CN109135740A - The polishing preparation process of perovskite quantum dot - Google Patents

The polishing preparation process of perovskite quantum dot Download PDF

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CN109135740A
CN109135740A CN201810647385.9A CN201810647385A CN109135740A CN 109135740 A CN109135740 A CN 109135740A CN 201810647385 A CN201810647385 A CN 201810647385A CN 109135740 A CN109135740 A CN 109135740A
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陈大钦
陈筱
李俊霓
钟家松
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Hangzhou Dianzi University
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C09K11/664—Halogenides
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Abstract

The invention discloses the polishing preparation processes of perovskite quantum dot.The present invention is based on the ion diffusions under macrostate, ion is after diffuseing to form perovskite crystal, its particle is set to be gradually reduced and (spread and reduce particle in other words while carrying out) with grinding, it is ionic higher due to raw material and product, therefore it is very easy to carry out ion diffusion, this is a kind of top-down synthesis mode.Colorful light-emitting quantum dot prepared by the present invention, centre of luminescence wavelength in 400nm to adjustable between 750nm, can development and application in display technology, the practical application in backlight especially on television.

Description

The polishing preparation process of perovskite quantum dot
Technical field
The present invention is a kind of novel perovskite nanometer crystal preparation method, specifically the polishing preparation of perovskite quantum dot Technique.This method is suitable for studying the nanocrystalline preparation of most hot several perovskites, such as full-inorganic perovskite CsPbX at present3 (X=Cl, Br, I) and organic inorganic hybridization perovskite MAPbX3(MA=CH3NH3), FAPbX3(FA=CH (NH2)2)。
Background technique
Quantum dot, most commonly used definition is zero dimension quantized system, i.e., the system being all restricted in three dimensions, one As for, particle size be close to or smaller than the material Exciton Bohr Radius.Studying at present relatively broad mainly has II B- V A race InP class quanta point material of VI A race CdSe class quantum dot and III A-, but due to such quanta point material preparation process Complicated (additional shell is such as needed to protect quantum dot), and research cost is higher and main core technology rests in state Outside.Furthermore cadmium element has stronger toxicity, therefore is unfavorable for actual application and industrialization production.
Recently a kind of novel perovskite structure (APbX3, A=Cs, MA, FA, X=Cl, Br, I) and quantum dot is high with its The extensive research of quantum efficiency, high chromatographic purity and high chromatography coverage rate by scholar.It is ground by science in recent years Study carefully and obtained high performance perovskite quanta point material and be applied in quantum dot LED component, to realize quantum dot material Expect the application in display technology, the practical application of backlight especially in quantum dot TV.
Currently, perovskite quantum dot mainly include the following types: hot injection method, supersaturated crystallisation, tip ultrasonic method are micro- Emulsion method, solvent-thermal method, microfluidic method.Part preparation method due to need at high temperature (120 DEG C~200 DEG C) progress, It is not suitable for the preparation of organic inorganic hybridization perovskite quantum dot, because organic amine group can decompose at high temperature, so as to cause Product is impure.In addition, complicated synthesis step also limits its application in actual production.
In conclusion the present invention proposes a kind of novel perovskite Syntheses method, synthesis step is simple, product hair Optical property is good, and quantum yield is high, and the nanocrystalline preparation of popular perovskite most of at present may be implemented.
Summary of the invention
Present invention is directed to the excessively simple preparations of one kind that is complicated and designing of the nanocrystalline synthesis step of current perovskite Method.It realizes to studying the most commonly used nanocrystalline CsPbX of full-inorganic perovskite recently3And organic inorganic hybridization perovskite MAPbX3, FAPbX3Preparation.Preparation step is simple, has a wide range of application, and product has preferable luminescent properties, higher quantum Yield, high spectrum coverage rate, narrow halfwidth.Organic inorganic hybridization perovskite MAPbX is synthesized with preparation3(X=Cl, Br, I) For, by adjusting the ratio of halogen, emission spectra can regulate and control between 750nm in 400nm, realize to visible light All standing, meanwhile, MAPbBr3Quantum yield reached 90% or more, halfwidth only has 25nm.
The present invention is achieved through the following technical solutions:
Two kinds of organic inorganic hybridization perovskite quantum dots and a kind of full-inorganic perovskite quantum dot, specific general formula are as follows:
APbX3(A=MA, FA, Cs).Wherein MA and FA is a kind of organic group of positive monovalence of band, and chemical formula is respectively CH3NH3With CH (NH2)2, X is negative the halogen atom of monovalence, can be Cl, Br, I or their mixture C l/Br, Br/ I, cannot have a Cl/I, mixing be because the radius of Cl ion and I ion has big difference and leads to the unstable of perovskite structure, Prevent the structure is from existing.
Perovskite quantum dot according to the present invention, it is characterised in that particle size is in Nano grade, large specific surface area, Actual element proportion is different from macroscopic view block A:Pb:X=1:1:3, and what it is due to particle surface enrichment is halogen atom, phase Corresponding is that the location A monovalent cation in octahedral interstices reduces naturally than regular meeting.
Perovskite quantum dot according to the present invention, AX:PbX2=0.7~0.9:1 be it is best, preferably AX be 1.6mmol~ 2mmol, preferably PbX2For 1.8mmol~2.2mmol.
The main object of the present invention is to provide a kind of preparation method of easy perovskite quantum dot, the multicolor luminous calcium titanium Mine quantum dot can realize full spectrum transmitting under burst of ultraviolel.This method process is simple, and the method is grinding preparation Method.This method is specifically:
(1) with AX (A=MA, FA, Cs), PbX2For raw material, is weighed by certain mol ratio, be added to agate mortar In, it is fully ground；
MAPbX3: 1~2.5mmolMAX, 1.5~3mmolPbX2, 0.1~0.2ml oleic acid, 0.01ml~0.05ml oleyl amine；
FAPbX3: 1~2.5mmolFAX, 1.5~3mmolPbX2, 0.1~0.2ml oleic acid, 0.01ml~0.05ml oleyl amine；
CsPbX3: 1~2.5mmolCsX, 1.5~3mmolPbX2, 0.1~0.2ml oleic acid, 0.01ml~0.05ml oleyl amine.
According to the present invention, the preferred content of each component is as follows:
MAX is preferably 1.6mmol~2mmol, and FAX is preferably 1.6mmol~2mmol；
CsX is preferably 1.6mmol~2mmol, PbX2Preferably 1.8mmol~2.2mmol.
(2) suitable surfactant is added again to continue to grind, while needing to be added nonpolarity or low pole and easily waving The solvent of hair increases the efficiency of grinding；
(3) prepared perovskite quantum dot is collected finally by hexamethylene is added.
MA and FA is a kind of organic group of positive monovalence of band, and chemical formula is respectively CH3NH3With CH (NH2)2。
AX and PbX2X be negative the halogen atom of monovalence, is respectively independently Cl, Br or I；AX and PbX2X can take it is the same Halogen atom, can also be different that (such as Cl/Br, Br/I, cannot have Cl/I, because the radius of Cl ion and I ion differs It is excessive and lead to the unstable of perovskite structure).
The surfactant is oleic acid, oleyl amine.
According to the present invention, the content of oleic acid is 0.1~0.2ml, preferably 0.15~0.2ml.The content of oleyl amine is 0.01ml~0.05ml, preferably 0.03~0.04ml.
According to the present invention, it needs to be fully ground before surfactant being added, mixes powder uniformly.
Step (1) milling time is 10~30min, preferably 20~30min
The nonpolarity or low pole and volatile solvent are hexamethylene or toluene.Solvent needs persistently to add Enter, so that system is maintained at a kind of sticky state, the efficiency of grinding can be increased.
Step (2) milling time is 1h~3h, preferably 2~3h.
AX (A=MA, FA, Cs) can use cesium carbonate (source Cs), cesium acetate (source Cs), Formamidine acetate (source FA), methylamine bromine (source MA) etc. replaces.
In the present invention, using the above material component and preparation process, colorful light-emitting quantum dot can get.In the purple of 365nm Under the excitation of outer light, centre of luminescence wavelength is in 400nm to adjustable between 750nm.Since perovskite quantum dot has wider excitation Spectrum, exciting light are not limited only to 365nm.
In addition to it is some prepare surfactant necessary to quantum dot other than, the method for the present invention only uses a kind of solvent, just It is hexamethylene, no pollution to the environment, and volatile, easily recycling.And other methods can then use octadecylene, nitrogen-nitrogen dimethyl methyl Amide, toluene equal solvent, wherein octadecylene is Long carbon chain macromolecule, and hardly possible recycling, nitrogen-nitrogen dimethylformamide and toluene then have Hypotoxicity.
The principle of the method for the present invention and other prior arts have essential difference, other prior art majorities are based on knot Dissolution of raw material is first become ion, then makes its crystallization by specific mode, and controls its particle size by crystallization, This is a kind of synthesis mode from bottom to top.And the method for the present invention is then spread based on the ion under macrostate, ion is being spread It is formed after perovskite crystal, so that its particle is gradually reduced and (is spread and reduce particle in other words while carrying out) with grinding, due to Raw material and product it is ionic higher, therefore be very easy to carry out ion diffusion, this be a kind of top-down synthesis mode.
The method of the present invention is very easy, and repeatability is high, and can be used for producing in enormous quantities.
Detailed description of the invention
Fig. 1 is MAPbBr in example 13The TEM map of perovskite quantum dot；
Fig. 2 is MAPbX in example 1~53Fluorescence spectra of the perovskite quantum dot under the excitation of 365nm wavelength；
Fig. 3 is MAPbX in example 1~53The X ray diffracting spectrum of perovskite quantum dot；
Specific embodiment
Below will by specific embodiment, the present invention will be described in detail, but skilled in the art realises that, Xia Shushi Applying example is not limiting the scope of the invention, and any improvements and changes made on the basis of the present invention are all of the invention Within protection scope.
Embodiment 1:
By following proportion 0.16mmolMABr, 0.2mmolPbBr2Accurate weighing is placed in agate mortar, and is ground 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, and appropriate grinding is uniform, accurate measuring 1ml ring Hexane is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, repeats above-mentioned plus hexamethylene and grinding Step 5~7 time.4ml hexamethylene is added into mortar and collects prepared perovskite quantum dot.Purple of the quantum dot in 365nm Under outer light excitation, bright green, central wavelength 522nm is presented.
Fig. 1 is MAPbBr in example 13The TEM map of perovskite quantum dot；The particle size of the quantum dot of this method preparation For 20~30nm.
Embodiment 2:
By following proportion 0.16mmolMACl, 0.2mmolPbCl2Accurate weighing is placed in agate mortar, and is ground 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, and appropriate grinding is uniform, accurate measuring 1ml ring Hexane is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, repeats above-mentioned plus hexamethylene and grinding Step 5~7 time.4ml hexamethylene is added into mortar and collects prepared perovskite quantum dot.Purple of the quantum dot in 365nm Under outer light excitation, light purple, central wavelength 408nm is presented.
Embodiment 3:
By following proportion 0.16mmolMAI, 0.2mmolPbI2Accurate weighing is placed in agate mortar, and is ground 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, and appropriate grinding is uniform, accurate measuring 1ml ring Hexane is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, repeats above-mentioned plus hexamethylene and grinding Step 5~7 time.4ml hexamethylene is added into mortar and collects prepared perovskite quantum dot.Purple of the quantum dot in 365nm Under outer light excitation, peony, central wavelength 758nm is presented.
Embodiment 4:
By following proportion 0.08mmolMABr, 0.08mmolMACl, 0.1mmolPbBr2, 0.1mmolPbCl2Accurate weighing It is placed in agate mortar, and grinds 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, fit When grinding is uniform, accurate measuring 1ml hexamethylene is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, Repeat above-mentioned plus hexamethylene and grinding steps 5~7 times.4ml hexamethylene is added into mortar and collects prepared perovskite amount Sub- point.Blue, central wavelength 475nm is presented under the ultraviolet excitation of 365nm in the quantum dot.
Embodiment 5:
By following proportion 0.08mmolMABr, 0.08mmolMAI, 0.1mmolPbBr2, 0.1mmolPbI2After accurate weighing It is placed in agate mortar, and grinds 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, suitably Uniformly, accurate measuring 1ml hexamethylene is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time for grinding, weight It is above-mentioned again to add hexamethylene and grinding steps 5~7 times.4ml hexamethylene is added into mortar and collects prepared perovskite quantum Point.Orange, central wavelength 648nm is presented under the ultraviolet excitation of 365nm in the quantum dot.
Fig. 2 is MAPbX in example 1~53Fluorescence spectra of the perovskite quantum dot under the excitation of 365nm wavelength；Pass through tune The ratio of halogen is saved, emission wavelength can be adjusted between 408~758nm.
Fig. 3 is MAPbX in example 1~53The X ray diffracting spectrum of perovskite quantum dot；Due to the area of halogen atom radius Not (Cl < Br < I), the XRD spectrum of MAPbX3 moves, and rule is, when the small halogen of radius increases, XRD spectrum can be toward greatly Angle direction is mobile, conversely, XRD spectrum can be mobile toward low-angle direction when the big halogen of radius increases.
Embodiment 6-16 is as shown in Table 1, and on the basis of being altered to the selection of 1 raw material of embodiment, other experiment conditions are not Become, FAPbX is prepared3Perovskite quantum dot.Due to FA group radius (R (FA+)=0.19~0.22nm) it is significantly larger than MA (R (MA+)=0.18nm) group radius, FA group is more likely to enter in the bigger gap of lattice constant.Therefore, match in raw material It is different from MAPbX than upper outline3The proportion of perovskite quantum dot.
Table one
Embodiment 17:
By following proportion 0.16mmolCsBr, 0.2mmolPbBr2Accurate weighing is placed in agate mortar, and is ground 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, and appropriate grinding is uniform, accurate measuring 1ml ring Hexane is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, repeats above-mentioned plus hexamethylene and grinding Step 5~7 time.4ml hexamethylene is added into mortar and collects prepared perovskite quantum dot.Purple of the quantum dot in 365nm Under outer light excitation, bright green, central wavelength 518nm is presented.
Embodiment 18:
By following proportion 0.16mmolCsCl, 0.2mmolPbCl2Accurate weighing is placed in agate mortar, and is ground 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, and appropriate grinding is uniform, accurate measuring 1ml ring Hexane is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, repeats above-mentioned plus hexamethylene and grinding Step 5~7 time.4ml hexamethylene is added into mortar and collects prepared perovskite quantum dot.Purple of the quantum dot in 365nm Under outer light excitation, light purple, central wavelength 404nm is presented.
Embodiment 19:
By following proportion 0.16mmolCsI, 0.2mmolPbI2Accurate weighing is placed in agate mortar, and is ground 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, and appropriate grinding is uniform, accurate measuring 1ml ring Hexane is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, repeats above-mentioned plus hexamethylene and grinding Step 5~7 time.4ml hexamethylene is added into mortar and collects prepared perovskite quantum dot.Purple of the quantum dot in 365nm Under outer light excitation, red, central wavelength 670nm is presented.
Embodiment 20:
By following proportion 0.08mmolCsBr, 0.08mmolCsCl, 0.1mmolPbBr2, 0.1mmolPbCl2Accurate weighing It is placed in agate mortar, and grinds 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, fit When grinding is uniform, accurate measuring 1ml hexamethylene is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time, Repeat above-mentioned plus hexamethylene and grinding steps 5~7 times.4ml hexamethylene is added into mortar and collects prepared perovskite amount Sub- point.Blue-green, central wavelength 488nm is presented under the ultraviolet excitation of 365nm in the quantum dot.
Embodiment 21:
By following proportion 0.053mmolCsBr, 0.107mmolCsCl, 0.67mmolPbBr2, 0.133mmolPbCl2Accurately Weighing is placed in agate mortar, and grinds 20min, and above-mentioned mortar is added in accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine In, uniformly, accurate measuring 1ml hexamethylene is added in above-mentioned mortar, and grinds 20min, and hexamethylene is complete at this time for appropriate grinding Volatilization repeats above-mentioned plus hexamethylene and grinding steps 5~7 times.4ml hexamethylene is added into mortar and collects prepared calcium titanium Mine quantum dot.Blue, central wavelength 443nm is presented under the ultraviolet excitation of 365nm in the quantum dot.
Embodiment 22:
By following proportion 0.08mmolCsBr, 0.08mmolCsI, 0.1mmolPbBr2, 0.1mmolPbI2After accurate weighing It is placed in agate mortar, and grinds 20min, accurate measuring 0.15ml oleic acid and 0.03ml oleyl amine are added in above-mentioned mortar, suitably Uniformly, accurate measuring 1ml hexamethylene is added in above-mentioned mortar, and grinds 20min, and hexamethylene volatilizees completely at this time for grinding, weight It is above-mentioned again to add hexamethylene and grinding steps 5~7 times.4ml hexamethylene is added into mortar and collects prepared perovskite quantum Point.Orange-yellow, central wavelength 588nm is presented under the ultraviolet excitation of 365nm in the quantum dot.

Claims (8)

1. the polishing preparation process of perovskite quantum dot, the perovskite quantum dot can realize full spectrum hair under burst of ultraviolel It penetrates, it is characterised in that this method is based on the ion diffusion under macrostate, and ion is after diffuseing to form perovskite crystal, with grinding It is gradually reduced its particle, specifically:
(1) with AX (A=MA, FA, Cs), PbX2For raw material, weighs, be added in agate mortar, sufficiently by certain mol ratio Grinding；
AX and PbX2Mol ratio be 0.7~0.9:1；
MA and FA is a kind of organic group of positive monovalence of band, and chemical formula is respectively CH3NH3With CH (NH2)2；
AX and PbX2X be negative the halogen atom of monovalence, is respectively independently Cl, Br or I；
Step (1) milling time is 10~30min；
(2) continue to grind adding suitable surfactant again among the above, at the same need to be added nonpolarity or low pole and Volatile solvent increases the efficiency of grinding；
Step (2) milling time is 1h~3h；
(3) prepared perovskite quantum dot is collected finally by hexamethylene is added.
2. the polishing preparation process of perovskite quantum dot as described in claim 1, it is characterised in that the surface-active Agent is oleic acid, oleyl amine.
3. the polishing preparation process of perovskite quantum dot as described in claim 1, it is characterised in that step (1) milling time For 20~30min.
4. the polishing preparation process of perovskite quantum dot as described in claim 1, it is characterised in that nothing described in step (2) Polarity or low pole and volatile solvent are hexamethylene or toluene；Solvent needs are continuously added into, so that system is maintained at Viscous pasty state increases the efficiency of grinding.
5. the polishing preparation process of perovskite quantum dot as described in claim 1, it is characterised in that step (2) milling time For 2~3h.
6. the polishing preparation process of perovskite quantum dot as described in claim 1, it is characterised in that AX (A=MA, FA, Cs) Cesium carbonate (source Cs) can be used, cesium acetate (source Cs), Formamidine acetate (source FA), methylamine bromine (source MA) replaces.
7. the polishing preparation process of the perovskite quantum dot as described in claim 1-6 is any, it is characterised in that be prepared Perovskite quantum dot under the ultraviolet excitation of 365nm, centre of luminescence wavelength is in 400nm to adjustable between 750nm.
8. the polishing preparation process of the perovskite quantum dot as described in claim 1-6 is any, it is characterised in that be prepared Application of the perovskite quantum dot in TV backlight.
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CN109777403A (en) * 2019-03-14 2019-05-21 吉林大学 A kind of high fluorescence efficiency Cs2AgxNa1-xInCl6The preparation method of Double Perovskite
CN109880618A (en) * 2019-03-14 2019-06-14 吉林大学 A kind of high fluorescence efficiency Mn doping Cs2AgInCl6Synthetic method
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CN110862103B (en) * 2019-12-03 2021-07-06 吉林大学 High-efficiency synthetic Cs2AgBr3Method for preparing lead-free inorganic perovskite
CN110790300A (en) * 2019-12-09 2020-02-14 吉林大学 Simple and efficient synthetic Cs2AgI3Method for perovskite
CN110790299A (en) * 2019-12-09 2020-02-14 吉林大学 Simply synthesized CsAg2I3Method for pure-phase inorganic non-lead perovskite
CN111233031A (en) * 2020-01-19 2020-06-05 国家纳米科学中心 Perovskite quantum dot and preparation method thereof
CN111233031B (en) * 2020-01-19 2022-08-02 国家纳米科学中心 Perovskite quantum dot and preparation method thereof
CN113105882A (en) * 2020-12-14 2021-07-13 中国计量大学上虞高等研究院有限公司 CsPbI for improving stability3Nanocrystalline composite material and preparation method thereof
CN113105882B (en) * 2020-12-14 2022-05-24 中国计量大学上虞高等研究院有限公司 CsPbI for improving stability3Nanocrystalline composite material and preparation method thereof

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Application publication date: 20190104