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Methylamine halogenated plumbate compound large-size crystal growth method and device

A technology of methylamine halide lead salt and growth method, which is applied in the direction of crystal growth, single crystal growth, single crystal growth, etc., can solve the problems of testing the anisotropic physical properties of large-sized crystals without compounds, and achieve easy large-scale High-quality crystals, easy to achieve operating conditions, and avoid the effect of stray crystals

Active Publication Date: 2015-02-25
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the reports on such materials are thin film materials, but for CH 3 NH 3 wxya 3 (X is a halogen) crystal material is rarely reported, and so far, there is no report on the growth of large-sized crystals of this type of compound and the physical properties of crystal anisotropy at home and abroad.

Method used

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  • Methylamine halogenated plumbate compound large-size crystal growth method and device
  • Methylamine halogenated plumbate compound large-size crystal growth method and device
  • Methylamine halogenated plumbate compound large-size crystal growth method and device

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Embodiment 1. Crystal growth device

[0052] A kind of methylamine type lead halide salt large-size crystal growth device, the structure is as follows figure 1 As shown, a seed crystal rod 1 driven by a rotating motor 2 is vertically arranged in the middle of the water tank 7. The lower end of the seed crystal rod 1 is connected to a seed crystal holder 9 which is composed of upper and lower parallel disks 10, 11 And the cage structure formed by the vertical support rods 12 connecting the two discs, the lower disc 11 is the seed crystal plate; in the water tank 7, one side of the seed crystal rod 1 is provided with a heater 3 and a temperature sensor 4 in order from the inside to the outside. A paddle stirrer 5 and a thermometer 6 are arranged on the opposite side from the inside to the outside. The rotating motor 2 is directly and fixedly connected with the rotating stirrer 13, and the seed crystal rod 1 is fixed on the rotating stirrer 13. The device heats the solution...

Embodiment 2

[0053] Example 2: Large size CH 3 NH 3 PbBr 3 Crystal growth

[0054] a. Methylamine bromide (CH 3 NH 3 Br) synthetic preparation: in an ice water bath, CH 3 NH 2 The aqueous solution was added to the HBr solution and reacted for 3.5 hours; CH 3 NH 2 :HBr=1.5:1 molar ratio. The mass percentage concentration of the methylamine aqueous solution is 30 wt%, and the mass percentage concentration of the HBr solution is 40 wt%.

[0055] After rotary evaporation with a vacuum rotary evaporator, white methylamine bromide is obtained. Add anhydrous ether to the obtained brominated methylamine and recrystallize 3 times to obtain white CH 3 NH 3 Br. Will get the white CH 3 NH 3 Br, placed in a vacuum drying oven for 2 hours, to obtain colorless CH 3 NH 3 Br crystals.

[0056] b. In a 300cm×30cm constant temperature water tank, accurately weigh Pb(CH 3 COOH) 2 ·3H 2 O was added to the 40wt% HBr solution to obtain a colorless and transparent solution.

[0057] c. Accurately weigh the CH prepared ...

Embodiment 3

[0059] Example 3. Large size CH 3 NH 3 PbI 3 Crystal growth

[0060] a. Methylamine iodide (CH 3 NH 3 I) Synthesis

[0061] Put CH in an ice water bath 3 NH 2 The aqueous solution is added to the HI solution, CH 3 NH 2 :HI=1.2:1 molar ratio, react for 4 hours. The mass percentage concentration of the methylamine aqueous solution is 30 wt%, and the mass percentage concentration of the HI solution is 40 wt%.

[0062] After rotary evaporation with a vacuum rotary evaporator, white methylamine iodide was obtained. Add anhydrous ether to the obtained methylamine iodide and recrystallize 3 times to obtain white CH 3 NH 3 I. Will get the white CH 3 NH 3 I, put it in a vacuum drying oven for several hours, and finally get colorless CH 3 NH 3 I crystal.

[0063] b. In a constant temperature water tank (300cm×30cm), accurately weigh Pb(CH 3 COOH) 2 ·3H 2 O was added to the 45wt% HI solution to obtain a yellow transparent solution.

[0064] c. Accurately weigh the CH prepared in step a accordin...

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Abstract

The invention relates to a methylamine halogenated plumbate compound large-size crystal growth method and device. The crystal growth method is a bottom seed crystal solution cooling process and comprises the following steps: sequentially adding raw materials CH3NH2 and Pb(CH3COOH)2.3H2O into an HX (X is halogen) solution according to the stoichiometric proportion to obtain a precipitate, continuously stirring, heating to completely dissolve the precipitate so as to obtain a clear solution, cooling to the saturation point of the solution, adding the seed crystal, and slowly cooling to perform crystal growth for about 1 month. The invention also relates to a large-size crystal growth device. The prepared CH3NH3PbX3 crystal has favorable light absorption range in the ultraviolet-visible light region, has the advantages of no deliquescence and favorable stability, and is applicable to the fields of solar cells, photoelectricity and the like. Compared with the high-temperature solution volatilization process, the method provided by the invention can obtain the large-size high-quality crystal more easily, and has the advantages of accessible raw materials and low cost.

Description

Technical field [0001] The invention relates to the crystal growth and application of organic-inorganic composite semiconductor crystal materials, in particular to a method and device for growing large-size crystals of methylamine lead halide compounds, and belongs to the technical field of crystal materials. Background technique [0002] The main group metal halide metalate compounds, it is particularly pointed out that, as a new type of semiconductor material, the lead halide has special photoconductivity, ion conduction, electrical conduction, photoluminescence and phase change properties. Due to its many excellent properties, the presence The field of effect transistors, light-emitting diodes and solar cells has potential application value and is currently a research focus in countries around the world. [0003] Most of the lead halides belong to the perovskite structure, and their chemical formula is APbX 3 (A is alkali metal or organic cation, X is halogen), PbX exists in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/54C30B7/08
CPCC30B7/08C30B29/54
Inventor 陶绪堂党洋洋孙友轩夏海兵
Owner SHANDONG UNIV
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