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Method for growing ABX3 perovskite single crystal by antisolvent diffusion

A perovskite, anti-solvent technology, applied in the directions of single crystal growth, crystal growth, single crystal growth, etc., can solve the problems of complex process and high equipment requirements, and achieve simple process, simple equipment requirements, and high raw material utilization. Effect

Inactive Publication Date: 2017-05-31
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of anti-solvent diffusion growth ABX 3 The method of perovskite single crystal aims to solve the problem that the preparation method of titanium ore single crystal has a relatively complicated process and high requirements for equipment

Method used

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  • Method for growing ABX3 perovskite single crystal by antisolvent diffusion
  • Method for growing ABX3 perovskite single crystal by antisolvent diffusion
  • Method for growing ABX3 perovskite single crystal by antisolvent diffusion

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Effect test

Embodiment 1

[0042] Anti-solvent diffusion growth ABX of the present invention 3 Perovskite single crystal, A is CH 3 NH 3 + 、H 2 N-CH=NH 2 + , (CH 3 ) 4 N + 、C 7 h 7 + 、Cs + 、C 3 h 11 SN 3 2+ One or more of, B is one or more of Pb, Ge, Sn; X is one or more of Cl, Br, I, and the specific method includes the following steps:

[0043] 1) Weigh one or more of the above-mentioned halogenated organic and inorganic substances containing A and one or more metal compounds containing B into a 100ml beaker that has been added with a stirring bar.

[0044] Among them, the A-containing halides contain organic or inorganic ions with a radius of One or more mixtures of organic or inorganic halogenated compounds, including chloromethylamine (CH 3 NH 3 Cl), chloroformamidine (H 2 N-CH=NH 2 Cl), tetramethylammonium chloride ((CH 3 ) 4 NCl), Chlorazolium (C 7 h 7 Cl), chlorinated 2-isothiourea (C 3 h 11 SN 3 Cl 2 ), methyl bromide (CH 3 NH 3 Br), formamidine bromide (H 2 N-C...

Embodiment 2

[0061] 1. Configure the precursor solution

[0062] Take by weighing 3.357g methyl bromide (CH 3 NH 3 Br), 11.01g lead bromide (PbBr 2 ) into a 100ml beaker with a stirring bar, add 30ml N,N-dimethylformamide (DMF), seal with PM-996 and polyethylene cling film double-layer film, and stir at room temperature for 2 hours with a magnetic stirrer The above can be dissolved with the aid of ultrasonic waves to obtain a colorless, clear and transparent precursor solution with a concentration of 1M and a molar ratio of methyl bromide to lead bromide of 1:1.

[0063] 2. Seed crystal cultivation

[0064] Take 10ml of the precursor solution in step 1 in a 50ml tall beaker, add an appropriate amount of absolute ethanol to make the solution close to saturation; make a small hole with a diameter of 2mm in the PM-996 sealing film, and seal the beaker with the sealing film to make the small hole Located in the center of the mouth of the beaker; add 70ml of absolute ethanol to a 500ml larg...

Embodiment 3

[0070] 1. Configure the precursor solution

[0071] Take by weighing 4.047g chloromethylamine (CH 3 NH 3 Cl), 16.686g lead chloride (PbCl 2 ) into a 100ml beaker with a stirring bar, add 30ml dimethyl sulfoxide (DMSO), seal with PM-996 and polyethylene cling film double-layer film, and stir with a heating magnetic stirrer at 50°C for more than 2 hours , can be dissolved with the aid of ultrasonic waves to obtain a colorless, clear and transparent precursor solution with a concentration of 2M and a molar ratio of chloromethylamine to lead chloride of 1:1.

[0072] 2. Seed crystal cultivation

[0073] Take 10ml of the precursor solution in step 1 in a 50ml tall beaker. After the solution is cooled to room temperature, add an appropriate amount of absolute ethanol to make the solution precipitate a small amount of white precipitate and the precipitate is insoluble. Filter the solution with a 0.22 μm polytetrafluoroethylene After filtering the solution with a membrane filter, ...

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Abstract

The invention discloses a method for growing an ABX3 perovskite single crystal by antisolvent diffusion. The method comprises the following steps: dissolving an A-containing halide and a B-containing metal compound in a solvent M, and adding a right amount of antisolvent N to obtain an approximately saturated single crystal growth solution, wherein the mole ratio of the A-containing halide to the B-containing metal compound is 1:(0.1-2); putting the open container P containing the approximately saturated single crystal growth solution into the closed container Q containing the antisolvent N; and at a certain temperature, carrying out seed crystal culture and seed crystal growth (two growth processes) to obtain the ABX3 perovskite single crystal with required size. According to the method for preparing the high-quality perovskite single crystal, the principle that the antisolvent diffuses to the single crystal growth solution is utilized to slowly lower the solubility of perovskite in the single crystal growth solution, so that the solution precipitates the perovskite single crystal. The method has the advantages of large size and high quality of the obtained single crystal, high utilization ratio of raw materials, simple facility request, simple technique, low environmental hazard and the like.

Description

technical field [0001] The invention belongs to the technical field of perovskite single crystal preparation, in particular to an anti-solvent diffusion growth ABX 3 Methods for perovskite single crystals. Background technique [0002] With the rapid development of human society, people's demand for energy is also increasing rapidly. The limited traditional fossil energy is consumed in large quantities and is increasingly exhausted, causing a series of problems such as environmental pollution and global warming, which has triggered people's urgent need for sustainable energy. need. The development of new energy sources provides an important guarantee for the sustainable development of human civilization. As a clean and inexhaustible energy source, solar energy can just solve the increasingly acute contradiction between the environment and energy. Currently, a perovskite-structured organic-inorganic hybrid material CH 3 NH 3 wxya 3 It is sparking a revolution in the fiel...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B7/14
CPCC30B7/14C30B29/12
Inventor 冯晶胡明钰种晓宇
Owner KUNMING UNIV OF SCI & TECH
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