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Preparation method of large-size mixed halogen methylamine lead bromine chloride crystal

A large-scale, crystal technology, applied in the field of crystal material preparation, can solve the problem of no large-scale and achieve high-quality results

Active Publication Date: 2018-07-24
NANJING UNIV OF INFORMATION SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently on CH 3 NH 3 Pb(Br 1-x Cl x ) 3 The research is mainly on thin film materials, there is no large size CH 3 NH 3 Pb(Br 1-x Cl x ) 3 Single crystal growth reports

Method used

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  • Preparation method of large-size mixed halogen methylamine lead bromine chloride crystal
  • Preparation method of large-size mixed halogen methylamine lead bromine chloride crystal
  • Preparation method of large-size mixed halogen methylamine lead bromine chloride crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1CH 3 NH 3 Pb(Br 1-x Cl x ) 3 The preparation of x=0.5 is Br:Cl=1:1

[0028] Comprise following preparation steps (flow process such as figure 1 shown):

[0029] Step S1, CH 3 NH 3 Preparation of Br: Mix monomethylamine aqueous solution (40wt%) and hydrobromic acid aqueous solution (48wt%) according to equimolar solute (0.01mol) in an ice-water bath and stir for 2h, then evaporate to dryness at 100°C to obtain 1.12g white powder thing;

[0030] Step S2, CH 3 NH 3 Preparation of Cl: Mix monomethylamine aqueous solution (40wt%) and hydrochloric acid aqueous solution (37wt%) according to equimolar solute (0.01mol) in an ice-water bath and stir for 2h, then evaporate to dryness at 100°C to obtain 0.67g white powder thing;

[0031] Step S3, preparation of crystallization mother liquor: under normal temperature conditions, PbBr 2 (0.01mol, 3.67g) with CH 3 NH3 Br (0.01mol, 1.12g) and PbCl 2 (0.01mol, 2.78g) with CH 3 NH 3 Cl (0.01mol, 0.67g) was disso...

Embodiment 2-4

[0033] Example 2-4CH 3 NH 3 Pb(Br 1-x Cl x ) 3 preparation of

[0034] By regulating PbBr 2 / PbCl 2 Molar ratio (PbBr 2 with CH 3 NH 3 Br equimolar, PbCl 2 with CH 3 NH 3 Cl equimolar) to prepare crystals with Br:Cl molar ratios of 3:1, 2:1, 1:2, and 1:3, and other conditions were the same as in Example 1.

Embodiment 5

[0035] Embodiment 5 physical parameters are measured

[0036] Measure the CH prepared by embodiment 1-4 respectively 3 NH 3 Pb(Br 1-x Cl x ) 3 The size, XRD, UV-VIS-NIR absorption spectrum and corresponding bandgap spectrum of crystals (Br:Cl molar ratios are 3:1, 2:1, 1:1, 1:2, 1:3, respectively).

[0037] Measurement results such as figure 2 and image 3 As shown, the length and width of the crystals are as high as 6-8mm, and as high as 2-4mm, with ideal spectral properties, adjustable band gap, and high quality.

[0038] The present invention adopts an inversion solution crystal growth process, and by changing the ratio of raw material components, CH with large size, high quality and adjustable band gap can be obtained with different halogen ratios. 3 NH 3 Pb(Br 1-x Cl x ) 3 crystals. The applicant also tried nearly a hundred different solvents, solvent combinations and crystallization processes for the crystallization of large-sized CH 3 NH 3 Pb(Br 1-x Cl ...

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Abstract

The invention discloses a preparation method of a large-sized mixed halogen methylamine lead-bromine-chlorine crystal. The preparation method comprises the following steps: step S1, stirring a monomethylamine water solution and a hydrobromic acid water solution, and drying by distillation; step S2, stirring a monomethylamine water solution and hydrochloric acid, and drying by distillation; step S3, dissolving PbBr2 with CH3NH3Br and dissolving PbCl2 with CH3NH3Cl into DMF and DMSO solvents to obtain a CH3NH3Pb(Br1-xClx)3 mother liquor; and changing the molar ratio of PbBr2 to PbCl2 to obtain CH3NH3Pb(Br1-xClx)3 mother liquor with different x values; and step S4, raising the temperature of the CH3NH3Pb(Br1-xClx)3 mother liquor to be 95 to 105 DEG C, maintaining a constant temperature until the crystal is separated out, and taking out the crystal when the size of the crystal is not increased any longer. The CH3NH3Pb(Br1-xClx)3 crystal with different halogen proportions can be obtained by changing the proportion of raw materials.

Description

technical field [0001] The invention belongs to the technical field of crystal material preparation, and relates to a method for preparing a large-sized mixed halogen methylamine lead, bromine and chloride crystal, which is a method for artificially cultivating crystals by adopting a solution inversion temperature growth method. Background technique [0002] Recently, organic-inorganic hybrid perovskite materials (CH 3 NH 3 wxya 3 , X=I, Br, Cl) has attracted extensive attention due to its excellent optical and electrical properties in solar cells, light-emitting diodes, photodetectors and other fields. The efficiency of solar cells based on perovskite materials has exceeded 21%, showing good prospects for development. Compared with traditional monocrystalline silicon and polycrystalline silicon solar cells, it has the advantages of low raw material cost, simple preparation technology, and low-temperature preparation, and is expected to become a substitute for silicon-bas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/00C07C211/04C30B29/54C30B7/14
CPCC07C209/00C30B7/14C30B29/54C07C211/04
Inventor 苏静王万富仲坤赖敏卢迪柏宇
Owner NANJING UNIV OF INFORMATION SCI & TECH
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