.05~0.24mmol.
7. solwution method according to claim 1 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, feature
It is, inert gas is high-purity argon gas or nitrogen.
8. solwution method according to claim 1 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, feature
It is, is separated by solid-liquid separation using centrifuge separation, centrifugation rate is 5000~9000r/min；Then it is cleaned with hexamethylene.
9. solwution method according to claim 1 prepares full-inorganic perovskite CsPbBr3The preparation method of nano wire, feature
It is, after separation of solid and liquid, controls 50~70 DEG C of temperature, it is orange-yellow single-phase complete that acquisition was dried within the time 30~60 minutes
Inorganic perovskite CsPbBr3Nano wire.
10. a kind of up-conversion luminescent material, according to claim 1 to CsPbBr prepared by any one of 9 the methods3Nano wire
It is prepared.
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