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Preparation method for growing perovskite single crystal by liquid-phase diffusion separation crystallization at room temperature

A liquid phase diffusion and perovskite technology, applied in the direction of single crystal growth, single crystal growth, crystal growth, etc., can solve the problems affecting human health and environmental protection, high sealing requirements of the reaction system, and slow solvent volatilization speed, etc., to achieve low The effect of carrier recombination rate, non-toxic and non-volatile, and huge application potential

Inactive Publication Date: 2019-12-10
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method needs to be incorporated into the precursor solution through solvent volatilization to cause single crystal precipitation, but the solvent volatilization speed is slow, and most of the solvents are organic solvents, which are toxic and harmful to the human body after volatilization, and will also cause environmental pollution. High energy consumption, The reaction system has high sealing requirements and heavy pollution, which affects human health and environmental protection, and has many disadvantages

Method used

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  • Preparation method for growing perovskite single crystal by liquid-phase diffusion separation crystallization at room temperature
  • Preparation method for growing perovskite single crystal by liquid-phase diffusion separation crystallization at room temperature
  • Preparation method for growing perovskite single crystal by liquid-phase diffusion separation crystallization at room temperature

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Effect test

Embodiment 1

[0040] The preparation method is as follows:

[0041] (1) Lead bromide and methylamine hydrobromide (CH 3 NH 3 Br, MABr) was added to dimethylformamide (DMF) solvent at a molar ratio of 1:1, dissolved at room temperature, prepared into a 0.8mol / L solution, and then filtered with a 0.22 micron filter head to obtain a saturated precursor solution;

[0042] (2) Add the precursor solution into the sample bottle, the height of the liquid level is about 3mm, and add 3mL of silicone oil on the upper layer of the precursor solution;

[0043] (3) Place the sample bottle on a heating stage at 35 degrees Celsius, place it for 72 hours, and obtain MAPbBr with a thickness of about 50 microns at the bottom of the solution 3 single crystal.

[0044] figure 1 The entire preparation process is shown. figure 2 a) is the resulting MAPbBr 3 Scanning electron microscope (SEM) image of a perovskite single crystal, inset showing a thickness of about 50 micrometers.

Embodiment 2

[0046] The preparation method is as follows:

[0047] (1) Lead bromide and methylamine hydrobromide (CH 3 NH 3 Br, MABr) was added to the dimethylformamide (DMF) solvent at a molar ratio of 1:1, dissolved at room temperature, prepared into a 1.6mol / L solution, and then filtered with a 0.22 micron filter head to obtain a saturated precursor solution;

[0048] (2) Add the precursor solution to the sample bottle, and add silicone oil (3ml) to the upper layer of the precursor solution;

[0049] (3) Place the sample bottle on a heating stage at 35 degrees Celsius for 72 hours, and obtain about 0.5 cm of MAPbBr at the bottom of the solution 3 single crystal.

[0050] figure 2 b) is the resulting MAPbBr 3 Optical photograph image of a perovskite single crystal, about 0.5 cm in size. image 3 is the resulting MAPbBr 3 X-ray diffraction pattern of perovskite single crystal, a) is 2θ diffraction curve, b) is MAPbBr 3 The rocking curves of single crystals (100) and (200); the F...

Embodiment 3

[0052] The preparation method is as follows:

[0053] (1) Lead chloride and methylamine hydrochloride (CH 3 NH 3 Cl, MACl) was added to a mixed solvent of dimethylformamide (DMF) and dimethyl sulfoxide at a molar ratio of 1:1, dissolved at room temperature, prepared into a 0.9mol / L solution, and then filtered with 0.22 microns Obtain a saturated precursor solution after head filtration;

[0054] (2) Add the precursor solution to the sample bottle, and add silicone oil (3mL) to the upper layer of the precursor;

[0055] (3) Place the sample bottle on a heating stage at 35 degrees Celsius, place it for 72 hours, and obtain MAPbCl at the bottom of the solution 3 single crystal.

[0056] Figure 5 On the left is MAPbCl 3 Optical photograph of a single crystal.

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Abstract

The invention discloses a preparation method for growing perovskite single crystals by liquid-phase diffusion separation crystallization at the room temperature. The preparation method comprises the following steps of (1) preparing a saturated perovskite precursor solution; (2) adding dimethylsilicone oil into the precursor solution, and forming a liquid seal on a perovskite solution by the dimethylsilicone oil; and (3) forming perovskite crystals by heating. The dimethylsilicone oil is insoluble with a solvent in the precursor solution; and a density relationship is that the solvent of the perovskite precursor solution is less than the dimethylsilicone oil and the dimethylsilicone oil is less than the perovskite precursor solution. According to different reactants, two-dimensional or three-dimensional perovskite single crystals can be prepared, the single crystals can be obtained at the room temperature, and the crystal quality is higher. The method is prepared in a lower-temperatureenvironment, nucleation is less, the crystal quality is higher, and defects are fewer. The perovskite single crystals have good application prospects in the photoelectric field, and the high-efficiency and simple preparation method has great potential for commercial application of the single crystals.

Description

technical field [0001] The invention belongs to the technical field of semiconductor optoelectronic materials and device preparation, and in particular relates to a method for preparing a perovskite single crystal grown by liquid phase diffusion separation and crystallization at room temperature. The method can prepare high-quality two-dimensional single crystal and bulk phase single crystal. Background technique [0002] Perovskite materials have many excellent properties such as few deep energy level defects, long carrier life and large light absorption coefficient, and have attracted the attention of researchers. Perovskite solar cells have developed rapidly, and the efficiency has increased from 3.9% to more than 24.2%, it also has a good application in light-emitting diodes, and its electroluminescent external quantum efficiency exceeds 28%. In addition, it also has a wide range of applications in detectors, lasers and other fields. Perovskite single crystal, because of...

Claims

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Application Information

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IPC IPC(8): C30B29/22C30B7/14
CPCC30B7/14C30B29/22
Inventor 方国家姚方
Owner WUHAN UNIV
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