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Method and device for growing large-sized methylammonium lead bromide crystals by controllable anti-solvent diffusion method

A technology of lead methylamine bromide and a growth method, which is applied in the directions of single crystal growth, single crystal growth, crystal growth, etc., can solve problems such as high corrosion of equipment, and achieve the effects of low equipment cost, easy availability of raw materials and good quality.

Active Publication Date: 2020-09-29
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses an acid solution, which is highly corrosive to equipment, and the size of the lead methylammonium bromide crystals obtained is only 5mm, which is still relatively small

Method used

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  • Method and device for growing large-sized methylammonium lead bromide crystals by controllable anti-solvent diffusion method
  • Method and device for growing large-sized methylammonium lead bromide crystals by controllable anti-solvent diffusion method
  • Method and device for growing large-sized methylammonium lead bromide crystals by controllable anti-solvent diffusion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1, crystal growth device

[0052] like figure 1 As shown, a growth device for a large-scale perovskite structure methylammonium lead bromide crystal, including a gas generator 1, a dryer 2, a gas control valve 3, an anti-solvent container 5, a heater 8, a crystal grower 9 and a heating container 12;

[0053] The gas generator 1 is connected with the drier 2, the gas control valve 3, the anti-solvent container 5 and the crystal grower 9 in turn through the vent pipe, and the crystal grower 9 is arranged in the heating container 12, and the heating A heater 8 is arranged in the container 12;

[0054] The anti-solvent container 5 is arranged in the heating device 4;

[0055] The growth device also includes a temperature controller 6, and the heating container 12 is also provided with a stirring motor 7 and a thermocouple 10, and the thermocouple 10 is connected with the heater 8, and the stirring motor 7, thermoelectric Even 10 is connected with temperature ...

Embodiment 2

[0059] Example 2, large size CH 3 NH 3 PbBr 3 crystal growth

[0060] The growth method of large-scale perovskite structure methylammonium lead bromide crystal adopts the method of anti-solvent diffusion, including the following steps:

[0061] (1) Methylamine bromide (CH 3 NH 3 Br) preparation

[0062] In an ice-water bath, CH 3 NH 2 The aqueous solution was added dropwise to the HBr solution to react for 2h; CH 3 NH 2 The molar ratio to HBr is 1:1. CH 3 NH 2 The mass concentration of the aqueous solution is 30%, and the mass concentration of the HBr solution is 40%.

[0063] Rotary evaporation by a vacuum rotary evaporator gave white methylamine bromide. Washed 3 times with ether, and recrystallized with ethanol, the obtained white CH 3 NH 3 Br, placed in a vacuum oven, dried overnight, to give CH 3 NH 3 Br white crystals.

[0064] (2) Lead methylamine bromide compound (CH 3 NH 3 PbBr 3 ) preparation and crystal growth

[0065] PbBr 2 with CH 3 NH 3 ...

Embodiment 3

[0070] As described in Example 2, the difference is:

[0071] Control CH 3 NH 3 PbBr 3 The concentration of the solution is 1.0mol / L, the temperature is 35°C, and the flow rate is 2.83cm 3 / sec. The growth cycle is 10 days, and orange-red transparent CH is obtained 3 NH 3 PbBr 3 crystals.

[0072] Obtained crystal size: 18×16×6mm 3 single crystal, such as image 3 shown.

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Abstract

The invention relates to a controllable anti-solvent diffusion method based large-size methylamine bromide lead crystal growth method and device. By adoption of a controllable anti-solvent diffusion method, the method includes steps: in a CH3NH3PbBr3 crystal growth process, feeding anti-solvent steam into CH3NH3PbBr3 solution, and performing crystal growth at 20-55DEG C to obtain large-size perovskite-structure methylamine bromide lead crystal. The method has advantages that the problem of failure in acquisition of large-size high-quality crystals in adoption of a volatilization method is effectively solved, and problems of high equipment corrosion, long growth period and the like due to adoption of acid solution in a traditional cooling method are solved as well; high-quality large-size crystals can be obtained easily, and the crystal size reaches 50*50*20mm<3>.

Description

technical field [0001] The invention relates to a method and a device for growing a large-sized perovskite structure methylammonium lead bromide crystal, and adopts a temperature-controlled and speed-controlled anti-solvent diffusion method to cultivate the crystal. In particular, the invention relates to a method and a device for growing a large-sized crystal of a methylamine halide lead salt compound, and belongs to the technical field of crystal materials. Background technique [0002] Organic-inorganic composite perovskite materials have excellent photoconductivity, ion conductivity, high carrier mobility, luminescence, ferroelectricity and other properties, and have potential in the fields of solar cells, field effect transistors, light-emitting diodes and detectors. application value. In 2009, the research group of Professor Miyasaka of Toin Yokohama University in Japan applied perovskite as a raw material to solar cells, and the photoelectric conversion efficiency ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/54C30B7/00
CPCC30B7/00C30B29/54
Inventor 刘阳陶绪堂张磊磊
Owner SHANDONG UNIV