Preparation method of small-size high-stability perovskite nanocrystalline Cs4PbBr6

A high-stability, perovskite technology, applied in the field of synthesis of Cs4PbX6 perovskite nanocrystals, can solve the problems of poor monodispersity and stability, cannot be obtained, and is not ideal enough to achieve good stability and regular morphology , the effect of rapid response

Inactive Publication Date: 2018-05-08
JILIN UNIV
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Problems solved by technology

This result is consistent with the previous Cs of the pure octadecylamine ligand 4 PbBr 6 Compared with the stability has been greatly improved, but still not ideal
Now, the direct synthesis of Cs 4 PbBr 6 Nanoparticles have been achieved, but due to the use of thermal injection, it is not possible to obtain small-sized Cs 4 PbBr 6 Nanoparticles
However, if the existing post-synthesis method, that is, the crystal conve...

Method used

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  • Preparation method of small-size high-stability perovskite nanocrystalline Cs4PbBr6
  • Preparation method of small-size high-stability perovskite nanocrystalline Cs4PbBr6
  • Preparation method of small-size high-stability perovskite nanocrystalline Cs4PbBr6

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Experimental program
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Effect test

Embodiment 1

[0027] First, a cesium oleate solution is prepared. Take 2mmol (0.6516g) of cesium carbonate powder, 8.78mmol (2.5mL) of OA (oleic acid) and 17.5mL of ODE (octadecene) and mix them, heat to 150°C under nitrogen protection to dissolve cesium carbonate, and prepare 0.2mol / L cesium oleate solution is light yellow and transparent. Take out the cesium carbonate solution while it is hot and set aside. Since the cesium carbonate octadecene solution will solidify below 100°C, it needs to be heated to 100°C to dissolve it before each use.

[0028] Then take 0.2mmol of lead bromide solid powder, 0.5mL of oleylamine, 0.5mL of oleic acid and 3mL of octadecene into a three-necked flask, vacuumize at 120°C for 30 minutes, fill with nitrogen protection, and then heat up to 140°C. After the lead bromide is dissolved, inject 0.2 mL of 0.2 mol / L cesium oleate octadecene solution heated and melted in advance, and react to obtain CsPbBr with an absorption peak at 452 nm (3.8 nm in size) 3 Pero...

Embodiment 2

[0031] First, a cesium oleate solution is prepared. Take 2mmol (0.6516g) of cesium carbonate powder, 8.78mmol (2.5mL) of OA (oleic acid) and 17.5mL of ODE (octadecene) and mix them, heat to 150°C under nitrogen protection to dissolve cesium carbonate, and prepare 0.2mol / L cesium oleate solution is light yellow and transparent. Take out the cesium carbonate solution while it is hot and set aside. Since the cesium carbonate octadecene solution will solidify below 100°C, it needs to be heated to 100°C to dissolve it before each use.

[0032] Then take 0.2mmol of lead bromide solid powder, 0.5mL of oleylamine, 0.5mL of oleic acid and 3mL of octadecene into a three-necked flask, vacuumize at 120°C for 30 minutes, fill with nitrogen protection, and then heat up to 140°C. After the lead bromide is dissolved, inject 0.2 mL of 0.2 mol / L cesium oleate octadecene solution heated and melted in advance, and react to obtain CsPbBr with an absorption peak at 452 nm (3.8 nm in size) 3 Pero...

Embodiment 3

[0035] First, a cesium oleate solution is prepared. Take 2mmol (0.6516g) of cesium carbonate powder, 8.78mmol (2.5mL) of OA (oleic acid) and 17.5mL of ODE (octadecene) and mix them, heat to 150°C under nitrogen protection to dissolve cesium carbonate, and prepare 0.2mol / L cesium oleate solution is light yellow and transparent. Take out the cesium carbonate solution while it is hot and set aside. Since the cesium carbonate octadecene solution will solidify below 100°C, it needs to be heated to 100°C to dissolve it before each use.

[0036] Then take 0.2mmol of lead bromide solid powder, 0.5mL of oleylamine, 0.5mL of oleic acid and 3mL of octadecene into a three-necked flask, vacuumize at 120°C for 30 minutes, fill with nitrogen protection, and then heat up to 140°C. After the lead bromide is dissolved, inject 0.2 mL of 0.2 mol / L cesium oleate octadecene solution heated and melted in advance, and react to obtain CsPbBr with an absorption peak at 452 nm (3.8 nm in size) 3 Pero...

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Abstract

The invention relates to a preparation method of a small-size high-stability perovskite nanocrystalline Cs4PbBr6, and belongs to the technical field of preparation of semiconductor nanomaterials. Thepreparation method comprises the following steps: firstly injecting a caesium carboxylate solution into a lead bromide solution at the temperature of 140 DEG C to 200 DEG C under the protection of N2,reacting, synthesizing a perovskite nano-block CsPbBr3 with the size of 3.8 nm to 11.8 nm, purifying the perovskite nano-block CsPbBr3, dispersing the perovskite nano-block CsPbBr3 by using octadecene, raising the temperature to 25 DEG C to 120 DEG C, injecting an ammonium bromide solution, reacting for 3-8 minutes, then centrifuging and purifying to obtain a nanoparticle Cs4PbBr6. The preparation method has the characteristics of easy operation, simple steps and rapid reaction, the raw materials are easy to get, the prepared particles Cs4PbBr6 are uniform in size, regular in morphology and excellent in stability, and the particle keeps unchanged even after a stock solution is placed in the air for a month.

Description

technical field [0001] The invention belongs to the technical field of semiconductor nanomaterial preparation, in particular to a Cs with small size and high stability 4 wxya 6 Synthesis of perovskite nanocrystals. Background technique [0002] As an emerging discipline, nanotechnology has changed from a beautiful idea of ​​scientists to a technology that can actually benefit mankind after more than 30 years of development. Semiconductor nanomaterials have always been a hot spot in the field of nanomaterials research. The unique feature of semiconductor nanocrystals is that their size range is limited between 1 and 100 nm. When the size of semiconductor materials is reduced from the macroscopic bulk phase to the nanoscale, the energy band structure will change, and some unique physical and chemical Nature also follows. Such as quantum size effect, surface effect, small size effect, macroscopic quantum tunneling effect, etc. [0003] In recent years, organic-inorganic mi...

Claims

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Application Information

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IPC IPC(8): C01G21/16B82Y40/00
CPCB82Y40/00C01G21/16C01P2002/72C01P2002/82C01P2004/04C01P2004/64
Inventor 李军耿敬解仁国张颖杨文胜
Owner JILIN UNIV
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