CN110255607A - A kind of high stability cross CsPbBr3The nanocrystalline preparation method of perovskite and its product obtained - Google Patents
A kind of high stability cross CsPbBr3The nanocrystalline preparation method of perovskite and its product obtained Download PDFInfo
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- CN110255607A CN110255607A CN201910622147.7A CN201910622147A CN110255607A CN 110255607 A CN110255607 A CN 110255607A CN 201910622147 A CN201910622147 A CN 201910622147A CN 110255607 A CN110255607 A CN 110255607A
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Abstract
The invention discloses a kind of high stability cross CsPbBr3The nanocrystalline preparation method of perovskite, with metal halide lead and Cs2CO3It for raw material, sequentially adds 1- octadecylene, oleic acid and oleyl amine and forms precursors, obtain mixed liquor after two sections of heating are reacted；Then precipitating reagent is added in mixed liquor, after being centrifuged off supernatant, be added dispersing agent disperse to precipitate again, through the obtained supernatant of centrifugal treating be pattern be criss-cross perovskite nanocrystal solution.Product made from above-mentioned preparation method is utilized in addition, also disclosing.Raw material needed for preparation method of the present invention is cheap and easy to get, and preparation process is simple, is suitble to large-scale production；Obtained cross CsPbBr3Perovskite is nanocrystalline to have good dispersibility, excellent luminescent properties and photostability.
Description
Technical field
The present invention relates to perovskite nanocrystalline material technical field more particularly to a kind of high stability cross CsPbBr3
The nanocrystalline preparation method of perovskite and its product obtained.
Background technique
Full-inorganic metal halide perovskite (CsPbX3, X=Cl, Br, I) and nanocrystalline due to tuning model with launch wavelength
The features such as enclosing wide (400~700nm), fluorescence quantum efficiency height (~100%), half-peak width (12~40nm), in solar-electricity
The fields such as pond, light emitting diode, laser, photodetection and backlight display are with a wide range of applications.Although CsPbX3Nanometer
Crystalline substance has an above excellent optical property, but its there are serious stability problems, if being chronically exposed under environmental condition
(such as wet, light, heat and oxygen) will all cause nanocrystalline degradation, lead to the sharp-decay of its fluorescence property, strongly limit
In the development and application of photoelectric field.
To solve the above-mentioned problems, researcher proposes a variety of methods to improve CsPbX in succession3Perovskite is nanocrystalline
Stability mainly includes modified surface, Shell Materials cladding and lattice optimization etc..Although surface cladding process mentions to a certain extent
The high nanocrystalline stability of perovskite, but its is complicated for operation, not only increases preparation cost, has also delayed manufacturing cycle,
It is unfavorable for its large-scale production.Therefore, develop a kind of nanocrystalline optical property of convenient and fast in situ regulation perovskite and to improve it steady
Qualitative method becomes the hot spot of current research.Preparing the nanocrystalline most important method of perovskite at present is hot injection method, should
Cs presoma is rapidly injected in the precursor solution containing Pb by method needs at 160~200 DEG C, and reaction obtains rapidly
CsPbX3It is nanocrystalline.But the harsh experiment conditions such as that there are reaction temperatures is higher for this method, needs inert atmosphere protection；Meanwhile
Nanocrystalline optical property depends on volume, injection rate and the cooling rate of presoma, and it is extensive raw to strongly limit it
It produces；In addition, nanocrystalline faster nucleation and growth rate (5~20s) is unfavorable for carrying out Effective Regulation to the pattern of crystal.This
Outside, also studies have reported that nanocrystalline to perovskite by adjusting response parameter (ligand additive amount, ligand species, reaction time etc.)
Pattern and surface nature regulated and controled, obtain the nanocrystalline of special appearance and optical property, such as: nano wire, is received nanometer sheet
Rice stick.However, these nanocrystalline fluorescence properties with special appearance are still to be improved, especially stability problem is not
It is solved at all.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of high stability cross CsPbBr3Calcium titanium
The nanocrystalline preparation method of mine prepares a kind of high stability cross CsPbBr by implementing two sections of heating3Perovskite nanometer
Crystalline substance, to improve the nanocrystalline stability of perovskite.Another object of the present invention is to provide using made from above-mentioned preparation method
Product.
The purpose of the present invention is achieved by the following technical programs:
A kind of high stability cross CsPbBr provided by the invention3The nanocrystalline preparation method of perovskite, including it is following
Step:
(1) by metal halide lead and Cs2CO3According to molar ratio Pb: Cs=1~3: 1 mix after, sequentially add 1- octadecylene,
Oleic acid and oleyl amine form precursors；
(2) two sections of heating are carried out to the precursors, i.e., after reacting 10~30min at a temperature of 70~90 DEG C, risen
Temperature obtains mixed liquor to 100~140 DEG C of the reaction was continued 15~40min；
(3) precipitating reagent is added in the mixed liquor, after being centrifuged, removing supernatant, dispersing agent weight is added in precipitating
New dispersion precipitating, the supernatant obtained after being centrifuged are that pattern is criss-cross CsPbBr3Perovskite nanocrystal solution.
Further, according to molar ratio metal ion in step (1) of the present invention: 1- octadecylene: oleic acid: oleyl amine=1:
45~90: 4~9: 3~8.The precipitating reagent is toluene, acetonitrile or ethyl acetate.The dispersing agent is n-hexane, chloroform or ring
Hexane.
The present invention utilizes above-mentioned high stability cross CsPbBr3Product made from the nanocrystalline preparation method of perovskite,
The pattern is criss-cross CsPbBr3Perovskite is nanocrystalline, and criss-cross a length of 10~30nm, width are 5~10nm.
The invention has the following advantages:
(1) present invention is prepared using two sections of heatings, first at low temperature Cs2CO3Slowly release Cs+Ion, it is raw
At CsPbBr3It is nanocrystalline, a kind of cross CsPbBr is then formed by molecular self-assembling3Perovskite is nanocrystalline.The cross is received
Meter Jing has good dispersibility, excellent luminescent properties and photostability.
(2) the required raw material of the present invention is simple and easy to get, and reaction condition is mild, easy to operate, efficiently, does not need inert atmosphere
Protection is suitable for large-scale industrial production.
Detailed description of the invention
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail:
Fig. 1 is the CsPbBr that the embodiment of the present invention one is prepared3The nanocrystalline XRD spectrum of perovskite；
Fig. 2 is the CsPbBr that the embodiment of the present invention one is prepared3The nanocrystalline uv-visible absorption spectra of perovskite；
Fig. 3 is the CsPbBr that the embodiment of the present invention one is prepared3The nanocrystalline TEM photo of perovskite；
Fig. 4 is the CsPbBr that comparative example is prepared3The nanocrystalline TEM photo of perovskite；
Fig. 5 is the CsPbBr that the embodiment of the present invention one and comparative example are prepared3The nanocrystalline PL spectrum of perovskite；
Fig. 6 is the CsPbBr that the embodiment of the present invention one is prepared3Perovskite is nanocrystalline and comparative example is in ultraviolet lighting
Photostability curve graph under the conditions of penetrating；
Fig. 7 is the CsPbBr that the embodiment of the present invention one is prepared3Perovskite is nanocrystalline and comparative example stores 30 days
Photostability curve graph；
Fig. 8 is the CsPbBr that the embodiment of the present invention two is prepared3The nanocrystalline TEM photo of perovskite；
Fig. 9 is the CsPbBr that the embodiment of the present invention two is prepared3The nanocrystalline PL spectrum of perovskite；
Figure 10 is the CsPbBr that the embodiment of the present invention three is prepared3The nanocrystalline TEM photo of perovskite；
Figure 11 is the CsPbBr that the embodiment of the present invention three is prepared3The nanocrystalline HRTEM photo of perovskite；
Figure 12 is the CsPbBr that the embodiment of the present invention four is prepared3The nanocrystalline PL map of perovskite；
Figure 13 is the CsPbBr that the embodiment of the present invention five is prepared3The nanocrystalline TEM photo of perovskite；
Figure 14 is the CsPbBr that the embodiment of the present invention five is prepared3The nanocrystalline PL map of perovskite.
Specific embodiment
Embodiment one:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, its step are as follows:
(1) PbBr of 0.3mmol is weighed2With the Cs of 0.12mmol2CO3Powder be placed in three-necked flask mix after, successively plus
The oleyl amine (mass fraction 90%) for entering the 1- octadecylene (mass fraction 90%) of 10mL, the oleic acid of 1mL and 1mL forms reaction precursor
Body；
(2) two sections of heating are carried out to above-mentioned precursors, i.e., above-mentioned precursors is placed in oil bath and is heated to 90
DEG C and after keeping the temperature 30min, be warming up to 120 DEG C the reaction was continued 30min, water-bath cooling to room temperature, is mixed after reaction
Liquid；
(3) in above-mentioned mixed liquor be added 10mL precipitating reagent toluene, on the centrifuge of 8000r/min be centrifuged 10min,
After removing supernatant, the dispersing agent n-hexane that 10mL is added in precipitating disperses to precipitate again, then in the centrifugation of 3000r/min
5min is centrifuged on machine to remove bulky grain, obtained supernatant is that pattern is criss-cross CsPbBr3Perovskite is nanocrystalline molten
Liquid.
CsPbBr made from the present embodiment3Perovskite is nanocrystalline, is as shown in Figure 1 monoclinic phase CsPbBr3, and free from admixture produces
It is raw；Occurs CsPbBr at 505nm3Absorption peak (see Fig. 2), further demonstrate that and synthesized CsPbBr3Perovskite is nanocrystalline；
As shown in figure 3, a length of 28.5nm, the width 9.5nm of crossed nano crystalline substance, while there is good dispersibility.
Comparative example:
According to the raw material proportioning of the embodiment of the present invention one, only reacted at a temperature of 120 DEG C using one section of heating
30min, the constant and obtained CsPbBr of remaining condition3It is nanocrystalline as a comparison case.
As shown in figure 4, the CsPbBr of comparative example3Nanocrystalline pattern is cube, crystallite dimension 20nm.
As shown in figure 5, pattern made from the embodiment of the present invention one is criss-cross CsPbBr3Perovskite is nanocrystalline,
Occur at 515nm apparent glow peak (glow peak occurs at 513nm in comparative example), while its fluorescence intensity is higher than comparison
Example, illustrates one CsPbBr of the embodiment of the present invention3Perovskite is nanocrystalline to have good luminescent properties.As shown in fig. 6,25 DEG C,
Under 30% damp condition, ultraviolet lamp Continuous irradiation for 24 hours after, the present embodiment still keeps 80% or more of original fluorescence intensity, the light
Stability is much higher than comparative example.As shown in fig. 7, after storage 30 days, the present embodiment is still protected under 25 DEG C, 30% damp condition
85% or more of original fluorescence intensity is held, which is also much higher than comparative example.
Embodiment two:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, not with embodiment one
It is with place:
1, in the present embodiment step (2), precursors are placed in oil bath be heated to 80 DEG C and keep the temperature 30min after, heating
To 120 DEG C of the reaction was continued 20min.
2, in the present embodiment step (3), precipitating reagent is acetonitrile.
As shown in figure 8, pattern made from the present embodiment is criss-cross CsPbBr3Perovskite is nanocrystalline, criss-cross length
For 22nm, width 7.5nm, there is good dispersibility；There are apparent glow peak (see Fig. 9) at 515nm, show excellent
Optical property.
Embodiment three:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, not with embodiment one
Be with place: in the present embodiment step (2), precursors are placed in oil bath be heated to 90 DEG C and keep the temperature 30min after, rise
Temperature is to 130 DEG C of the reaction was continued 35min.
As shown in Figure 10, pattern made from the present embodiment is criss-cross CsPbBr3Perovskite is nanocrystalline, criss-cross length
For 30nm, width 10nm.From Figure 11 it can be observed that clearly lattice fringe, illustrates nanocrystalline crystallinity with higher, together
When the interplanar distance that measures beCorresponding to monoclinic phase CsPbBr3(110) crystal face.Fluorometric investigation is the result shows that the nanometer
There is apparent glow peak at 519nm in crystalline substance.
Example IV:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, not with embodiment one
It is with place:
1, in the present embodiment step (2), precursors are placed in oil bath be heated to 70 DEG C and keep the temperature 30min after, heating
To 140 DEG C of the reaction was continued 40min.
2, in the present embodiment step (3), dispersing agent is hexamethylene.
As shown in figure 12, pattern made from the present embodiment is criss-cross CsPbBr3Perovskite is nanocrystalline to be deposited at 516nm
In apparent emission peak.
Embodiment five:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, not with embodiment one
It is with place: in the present embodiment step (1), Cs2CO3Dosage be 0.14mmol, oleic acid and oleyl amine (mass fraction 90%)
Dosage is respectively 0.8mL and 1.2mL.
As shown in figure 13, pattern made from the present embodiment is criss-cross CsPbBr3Perovskite is nanocrystalline, criss-cross length
For 10~15nm, width 5nm；Occur apparent glow peak at 518nm (see Figure 14).
Embodiment six:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, not with embodiment one
It is with place: in the present embodiment step (1), Cs2CO3Dosage be 0.08mmol, oleic acid and oleyl amine (mass fraction 90%)
Dosage is respectively 0.9mL and 0.8mL
Embodiment seven:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, not with embodiment one
Be with place: in the present embodiment step (3), precipitating reagent is changed to ethyl acetate.
Pattern made from the present embodiment is criss-cross CsPbBr3Perovskite is nanocrystalline, and criss-cross a length of 30nm, width are
There is apparent glow peak at 520nm in 10nm.
Embodiment eight:
A kind of high stability cross CsPbBr of the present embodiment3The nanocrystalline preparation method of perovskite, not with embodiment one
Be with place: in the present embodiment step (3), dispersing agent is chloroform.
Pattern made from the present embodiment is criss-cross CsPbBr3Perovskite is nanocrystalline, and criss-cross a length of 27nm, width are
There is apparent glow peak at 514nm in 9nm.
Claims (6)
1. a kind of high stability cross CsPbBr3The nanocrystalline preparation method of perovskite, it is characterised in that the following steps are included:
(1) by metal halide lead and Cs2CO3After mixing according to molar ratio Pb: Cs=1~3: 1,1- octadecylene, oleic acid are sequentially added
Precursors are formed with oleyl amine；
(2) two sections of heating are carried out to the precursors to be warming up to after reacting 10~30min at a temperature of 70~90 DEG C
100~140 DEG C of the reaction was continued 15~40min, obtain mixed liquor；
(3) precipitating reagent is added in the mixed liquor, after being centrifuged, removing supernatant, dispersing agent is added in precipitating and divides again
Precipitating is dissipated, the supernatant obtained after being centrifuged is that pattern is criss-cross CsPbBr3Perovskite nanocrystal solution.
2. high stability cross CsPbBr according to claim 13The nanocrystalline preparation method of perovskite, feature exist
In: according to molar ratio metal ion in the step (1): 1- octadecylene: oleic acid: oleyl amine=1: 45~90: 4~9: 3~8.
3. high stability cross CsPbBr according to claim 13The nanocrystalline preparation method of perovskite, feature exist
In: the precipitating reagent is toluene, acetonitrile or ethyl acetate.
4. high stability cross CsPbBr according to claim 13The nanocrystalline preparation method of perovskite, feature exist
In: the dispersing agent is n-hexane, chloroform or hexamethylene.
5. utilizing high stability cross CsPbBr described in one of claim 1-43Made from the nanocrystalline preparation method of perovskite
Product.
6. high stability cross CsPbBr according to claim 53The nanocrystalline preparation method of perovskite is obtained to be produced
Product, it is characterised in that: the pattern is criss-cross CsPbBr3Perovskite is nanocrystalline, criss-cross a length of 10~30nm, width
For 5~10nm.
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| CN110943178A (en) * | 2019-11-25 | 2020-03-31 | 北京科技大学 | Self-assembly multi-dimensional quantum well CsPbX3Perovskite nanocrystalline electroluminescent diode |
| CN111171814A (en) * | 2020-01-08 | 2020-05-19 | 上海大学 | Synthesis method of perovskite nanorod |
| CN111573716A (en) * | 2020-05-15 | 2020-08-25 | 南京工业大学 | Spindle-type perovskite CsPbBr3Method for preparing micron particles |
| CN114906872A (en) * | 2022-04-19 | 2022-08-16 | 东华大学 | Stably dispersed all-inorganic CsPbBr 3 Preparation method of perovskite nanorod |
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