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Method for preparing high-stability CsPbBr3 quantum dots by solvent-free and ligand-free ball milling method

A high-stability, ligand-free technology, applied in chemical instruments and methods, luminescent materials, nanotechnology, etc., can solve the problems of difficult product separation, cumbersome preparation process, poor product stability, etc., and achieve simple process and environmental stability. Strong, no attenuation effect of emission intensity

Active Publication Date: 2022-05-06
XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For the above technical requirements, the present invention proposes a solvent-free and ligand-free ball milling method to prepare high-stability CsPbBr 3 The method of quantum dots effectively solves the problems of cumbersome preparation process, difficult product separation, large environmental pollution, poor product stability and low quantum yield.

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  • Method for preparing high-stability CsPbBr3 quantum dots by solvent-free and ligand-free ball milling method
  • Method for preparing high-stability CsPbBr3 quantum dots by solvent-free and ligand-free ball milling method
  • Method for preparing high-stability CsPbBr3 quantum dots by solvent-free and ligand-free ball milling method

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Experimental program
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Embodiment 1

[0030] In this embodiment, cesium bromide, lead bromide, and potassium bromide are used as the perovskite source, and the molar ratio is 1:1:3. The perovskite source is mixed with the PMMA polymer material. 1.5% of the total mass of polymer materials. Put the mixture into a 100mL ball mill jar, add 2mm, 4mm and 8mm combined zirconia balls, and mill them in a planetary ball mill at the speeds of 360r / min, 500r / min, and 630r / min, respectively. After 1 hour of ball milling, you get CbBr 3 PQDs / PMMA luminescent material.

[0031] Separate and sieve the luminescent material from the grinding ball, and measure the fluorescence spectrum, such as figure 1 shown. From figure 1 It can be seen that the fluorescence intensity is the highest when the milling speed is 500r / min.

Embodiment 2

[0033] In this embodiment, "cesium bromide+lead bromide+potassium bromide", "cesium stearate+lead bromide+potassium bromide", "cesium stearate+lead stearate+potassium bromide", Several combinations of "cesium carbonate + lead bromide + potassium bromide" are used as perovskite sources. Wherein the molar ratio of Cs source, Pb source, Br source and the quality of perovskite source are the same as that of Example 1, that is, the molar ratio of Cs source, Pb source and Br source is 1:1:3, and the quality of perovskite source accounts for 1.5% of the total mass ; The ball milling speed of the present embodiment is 500r / min, and the ball milling time is 1 hour. Finally get CsPbBr 3 PQDs / PMMA luminescent material.

[0034] Separate and sieve the luminescent material from the grinding ball, measure the fluorescence spectrum, see figure 2 . Such as figure 2 As shown, CsPbBr with the combination of "cesium stearate + lead bromide + potassium bromide" as the source of perovskite...

Embodiment 3

[0036] In this embodiment, cesium stearate, lead bromide, and potassium bromide are used as perovskite sources, and the molar ratio of cesium stearate, lead bromide, and potassium bromide is 1:1:3. The molecular materials are mixed, and the mass of the perovskite source is controlled to account for 0.5%, 0.75%, 1.0%, and 1.25% of the total mass. Put the mixture into a 100mL ball mill jar, add 2mm, 4mm and 8mm combined zirconia balls, and mill in a planetary ball mill with a milling speed of 500r / min. After milling for 1 hour, CsPbBr was obtained. 3 PQDs / PMMA luminescent material.

[0037] Separate and sieve the luminescent material from the grinding ball, measure the fluorescence spectrum image 3 shown. From image 3 It can be seen that with the increase of the mass of the perovskite source, the intensity of the fluorescence spectrum increases first, then decreases, and reaches the maximum when the mass of the perovskite source is 0.75%.

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Abstract

The invention discloses a method for preparing high-stability CsPbBr3 quantum dots by a solvent-free and ligand-free ball milling method, which comprises the following steps: mixing a Cs source, a Pb source and a Br source according to a molar ratio of 1: (1-6): (1-9), adding PMMA (polymethyl methacrylate) to obtain a mixture, and ball-milling the mixture at 360-630r / min for 1-2 hours to obtain a product CsPbBr3 quantum dots; wherein the Cs source is cesium bromide or cesium stearate, the Pb source is lead bromide or lead stearate, and the Br source is potassium bromide; the total mass of the Cs source, the Pb source and the Br source accounts for 0.5%-2.5% of the total mass of the Cs source, the Pb source, the Br source and the PMMA. The method is simple in process and easy for industrial production; solvents and organic ligands are not used, so that the cost is saved and environmental protection is facilitated; the quantum yield of the product is high and is as high as 78%; the product is high in environmental stability, and the emission intensity is not attenuated after the product is placed in air for one year; the preparation temperature is low, high-temperature treatment is not needed, and the reaction can be completed at room temperature.

Description

technical field [0001] The invention belongs to the technical field of preparation of perovskite quantum dots, in particular to a solvent-free and ligand-free ball milling method for preparing high-stability CsPbBr 3 method of quantum dots. Background technique [0002] In recent years, lead halide perovskite quantum dots (APbX 3 PQDs, A=Cs + 、MA + 、FA + ,X=Cl - 、Br - , I - ) has attracted people's attention and research because of its excellent photoelectric properties. Compared with traditional II-VI inorganic semiconductor quantum dots (CdSe, etc.), PQDs have the advantages of wider adjustable emission wavelength range, excellent photoelectric transmission performance, simple synthesis, and low cost. They are used in light-emitting diodes (LEDs) and solar cells , laser and other fields have broad application prospects. However, its poor long-term stability to ultraviolet light, heat, and moisture limits its development. [0003] At present, the main preparation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/66C09K11/02B82Y40/00B82Y20/00
CPCC09K11/665C09K11/025B82Y20/00B82Y40/00C08F20/14C09K11/02C08K3/16C01G21/006B82Y30/00C01P2002/34
Inventor 谢会东刘伟汪志腾杨厂
Owner XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY