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Process for preparing perovskite structure light-emitting material through temperature inversion method

A technology of perovskite structure and light-emitting material, applied in the direction of light-emitting material, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of inability to obtain large crystals, slow crystal growth rate, strict temperature control requirements, etc. Mild production conditions, high reproducibility, and energy savings

Inactive Publication Date: 2017-11-10
苏州虹霞晶体科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For single crystal ABX 3 Material, its preparation method is mainly based on the cooling crystallization method, but first of all, this method has strict requirements on temperature control. Temperature changes will not only affect the solubility of the solute, and even phase change, but also affect the quality of the final crystal. Secondly, the crystal growth rate It is very slow, the preparation cycle is long, and large crystals cannot be obtained. At the same time, the equipment required is relatively complicated and difficult to implement, so there is a lot of room for improvement.

Method used

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  • Process for preparing perovskite structure light-emitting material through temperature inversion method
  • Process for preparing perovskite structure light-emitting material through temperature inversion method
  • Process for preparing perovskite structure light-emitting material through temperature inversion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]CH 3 NH 3 PbBr 3 Preparation method of material:

[0031] 1. Configure the precursor solution

[0032] Weigh 0.7833g methyl bromide (CH 3 NH 3 Br), 2.569g lead bromide (PbBr 2 ) into a 50ml beaker with a stirring bar, add 10ml N,N-dimethylformamide (DMF), seal with PM-996 and polytetrafluoroethylene film double-layer film, stir at room temperature with a magnetic stirrer After more than 12 hours, ultrasonic waves can be used to assist dissolution, and the solution is filtered through a PTFE filter membrane with a diameter of 22 μm to obtain a precursor solution.

[0033] 2. Material preparation

[0034] Take the precursor solution in step 1 in four 10ml sample bottles, 2.5ml in each bottle, put the sample bottles containing the precursor solution in an oil bath at 80°C for 3 hours, and a 0.5~10mm particle will be precipitated at the bottom of the container CH 3 NH 3 PbBr 3 .

[0035] 3. CH 3 NH 3 PbBr 3 Washing, drying and collection of materials

[0036]...

Embodiment 2

[0038] CH 3 NH 3 PbCl 3 Preparation method of material:

[0039] 1. Configure the precursor solution

[0040] Weigh 0.4722g chloromethylamine (CH 3 NH 3 Cl), 1.9467g lead chloride (PbCl 2 ) into the 50ml beaker P that has been put into the stirring bar, add 10ml dimethyl sulfoxide (DMSO), seal with PM-996 and polytetrafluoroethylene film double-layer film, and stir at room temperature for more than 12 hours with a magnetic stirrer , can be dissolved with the aid of ultrasonic waves, and after the solution is fully dissolved, filter the solution with a PTFE filter membrane with a diameter of 22 μm to obtain a precursor solution.

[0041] 2. Material preparation

[0042] Take the precursor solution in step 1 in four 10ml sample bottles, each bottle is 2.5ml, put the sample bottle containing the precursor solution in an oil bath at 90°C for 3 hours, and 0.5~10mm particles can be precipitated at the bottom of the container CH 3 NH 3 PbCl 3 .

[0043] 3. CH 3 NH 3 PbC...

Embodiment 3

[0046] CH 3 NH 3 PBr 2 Preparation method of material:

[0047] 1. Configure the precursor solution

[0048] Weigh 0.6885g methyl iodide (CH 3 NH 3 I), 1.997g lead iodide (PbI 2 ) in a 50ml beaker with a stirring bar,

[0049] Add 3ml of γ-butyrolactone (GBL) and seal with PM-996 and polytetrafluoroethylene film double-layer film, stir at room temperature with a magnetic stirrer for more than 12 hours, and dissolve with the aid of ultrasonic waves.

[0050] Weigh 0.5222 bromomethylamine (CH 3 NH 3 Br), 1.1726g lead bromide (PbBr 2 ) into a 50ml beaker with a stirring bar, add 7ml of N,N-dimethylformamide (DMF), seal with PM-996 and polytetrafluoroethylene film, and stir at room temperature with a magnetic stirrer For more than 12 hours, it can be dissolved with the aid of ultrasound.

[0051] After the above two solutions are fully dissolved, mix them in a 50ml beaker with a stirring bar, and dissolve them at room temperature for 30 minutes with a magnetic stirrer. ...

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Abstract

The invention discloses a process for preparing a perovskite structure light-emitting material through a temperature inversion method. The process comprises: 1, dissolving an A-containing halide and a B-containing metal halide or oxide in a solvent M, and filtering the obtained solution to obtain a precursor solution, wherein A is the mixture comprising one or a plurality of materials selected from CH3NH3<+>, Cs<+>, H2N-CH=NH2<+>, (CH3)4N<+>, C7H7<+> and C3H11SN3<2+>, B is the mixture comprising one or a plurality of materials selected from Pb, Ge and Sn, and X is the mixture comprising one or a plurality of halogen elements selected from Cl, Br and I; 2, placing the container filled with the precursor solution into an oil bath with a temperature of 50-200 DEG C for 0.5-5 h, and precipitating ABX3 at the bottom portion of the container; and 3, washing the precipitated ABX3 by using a solvent N, carrying out vacuum drying for 0.5-48 h at a temperature of 20-200 DEG C, and carrying out sealed storage. With the technical scheme of the present invention, the prepared perovskite structure light-emitting material ABX3 has advantages of high purity, high light-emitting efficiency, short production period, simple requirement on the equipment, and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of luminescent materials, in particular to a perovskite structure luminescent material ABX prepared by an inversion temperature method 3 craft. Background technique [0002] Luminescent materials have played a vital role in the development of human society from the beginning to the present. In addition to being used for daily lighting, it is also widely used in high-tech fields such as communications, optical computers, biomolecular probes, and aerospace. In recent years, a perovskite structure A n BX 2+n materials (especially organic-inorganic hybrid materials CH 3 NH 3 wxya 3 ) is causing a revolution in the field of semiconductors, which has brought great attention to this series of materials. The study found that this series of perovskite structure materials has excellent optical and electrical properties, and the most common perovskite material is methylamine lead iodide (CH 3 NH ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/66C07C211/04C07C211/05C07C209/00C01G9/00C01G21/00
CPCC09K11/06C09K11/66C01G9/006C01G21/006C07C209/00C07C211/04C07C211/05C01P2002/34C01P2006/80
Inventor 冯晶葛春宇胡明钰于杰
Owner 苏州虹霞晶体科技有限公司
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