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a kind of abx 3 Preparation method of type all-inorganic perovskite nanocrystal

A technology of inorganic calcium and nanocrystals, applied in inorganic chemistry, nanotechnology, nano-optics, etc., can solve the problems of large amount of solvent, high price, and unsuitable for industrial production.

Active Publication Date: 2020-11-20
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The advantage of this method is that the reaction can be carried out at room temperature, but PbX 2 and CsX have low solubility in DMF and / or DMSO, requiring a large amount of solvent to dissolve, and PbX 2 and CsX are expensive and therefore not suitable for industrial production
Although people have improved the synthesis on the basis of these two methods, such as microwave-assisted synthesis, ultrasonic-assisted synthesis, etc., the Pb sources used are all PbX 2 , and the amount of solvent used is large and the cost is high

Method used

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  • a kind of abx <sub>3</sub> Preparation method of type all-inorganic perovskite nanocrystal
  • a kind of abx <sub>3</sub> Preparation method of type all-inorganic perovskite nanocrystal
  • a kind of abx <sub>3</sub> Preparation method of type all-inorganic perovskite nanocrystal

Examples

Experimental program
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Effect test

Embodiment 1

[0064] Example 1: CsPbCl 3 Preparation of perovskite quantum dots.

[0065] Weigh 0.5mmol lead acetate and 0.1mmol cesium carbonate, then add 1mL oleic acid, 1mL oleylamine, 1mL tri-n-octylphosphine and 10mL octadecene, heat to 120°C with nitrogen gas and keep it warm for 10 minutes to form a transparent solution A, then Raise the temperature to 180°C; quickly inject 124 μL of hydrochloric acid into solution A, keep warm for 10 seconds, and quickly cool it in an ice bath (cooling rate is about 10-15°C / second) to room temperature; first centrifuge and then use 10mL cyclohexane and 10mL acetone Wash once, and disperse the precipitate in 30mL cyclohexane to obtain CsPbCl with a particle size of about 11.0 nm 3 Perovskite quantum dots.

[0066] X-ray powder diffraction pattern ( figure 1 a) shows that the quantum dots have good crystallinity, and the position and relative intensity of the diffraction peaks are the same as those of the cubic phase CsPbCl 3 The PDF standard card...

Embodiment 2

[0067] Example 2: CsPbCl 2 Preparation of Br perovskite quantum dots.

[0068] Weigh 0.5mmol lead oxalate and 0.2mmol cesium acetate, then add 1mL oleic acid, 1mL oleylamine, 1.5mL tri-n-octylphosphine and 20mL octadecene, heat to 120°C with nitrogen gas and keep it warm for 20 minutes to form a transparent solution A , and then warmed up to 200°C; quickly inject 83 μL of hydrochloric acid and 58 μL of hydrogen bromide into solution A, keep warm for 5 seconds, and cool down to room temperature; centrifuge and wash once with 10 mL of cyclohexane and 10 mL of acetone, and remove the precipitate Disperse in 30mL cyclohexane to obtain CsPbCl with a particle size of about 15.0nm 2 Br perovskite quantum dots.

[0069] X-ray powder diffraction pattern ( figure 1 b) shows that the quantum dots have good crystallinity, and the position and relative intensity of the diffraction peaks are the same as those of the cubic phase CsPbCl 3 and CsPbBr 3 The PDF standard cards (JCPDS NO.75-...

Embodiment 3

[0070] Example 3: CsPbCl 1.5 Br 1.5 Preparation of perovskite quantum dots.

[0071] Weigh 0.5mmol lead acetate and 0.05mmol cesium carbonate, then add 0.5mL oleic acid, 0.5mL oleylamine and 6mL octadecene, heat to 120°C with nitrogen gas and keep it warm for 30 minutes to form a transparent solution A, then raise the temperature to 190°C; Quickly inject 62 μL of hydrochloric acid and 87 μL of hydrogen bromide into solution A, keep warm for 5 seconds, and quickly cool to room temperature in an ice-water bath; centrifuge first, then wash once with 5 mL of cyclohexane and 5 mL of acetone, and disperse the precipitate in a 30 mL ring In hexane, CsPbCl with a particle size of about 13.0nm was obtained 1.5 Br 1.5 Perovskite quantum dots.

[0072] X-ray powder diffraction pattern ( figure 1 c) shows that the quantum dots have good crystallinity, and the position and relative intensity of the diffraction peaks are the same as those of the cubic phase CsPbCl 3 and CsPbBr 3 The ...

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Abstract

The invention discloses a preparation method of an ABX3 type all-inorganic perovskite nanocrystal. In the preparation process, a solvent is used in a small amount, and the raw material unit price is low (for example, an expensive PbX2 raw material is replaced by cheap lead acetate), environmental requirements are not high in the preparation process, a glove box is not required, the operation procedure is simple, and the cost of raw materials and instruments is greatly reduced. The nanocrystal can synthesize a target product in a wide temperature range of 0 to 300 DEG C in the preparation process, and the morphology, phase, size and luminous performance of the nanocrystal can be controlled by changing the raw material ratio, solvent ratio, reaction temperature and / or reaction time, for example, perovskite nanowires can be prepared at the reaction temperature of greater than or equal to 0 DEG C and less than 90 DEG C, and perovskite quantum dots can be prepared at the reaction temperature of 90 to 300 DEG C. The nanocrystal has good stability and high fluorescence quantum yield (26%-80%), and can realize full visible spectrum (400-700 nm) luminescence. The preparation method is simple in process, short in time consumption, low in cost, easy to amplify and synthesize, and suitable for industrial large-scale preparation.

Description

technical field [0001] The invention belongs to the technical field of nanocrystalline luminescent materials, in particular to an ABX 3 A method for preparing all-inorganic perovskite nanocrystals. Background technique [0002] All-inorganic perovskite nanocrystals (CsPbX 3 ,X=Cl,Br,I) has excellent optical properties such as large absorption cross section, high fluorescence quantum yield, and tunable fluorescence emission wavelength, and has shown great applications in optoelectronic devices such as solar cells, light-emitting diodes, and lasers. prospect. At present, there are mainly two methods for preparing all-inorganic perovskite nanocrystals: high-temperature injection method and normal temperature supersaturated recrystallization method. The high-temperature injection method is to separately inject PbX 2 and CsCO 3 The two raw materials are heated and dissolved in a mixed solvent of oleic acid, oleylamine and octadecene to form a Pb oleic acid complex solution a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/66B82Y20/00B82Y40/00C01G21/00
CPCB82Y20/00B82Y40/00C01G21/006C01P2002/72C09K11/665
Inventor 郑伟陈学元宫仲亮黄萍
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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