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A kind of preparation method of lead halide perovskite

A perovskite and powder technology, applied in chemical instruments and methods, lead compounds, inorganic chemistry, etc., can solve problems such as difficulties in lead halide perovskite, and achieve the effects of avoiding difficult operation, diverse three-dimensional structures, and economical preparation methods

Active Publication Date: 2020-11-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the difficult problem of preparing micron-scale three-dimensional complex structure lead halide perovskite, and propose a three-dimensional self-assembled lead halide perovskite as a template, in situ transformation to prepare lead halide perovskite, especially micron-scale three-dimensional The method of structural lead halide perovskite, and for the first time revealed the rich self-assembly behavior of lead halide in the oil phase solution system and the factors affecting the growth of lead halide, making the three-dimensional self-assembled lead halide system [ Pb(OH)X, X=Cl - ,Br - ,I - etc.] can be transformed into three-dimensional lead halide perovskite materials with different microscopic morphologies

Method used

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  • A kind of preparation method of lead halide perovskite
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  • A kind of preparation method of lead halide perovskite

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The preparation process of Pb(OH)Br is as follows figure 1Shown in b: (1) At room temperature, weigh 4 parts of 0.1101g PbBr 2 The powders were dissolved in 1.5mL N,N-dimethylformamide (DMF), and after stirring vigorously for 3min, the solution was clear, which were recorded as A1, B1, C1 and D1, and then 150μL oleic acid (OA ), 10 μL oleylamine (OAM), add 75 μL oleic acid and 75 μL oleylamine to B1 in sequence, add 150 μL oleic acid and 75 μL oleylamine to C1 in sequence, add 150 μL oleic acid and 1000 μL oleylamine to D1 in sequence, and continue stirring A clear solution was obtained.

[0027] (2) Use a pipette to measure 1.4 mL of the clear solutions of A1, B1, C1, and D1 in (1) above, and then quickly add them to 20 mL of toluene, stir vigorously for 10 minutes, and then let stand for 30 hours to obtain the mother liquor.

[0028] (3) After the mother liquors were transferred to centrifuge tubes, high-speed centrifugation was used at a speed of 7000 rpm for 5 min...

Embodiment 2

[0031] (1) At room temperature, weigh 0.1101g PbBr 2 Powder, dissolved in 1.5mL N,N-dimethylformamide (DMF). After vigorous stirring for 3 minutes, the solution was clear, and 150 μL oleic acid and 75 μL oleylamine were added in sequence, and the stirring was continued to obtain a clear solution.

[0032] (2) Use a pipette gun to measure 1.4 mL of the above clear solution, and then quickly add them to 20 mL of toluene respectively, stir vigorously for 10 s, and then let stand for 20 hours to obtain the mother liquor.

[0033] (3) After transferring the mother liquor to a centrifuge tube, use high-speed centrifugation at a speed of 7000 rpm for 5 minutes. Then the precipitate was washed several times with toluene to obtain the diplococcus-like micron-sized Pb(OH)Br self-assembled material.

[0034] Scanning electron microscopy shows that the Pb(OH)Br self-assembled material prepared by the above method has a uniform shape and size distribution, such as figure 2 as shown in ...

Embodiment 3

[0036] (1) At room temperature, weigh 0.1101g PbBr 2 Powder, dissolved in 1.5mL N,N-dimethylformamide (DMF). After vigorous stirring for 3 minutes, the solution was clear, and 150 μL oleic acid and 75 μL oleylamine were added in sequence, and the stirring was continued to obtain a clear solution.

[0037] (2) Use a pipette gun to measure 1.4mL of the above clear solution, and then quickly add them to 20mL of toluene respectively, stir vigorously for 30s, and let stand for 1min, 1h, 3, 10h and 24h respectively to obtain the mother liquor.

[0038] (3) After transferring the mother liquor to a centrifuge tube, use high-speed centrifugation at a speed of 7000 rpm for 5 minutes. Then the precipitate was washed several times with toluene to obtain Pb(OH)Br self-assembled materials under different growth times.

[0039] The Pb(OH)Br self-assembled materials obtained in the above examples under different growth times were tested by scanning electron microscopy to observe in detail ...

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Abstract

The invention discloses a method for preparing lead halide perovskite, and belongs to the field of lead halide perovskite. According to the method, a self-assembly behavior of hydroxy halide lead oresare regulated and controlled through regulation and control of the composition of ligands, so that hydroxy halide lead ore structures with different micron-sized microscopic shapes can be obtained; and then, Cs<+>, CH3NH3<+> or HC(NH2)2<+> ions are introduced by taking the structures as lead sources and templates, and lead halide perovskite materials with different structures can be obtained. Themethod is economical, simple and reliable, and the prepared lead halide perovskite materials have various three-dimensional structures and adjustable components.

Description

technical field [0001] The invention belongs to the field of lead halide perovskite, and in particular relates to a preparation method of lead halide perovskite. Background technique [0002] In recent years, lead-based halide perovskites (APbX 3 ) has attracted extensive attention in the fields of solar cells, LEDs, and photodetectors due to its unique properties such as high quantum efficiency, tunable band gap, and long carrier diffusion length. With the deepening of research, it has been found that lead halide perovskite micro-nanomaterials with three-dimensional complex structures have more fascinating physical properties, for example, CsPbBr 3 The micron-scale superlattice structure formed by stacking nanocubes has superfluorescence phenomenon. This discovery provides the possibility for the preparation of multi-photon entangled quantum light sources. However, although researchers have proposed methods such as surface ligand confinement (soft template) and hard templ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G21/00
CPCC01G21/006C01P2002/34C01P2002/72C01P2004/03C01P2004/61
Inventor 杨士宽余阳春侯嘉慧孙启升张玲惠
Owner ZHEJIANG UNIV