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Inorganic perovskite crystal preparation method and product thereof

A perovskite precursor, inorganic calcium technology, applied in crystal growth, chemical instruments and methods, single crystal growth and other directions, can solve the problems of difficulty in preparing large-sized crystals, difficult to control the preparation process, and high crystal defect density. Inhibition of the effect of perovskite crystal nucleation, high crystal growth success rate, and low defect density

Inactive Publication Date: 2020-06-23
CHENGDU SCI & TECH DEV CENT CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve technical problems such as complex process parameters in the process of preparing inorganic perovskite materials in the prior art, difficulty in controlling the preparation process, difficulty in preparing large-sized crystals with a particle size above 5mm, and high crystal defect density. The invention provides a method for preparing inorganic perovskite crystals and its products. The method is simple to operate, and the obtained crystals have a high success rate of growth, and have the advantages of large size and low defect density

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  • Inorganic perovskite crystal preparation method and product thereof
  • Inorganic perovskite crystal preparation method and product thereof
  • Inorganic perovskite crystal preparation method and product thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Preparation of Inorganic Perovskite Crystals

[0049] The experimental device and experimental scene for preparing inorganic perovskite are as follows: figure 1 As shown, weigh 6mmol CsBr and 6mmolPbBr 2 Add the powder into the reaction vessel 103, then add 10 mL of dimethyl sulfoxide (DMSO) using a pipette gun, cover the airtight plug 104, close the inlet and outlet 105 and the gas outlet 106, put the reaction vessel 103 into a vibrator, and vibrate Half an hour to ensure that the solute is fully dissolved to obtain the perovskite precursor solution 102, put the reaction vessel 103 filled with the perovskite precursor solution 102 into the constant temperature water bath 101, and ensure that the liquid level of the water bath is higher than that of the perovskite precursor solution 102 On the surface, the constant temperature water bath 101 was heated to 45°C and kept constant. Into the air inlet 105, a constant flow of nitrogen gas is introduced, and the flow rate o...

Embodiment 2

[0055] Preparation of Inorganic Perovskite Crystals

[0056] The experimental device and experimental scene for preparing inorganic perovskite are as follows: figure 1 As shown, weigh 4mmolCsI and 5mmolPbBr 2 Add the powder into the reaction vessel 103, then add 10 mL of dimethylformamide (DMF) using a pipette gun, cover the airtight plug 104, close the inlet and outlet 105 and the gas outlet 106, put the reaction vessel 103 into a vibrator, and vibrate Half an hour to ensure that the solute is fully dissolved to obtain the perovskite precursor solution 102, put the reaction vessel 103 filled with the perovskite precursor solution 102 into the constant temperature water bath 101, and ensure that the liquid level of the water bath is higher than that of the perovskite precursor solution 102 On the other hand, the constant temperature water bath 101 was heated to 60°C and kept constant. Into the air inlet 105, a constant flow of nitrogen gas is introduced, and the flow rate of...

Embodiment 3

[0060] Preparation of Inorganic Perovskite Crystals

[0061] The experimental device and experimental scene for preparing inorganic perovskite are as follows: figure 1 As shown, weigh 5mmol CsBr and 6mmol PbBr 2 Add the powder into the reaction vessel 103, then add 10 mL of a mixture of butyrolactone (GBL) and dimethylformamide (DMF) using a pipette gun, cover the airtight plug 104, close the inlet and outlet 105 and the gas outlet 106, Put the reaction vessel 103 into a vibrator and vibrate for half an hour to ensure that the solute is fully dissolved to obtain a perovskite precursor solution 102. Put the reaction vessel 103 filled with the perovskite precursor solution 102 into a constant temperature water bath 101 to ensure that the water bath The surface is higher than the liquid surface of the perovskite precursor solution 102, and the constant temperature water bath 101 is heated to 50° C. and kept constant. Into the air inlet 105, a constant flow of nitrogen gas is in...

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Abstract

The invention relates to an inorganic perovskite crystal preparation method and a product thereof. The preparation method comprises the following steps: step 1, putting a reaction container filled with a perovskite precursor solution into a constant-temperature water bath with the temperature of 30-80 DEG C; wherein the liquid level of the water bath is higher than or equal to the liquid level ofthe perovskite precursor solution, continuously introducing nitrogen or inert gas into the reaction container at the flow rate of 0.2 L / min-5 L / min, keeping for a period of time, and waiting for crystals to be separated out and gradually grow until the crystals are not changed; step 2, taking out the crystal obtained in the step 1 from the solution, cleaning and blow-drying to obtain an inorganicperovskite crystal; wherein halogen elements X of the cesium halide and the lead halide are Br or I; wherein the molar concentration of the cesium halide and the molar concentration of the lead halideare 0.2 mol / L-0.6mol / L. According to the method, a constant-temperature solution growth process is adopted, and nitrogen or inert gas is introduced to assist in solvent evaporation, so that the prepared inorganic perovskite crystal has the advantages of large size and low defect density, and the method is simple and high in crystal growth success rate.

Description

technical field [0001] The invention belongs to the technical field of perovskite material preparation, and in particular relates to a method for preparing an inorganic perovskite crystal and a product thereof. Background technique [0002] In recent years, CH 3 NH 3 PB 3 The representative organic-inorganic hybrid perovskite material has developed rapidly, and its thin-film morphology has been proved to have excellent optoelectronic properties in the field of photovoltaic devices and photodetectors. In addition, this material also has the characteristics of high atomic number, high resistivity, and low leakage current, which more meet the material requirements for the preparation of X-ray and other nuclear radiation detectors. Typical organic-inorganic perovskite materials have low thermal stability due to the organic component methylamine or formamidine functional groups. To avoid this problem, it was found that inorganic alkali metal atoms Cs can be used to replace th...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B7/06
CPCC30B7/06C30B29/12
Inventor 刘江廖成
Owner CHENGDU SCI & TECH DEV CENT CHINA ACAD OF ENG PHYSICS
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