Preparation method of CsPbBr3 spindle type perovskite micro-particles with adjustable size

A technology of micron particles and perovskite, applied in chemical instruments and methods, lead compounds, inorganic chemistry, etc., can solve the problem of continuous and precise control of material shape and size, control of perovskite micron particles, and small radiation recombination efficiency coefficient and other issues, to achieve the effect of adjusting the luminous lifetime, excellent photoelectric performance, and precisely controlling the shape

Active Publication Date: 2020-08-28
NANJING UNIV OF TECH
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  • Abstract
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  • Application Information

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Problems solved by technology

Currently, in order to improve perovskite CsPbX 3 Stability in the air and luminescent properties, researchers have studied and synthesized perovskite nanocrystals with various shapes such as nanoblocks, nanosheets and nanorods to control and improve the performance of materials, but the existing technology can obtain calcium Titanium CsPbX 3 The size of the material is in the nanometer scale, and these materials all have the problems of wide band gap, small radiation recombination efficiency coefficient, low color purity and short luminous lifetime, which seriously affect the photoelectric performance of the material; in addition, the prior art preparation The method cannot achieve continuous and precise control of the shape and size of the material, thereby realizing the control of the luminous lifetime and the luminous performance, and it is also impossible to control the CsPbBr with high luminous purity and adjustable luminous lifetime according to the luminous performance requirements of the product. 3 Perovskite Microparticles

Method used

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  • Preparation method of CsPbBr3 spindle type perovskite micro-particles with adjustable size
  • Preparation method of CsPbBr3 spindle type perovskite micro-particles with adjustable size
  • Preparation method of CsPbBr3 spindle type perovskite micro-particles with adjustable size

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Preparation of a size-tunable CsPbBr 3 Spindle-shaped perovskite micro-particles, the preparation method is as follows:

[0040] (1) Add 0.2g of cesium carbonate, 10ml of octadecene and 0.75ml of oleic acid into a 50ml round-bottomed flask in turn, heat up to 150°C under nitrogen protection and stir until completely dissolved, the solution is clear and transparent, and a spare solution is obtained, which is named as Solution 1;

[0041] (2) Add 0.1g of lead bromide, 10ml of octadecene, 1ml of oleylamine, and 0.2ml of 5-hexynoic acid into a 50ml round bottom flask and mix them. After mixing, stir at a constant temperature of 100°C under the protection of nitrogen until completely dissolved. At a temperature of 140°C, take 0.8ml of the spare solution 1 in step (1) and quickly inject it, stir for 5s and cool it to room temperature with an ice-water bath, put the cooled solution into a 50ml centrifuge tube, add absolute ethanol for washing, and ultrasonically Mix the solu...

Embodiment 2

[0045] Preparation of a size-tunable CsPbBr 3 Spindle-shaped perovskite micro-particles, the preparation method is as follows:

[0046] (1) Add 0.3g of cesium carbonate, 20ml of octadecene and 1.5ml of oleic acid into a 50ml round-bottomed flask in turn, heat up to 150°C under nitrogen protection and stir until completely dissolved, the solution is clear and transparent, and a spare solution is obtained, which is named as Solution 2;

[0047] (2) Add 0.2g of lead bromide, 20ml of octadecene, 3ml of oleylamine, and 0.4ml of 5-hexynoic acid into a 50ml round bottom flask and mix them. After mixing, stir at a constant temperature of 100°C under nitrogen protection until completely dissolved. At a temperature of 150°C, take 1.2ml of the spare solution 2 in step (1) and quickly inject it, stir for 5s and cool it to room temperature with an ice-water bath, put the cooled solution into a 50ml centrifuge tube, add absolute ethanol for washing, and ultrasonically Mix the solution eve...

Embodiment 3

[0051] Preparation of a size-tunable CsPbBr 3 Spindle-shaped perovskite micro-particles, the preparation method is as follows:

[0052] (1) Add 0.3g of cesium carbonate, 15ml of octadecene and 1.0ml of oleic acid into a 50ml round-bottomed flask in turn, raise the temperature to 150°C under the protection of nitrogen and stir until they are completely dissolved. The solution is clear and transparent, and a spare solution is obtained, named as Solution 3;

[0053] (2) Add 0.2g of lead bromide, 15ml of octadecene, 2ml of oleylamine, and 0.3ml of 5-hexynoic acid into a 50ml round bottom flask and mix them. After mixing, stir at a constant temperature of 110°C under nitrogen protection until completely dissolved. At a temperature of 140°C, take 1.0ml of the spare solution 3 in step (1) and quickly inject it, stir for 5s and cool it to room temperature with an ice-water bath, put the cooled solution into a 50ml centrifuge tube, add absolute ethanol for washing, and ultrasonically ...

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Abstract

The invention discloses a preparation method of CsPbBr3 spindle type perovskite micro-particles with an adjustable size. The preparation method comprises the following steps: firstly, by taking 5-hexynoic acid and 10-undecynoic acid as surface ligands, respectively preparing a 5-hexynoic acid CsPbBr3 perovskite nanocrystal solution and a 10-undecynoic acid CsPbBr3 perovskite nanocrystal solution;respectively mixing the 5-hexynoic acid CsPbBr3 perovskite nanocrystal solution and the 10-undecynoic acid CsPbBr3 perovskite nanocrystal solution according to different volume ratios to obtain mixedsolutions; and finally, reacting the mixed solutions under the irradiation of an ultraviolet lamp to obtain the CsPbBr3 spindle type perovskite micro-particles with different length-width ratios. Thepreparation method is simple, the CsPbBr3 spindle type perovskite micro-particles with higher luminous purity and adjustable luminous life can be prepared at one time; the spindle type perovskite CsPbBr3 micro-particles prepared by the method disclosed by the invention are adjustable in length-width ratio, smaller in band gap, narrow in light-emitting half-peak width, high in color purity, long inlight-emitting service life and excellent in photoelectric property.

Description

technical field [0001] The invention relates to the technical field of preparation of phosphorescent materials, more specifically, to a size-adjustable CsPbBr 3 Preparation method of spindle-shaped perovskite microparticles. Background technique [0002] All-inorganic halide perovskite CsPbX 3 (X=Cl, Br, I) quantum dots have been widely used in light-emitting diodes, solar cells, photodetectors and other fields since they were first reported in 2015. CaB 3 The material has many advantages. First, the halogen perovskite CsPbX 3 The half-peak width of the luminescence can easily reach below 20nm, and has ultra-high photoluminescence color purity. Second, CsPbX 3 The exciton Bohr radius of quantum dots is about 7nm. In theory, only when the particle size is smaller than or close to the exciton Bohr radius, the crystal grains will show obvious quantum confinement effect. Although the perovskite CsPbX 3 (X=Cl, Br, I) has become a rising star in the material world, but it i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G21/00C09K11/66C09K11/02
CPCC01G21/006C09K11/665C09K11/025C01P2004/03C01P2002/72C01P2006/60
Inventor 李红波英起飞刘向东黄岭
Owner NANJING UNIV OF TECH
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