Preparation method of large-sized perovskite structure CH3NH3PbI3 crystal

A technology of perovskite structure and lead methylamine iodide is applied in crystal growth, chemical instruments and methods, single crystal growth, etc., to achieve the effects of simple synthesis process, simple growth device and less side reactions

Active Publication Date: 2014-11-05
江苏荣辉电力设备制造有限公司
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  • Preparation method of large-sized perovskite structure CH3NH3PbI3 crystal
  • Preparation method of large-sized perovskite structure CH3NH3PbI3 crystal
  • Preparation method of large-sized perovskite structure CH3NH3PbI3 crystal

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[0025] Example 1

[0026] The preparation method of large-size perovskite structure methamine iodine lead crystal adopts the solution cooling method, and the specific steps are as follows:

[0027] 1) Weigh 0.01mol of PbI 2 ,Use 25ml, 57% HI solution to dissolve at room temperature to get Pb 2+ -HI solution;

[0028] 2) According to HI and CH 3 NH 2 The molar ratio is 1:1. Use a pipette to measure 57% HI solution and 40% CH 3 NH 2 The solution is 2.64ml, 1.72ml, the two solutions are mixed and sealed, placed in an ice water bath at 0℃ for 2h to obtain CH 3 NH 2 I solution;

[0029] 3) At room temperature, the Pb 2+ -HI solution and CH 3 NH 2 When the solution is mixed, a black solid substance is formed immediately. Place the solution in an oil bath at 95°C for preheating for 48 hours;

[0030] 4) Keep the solution temperature at 95℃, filter to remove the black solid material at the bottom. Preheat the resulting clear brown liquid in an oil bath at 96°C for 24 hours as CH 3 NH 3 PbI 3...

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Abstract

The invention discloses a preparation method of a large-sized perovskite structure CH3NH3PbI3 crystal. The method comprises the following steps: dissolving PbI2 into an HI (Hydrogen Iodide) solution, and preparing a Pb<2+>-HI solution; mixing the HI solution with a CH3NH2 solution in the molar ratio of 1:1, and reacting the mixture at the temperature of 0 DEG C for 2 hours to obtain a CH3NH2I solution; mixing the Pb<2+>-HI solution with the CH3NH2I solution, preheating at the temperature of 95 DEG C for 48-72 hours to obtain an oversaturated solution, and filtering the oversaturated solution to obtain a mother liquor for growing the CH3NH3PbI3 crystal, wherein the molar ratio of CH3NH2I to Pb<2+> is (1-2):1; and preheating the mother liquor in a water bath of 95.5-96 DEG C for 12-24 hours, placing the preheated mother liquor into a crystal growing container, performing programmed cooling to 45 DEG C, and keeping a constant temperature to obtain the CH3NH3PbI3 crystal. In a process of the method, the HI solution participates in the synthesis of raw materials, and is taken as a solvent of crystal growing, so that the method has the advantages of simple synthesizing process and small number of side reactions; and a growing device is simple, and a high-quality and large-sized crystal can be grown.

Description

technical field [0001] The invention relates to a method for preparing a large-sized perovskite structure methylammonium iodine lead crystal, which is a method for artificially cultivating crystals by adopting a solution cooling method, and belongs to the technical field of crystal material preparation. Background technique [0002] From 2009 to 2013, CH 3 NH 3 wxya 3 (X=Cl, Br, I) The power conversion efficiency of perovskite solar cells ranges from 3.8% to more than 15%. Worldwide, the research on perovskite solar cells has reached unprecedented popularity, and it was selected into the "Science" magazine Published top ten scientific and technological breakthroughs in 2013. This kind of material combines the high carrier mobility of inorganic components and the good flexible processing performance of organic components, which can efficiently absorb broad-spectrum light from visible light to 800nm ​​wavelength, and can also be used in TiO 2 , Al 2 o 3 The characteristi...

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Application Information

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IPC IPC(8): C30B29/54C30B7/08
Inventor 苏静赖敏徐林华雷勇张颖桑琳
Owner 江苏荣辉电力设备制造有限公司
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