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Technology for preparing all-inorganic perovskite nanocrystals by using high-energy ball milling method

A technology of high-energy ball milling and nanocrystals, applied in the direction of inorganic chemistry, chemical instruments and methods, lead compounds, etc., can solve problems such as complexity, poor product repeatability, and many factors, and achieve simple process flow, reduced Pb content, and wide sources of raw materials Effect

Pending Publication Date: 2021-11-23
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using the thermal injection method to synthesize nanocrystals, the reaction process needs to be under the protection environment of high temperature and inert gas, and after injecting the precursor solution, the temperature is difficult to control, resulting in poor product repeatability. In large-scale industrial production, this problem Especially prominent; the supersaturated recrystallization method at room temperature is too fast to cause the size uniformity and crystallinity of the synthesized nanocrystals to be poor. The growth process and further adjustment of its luminescent properties, and the stability of the synthesized nanocrystals is poor; the anion exchange method cannot realize the complete exchange of halide ions, the repeatability is poor, and the stability of the synthesized mixed halogen perovskite is poor, especially sensitive to light
In addition, researchers have developed many other synthetic CsPbX 3 Liquid-phase methods for nanocrystals, such as microwave, microfluidic, and solvothermal methods, but all liquid-phase methods are used in the synthesis of CsPbX 3 There are many and complicated factors in the process, it is difficult to realize the repeatable and batch preparation of high-quality nanocrystals, and it is inevitable to use a large amount of organic polar solvents, so the resulting environmental problems have also attracted the attention of researchers.

Method used

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  • Technology for preparing all-inorganic perovskite nanocrystals by using high-energy ball milling method
  • Technology for preparing all-inorganic perovskite nanocrystals by using high-energy ball milling method
  • Technology for preparing all-inorganic perovskite nanocrystals by using high-energy ball milling method

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Effect test

Embodiment 1

[0043] Such as figure 1 Shown, a kind of technology that utilizes the method for high-energy ball milling to prepare all-inorganic perovskite nanocrystals, the chemical formula of described all-inorganic perovskite nanocrystals is CsPbBr 3 ;

[0044] CbBr 3 The preparation process comprises the following steps:

[0045] 1) Weighing: according to CsPbBr 3 The chemical formula of weighing raw material CsBr, PbBr 2 , CsBr, PbBr 2 Weigh 5 mmol in average; the weighed raw materials are vacuum-dried at 60° C. for 1 to 2 hours.

[0046] 2) The first ball mill: the weighed CsBr, PbBr 2 Put it into a ball mill jar, add grinding balls (the ratio of ball to material is 3.5:1) to carry out the first ball mill; the ball mill time of the first ball mill is 5min, and the ball mill speed is 1000rpm.

[0047] 3) The second ball milling: after the first ball milling, add 0.4mL oleylamine into the ball milling tank and then carry out the second ball milling; the milling time of the second...

Embodiment 2

[0055] A process for preparing all-inorganic perovskite nanocrystals by means of high-energy ball milling, wherein the chemical formula of the all-inorganic perovskite nanocrystals is CsPb 2 Br 5 ;

[0056] According to the step 1) of embodiment 1) to step 6) preparation obtains CsPbBr 3 Nanocrystalline finished product, the CsPbBr 3 The nanocrystalline finished product was soaked in water for 8 hours, transferred to a centrifuge tube for centrifugation; after centrifugation, the supernatant was discarded, and the obtained precipitate was vacuum-dried and ground to obtain CsPb 2 Br 5 Nanocrystalline finished product.

[0057] The CsPb that this embodiment obtains 2 Br 5 The fluorescence quantum yield of nanocrystals is 92%.

Embodiment 3

[0059] A process for preparing all-inorganic perovskite nanocrystals by means of high-energy ball milling, the chemical formula of the all-inorganic perovskite nanocrystals is CsPbBr 3 ;

[0060] CbBr 3 The preparation process comprises the following steps:

[0061] 1) Weighing: according to CsPbBr 3 The chemical formula of weighing raw material CsBr, PbBr 2 , CsBr, PbBr 2 Weigh 5 mmol in average; the weighed raw materials are vacuum-dried at 60° C. for 1 to 2 hours.

[0062] 2) The first ball mill: the weighed CsBr, PbBr 2 Put it into a ball mill jar, add grinding balls (the ratio of ball to material is 3.5:1) to carry out the first ball mill; the ball mill time of the first ball mill is 5min, and the ball mill speed is 1000rpm.

[0063] 3) The second ball milling: after the first ball milling, add 0.5mL oleylamine into the ball milling tank and then carry out the second ball milling; the milling time of the second ball milling is 20min, and the ball milling speed is 10...

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Abstract

The invention relates to the technical field of nano material preparation, and discloses a technology for preparing all-inorganic perovskite nanocrystals by using a high-energy ball milling method. The chemical formula of the all-inorganic perovskite nanocrystals is CsaMbXc. The preparation technology comprises the following steps: weighing, first-time ball milling, second-time ball milling, cleaning, centrifuging, drying and grinding. The CsPbX3 nanocrystals with excellent luminescence performance are prepared by adopting the high-energy ball milling method, and the finished product has good crystallinity, uniformity and luminescence; the low-lead or lead-free multi-doped CsMX3 nanocrystal is synthesized by introducing ions such as Mn<2+>, Ni<2+>, Cu<2+>, Cd<2+>, Zn<2+>, Sn<2+> and Fe<2+> to replace Pb<2+>, so that the content of Pb in the material is effectively reduced; and the technology is simple in technological process, high in repeatability, small in pollution in the production process, low in energy consumption, wide in raw material source, capable of achieving batch production and high in economic benefit.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a process for preparing all-inorganic perovskite nanocrystals by using a high-energy ball milling method. Background technique [0002] In recent years, a new type of all-inorganic lead halide perovskite nanocrystals has been extensively studied. Due to its excellent optical properties, it has attracted great attention in the field of optoelectronics, such as backlight displays, solar cells, and photodetectors. and fluorescent probes. At present, the synthesis of all inorganic lead halide perovskite CsPbX at home and abroad 3 (X=Cl ― 、Br ― , I ― ) The methods of nanocrystals are mainly liquid phase methods, such as high temperature hot injection method, room temperature supersaturated recrystallization method, anion exchange method, etc. When using the thermal injection method to synthesize nanocrystals, the reaction process needs to be under the protection ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G21/00C01G21/16C09K11/66B02C17/00B02C17/18
CPCC01G21/006C01G21/16C09K11/664B02C17/00B02C17/18C01P2002/72C01P2002/80C01P2004/04C01P2002/34
Inventor 卢红霞王磊李俊辉姜欣李翼卞长路毛恒彬邵刚范冰冰王海龙许红亮张锐
Owner ZHENGZHOU UNIV
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