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Perovskite CsPbX3 nanocrystal as well as preparation method and application thereof

A nanocrystal and titanium ore technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of precursor purity, demanding storage conditions, poor reproducibility of nanocrystal synthesis, and achieve easy process control, Improve luminous efficiency and reduce the effect of halogen vacancies

Active Publication Date: 2021-12-28
XIAMEN INST OF RARE EARTH MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in the existing preparation method, for PbX 2 Precursor purity and storage conditions are quite demanding, resulting in poor reproducibility of nanocrystal synthesis

Method used

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  • Perovskite CsPbX3 nanocrystal as well as preparation method and application thereof
  • Perovskite CsPbX3 nanocrystal as well as preparation method and application thereof
  • Perovskite CsPbX3 nanocrystal as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1: CsPbCl 3 Preparation of nanocrystals

[0055] Step 1. Take 5.0g of lead particles and 5mL of concentrated hydrochloric acid into a 25mL three-necked flask, heat the mixture to 80°C for 6h at 1000rpm, and cool to room temperature naturally to obtain a white precipitate. The white precipitate was washed 5 times with ether. Finally, dry under vacuum overnight at 60 °C to obtain HPbCl 3 .

[0056] Step 2. Add 0.814g of cesium carbonate, 20mL of octadecene and 2.5mL of oleic acid into a 50mL three-necked flask. Under a nitrogen atmosphere, heat the mixture to 110°C and keep the temperature for 60min to complete the cesium carbonate Dissolved, then naturally cooled to room temperature to form a precursor solution of cesium oleate.

[0057] Step 3, weigh 0.118g of HPbCl obtained in step 1 3 The powder was added to a three-necked flask containing 1 mL of oleic acid, 1 mL of oleylamine and 10 mL of octadecene, and stirred at 130 °C for 35 min under a nitrogen atm...

Embodiment 2

[0060] Example 2: CsPbBr 3 Preparation of nanocrystals

[0061] Step 1, take 5g PbBr respectively 2 , 5mL, 48wt% HBr aqueous solution and 10mL dimethylformamide were placed in a 25mL three-necked flask, and at 1000rpm, the mixture was heated to 80°C and kept at this temperature to react overnight, adding 5mL of absolute ethanol for precipitation, and then Cooling to room temperature gave a white precipitate. The white precipitate was washed 5 times with ether. Finally, vacuum drying at 60 °C overnight to obtain APbBr 3 Powder (A=H or DMA).

[0062] Step 2. Add 0.814g of cesium carbonate, 20mL of octadecene and 2.5mL of oleic acid into a 50mL three-necked flask. Under a nitrogen atmosphere, heat the mixture to 110°C and keep the temperature for 60min to complete the cesium carbonate Dissolved, then naturally cooled to room temperature to form a precursor solution of cesium oleate.

[0063] Step 3, weigh 0.168g APbBr obtained in step 1 3 The powder was added to a three-ne...

Embodiment 3

[0066] Example 3: CsPbBr 1.5 I 1.5 Preparation of nanocrystals

[0067] Step 1, a) take 5g PbBr 2 , 5mL, 48wt% HBr aqueous solution and 10mL dimethylformamide were placed in a 25mL three-necked flask, and at 1000rpm, the mixture was heated to 80°C and kept at this temperature to react overnight, adding 5mL of absolute ethanol for precipitation, and then Cooling to room temperature gave a white precipitate. The white precipitate was washed 5 times with ether. Finally, vacuum-dried at 60 °C overnight to obtain APbBr 3 (A=H or DMA). b) Take 5g PbI 2 , 5mL, 57wt% HI aqueous solution and 10mL dimethylformamide were placed in a 25mL three-necked flask, and at 1000rpm, the mixture was heated to 80°C and kept at this temperature for overnight reaction, and 5mL of absolute ethanol was added for precipitation, then naturally Cooling to room temperature gave a yellow precipitate. The yellow precipitate was washed 5 times with ether. Finally, dry in vacuum at 60 °C overnight to o...

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Abstract

The invention discloses a perovskite CsPbX3 nanocrystal as well as a preparation method and application thereof. The preparation method comprises the following steps: in an inert atmosphere, heating a metal halide APbX3 precursor solution with an equivalent stoichiometric ratio, where A is H and / or DMA ions, and X is one or more halogens; and adding the cesium precursor solution into the mixed solution, reacting and rapidly cooling to obtain the CsPbX3 nanocrystal. In the method, the APbX3 compound which is easy to prepare and store is adopted as a lead and halogen source, so that the synthesized CsPbX3 nanocrystal has few defects, the situation that a perovskite structure is degraded due to the influence of light, heat, oxygen and water due to halogen defects is avoided, excellent physical and chemical stability is shown, and the luminous efficiency of the nanocrystal is further improved. Besides, the raw materials are cheap and easy to obtain, preparation is simple, the obtained nanocrystals are more stable, experimental reproducibility is good, and the method is suitable for industrial popularization and preparation.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, in particular to a perovskite CsPbX 3 Nanocrystals and their preparation methods and applications. Background technique [0002] All inorganic lead halide perovskites (CsPbX 3 , X=Cl, Br, I) nanocrystals have high fluorescence quantum yield (~90%), narrow emission bandwidth (12-42nm), luminous wavelength covers the entire visible spectrum (400-700nm) and low-cost solution preparation, etc. It has developed rapidly in the fields of solar cells, light-emitting diodes, photodetectors and lasers, and has set off a research boom. Currently, synthetic CsPbX 3 There are two main categories of methods: thermal injection and ligand-assisted co-precipitation. However, in the existing preparation methods of perovskite nanocrystals, lead halide (ie PbX 2 , X = Cl, Br, I) as a common source of lead and halogen, resulting in a mismatch of lead and halogen stoichiometry with the target produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/14C30B29/10C01G21/00B82Y30/00B82Y40/00
CPCC30B7/14C30B29/10C01G21/00B82Y30/00B82Y40/00C01P2002/60C01P2004/64C01P2002/72C01P2004/52C01P2004/04C01P2002/85C01P2002/34
Inventor 朱浩淼陈德建
Owner XIAMEN INST OF RARE EARTH MATERIALS
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