Preparation method of abx3 type all-inorganic perovskite nanocrystal

An inorganic calcium and nanocrystal technology, applied in inorganic chemistry, nanotechnology, nano-optics, etc., can solve the problems of high price, unsuitable for industrial production, and high cost

Active Publication Date: 2019-09-03
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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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 the 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 ind

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  • Preparation method of abx3 type all-inorganic perovskite nanocrystal
  • Preparation method of abx3 type all-inorganic perovskite nanocrystal
  • Preparation method of abx3 type all-inorganic perovskite nanocrystal

Examples

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Example Embodiment

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

[0065] Weigh 0.5mmol of lead acetate and 0.1mmol of cesium carbonate, then add 1mL of oleic acid, 1mL of oleylamine, 1mL of tri-n-octylphosphine and 10mL of octadecene, heat to 120℃ with nitrogen and keep it for 10 minutes to form a transparent solution A, then Warm up to 180°C; quickly inject 124μL of hydrochloric acid into solution A, keep it warm for 10 seconds, and quickly cool with an ice bath (cooling rate is about 10-15°C / sec) to room temperature; centrifuge first, 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 11.0nm 3 Perovskite quantum dots.

[0066] X-ray powder diffraction pattern ( figure 1 a) It shows that the quantum dot has good crystallinity, and its diffraction peak position and relative intensity are the same as the cubic phase CsPbCl 3 The PDF standard card (JCPDS NO.75-0411) is the same, belo...

Example Embodiment

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

[0068] Weigh 0.5mmol of lead oxalate, 0.2mmol of cesium acetate, and then add 1mL of oleic acid, 1mL of oleylamine, 1.5mL of tri-n-octylphosphine and 20mL of octadecene, and heat to 120℃ with nitrogen and keep it for 20 minutes to form a transparent solution A Then the temperature was raised to 200℃; 83μL of hydrochloric acid and 58μL of hydrogen bromide were quickly injected into solution A, kept for 5 seconds, and naturally cooled to room temperature; centrifuged and then washed with 10mL cyclohexane and 10mL acetone once, and 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) It shows that the quantum dot has good crystallinity, and its diffraction peak position and relative intensity are the same as the cubic phase CsPbCl 3 And CsPbBr 3 The PDF standard cards (JCPDS NO.75-041...

Example Embodiment

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

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

[0072] X-ray powder diffraction pattern ( figure 1 c) It shows that the quantum dot has good crystallinity, and its diffraction peak position and relative intensity are the same as the cubic phase CsPbCl 3 And CsPbBr 3 The PDF standard cards (JCPDS NO.75-0411 and 75-041...

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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 were heated and dissolved in a mixed solvent of oleic acid, oleylamine and octadecene to form a Pb oleic acid complex solution ...

Claims

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Application Information

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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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