Silicon dioxide coated caesium-lead-bromine-perovskite nanocrystal compound and microwave assisted heating synthesis method thereof

A microwave-assisted, synthetic method technology, applied in chemical instruments and methods, nanotechnology, nano-optics, etc., can solve the problems of poor fluorescence performance, poor reproducibility, time-consuming, etc., and achieve fast heating efficiency and high thermal energy utilization rate. Effect

Active Publication Date: 2018-09-14
MINNAN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above-mentioned SiO2 coating provides a good idea for improving the stability of PNCs. However, there are still two problems in the coating process of PNCs: (1) The controllable release of water is currently mainly based on the release of water in solvents or in the air. Water molecules are hydrolyzed, the process is often affected by the purity of the reagents and changes in the weather, the reproducibility is poor, and time-consuming; (2) The fluorescence properties of PNCs are greatly affected by the hydrolyzed product alcohol, which often leads to fluorescence properties becomes worse, so how to achieve SiO on PNCs 2 Efficient coating is of great significance

Method used

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  • Silicon dioxide coated caesium-lead-bromine-perovskite nanocrystal compound and microwave assisted heating synthesis method thereof
  • Silicon dioxide coated caesium-lead-bromine-perovskite nanocrystal compound and microwave assisted heating synthesis method thereof
  • Silicon dioxide coated caesium-lead-bromine-perovskite nanocrystal compound and microwave assisted heating synthesis method thereof

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Experimental program
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Effect test

Embodiment 1

[0035] Discussion on Optimum Synthesis Temperature and Time

[0036] Add 16.3mg Cs to the reaction tube sequentially 2 CO 3 , 38.7mg of lead stearate, 71.6mg of TBB, 5mL of ODE and 0.28ml of APTES, then add a small stirring bar and cover with a PEEK card cover, and finally put it into the reaction chamber of the microwave synthesizer. Discuss the reaction conditions at different temperatures of 80, 100, 120, 140, and 160°C (reaction time is 6 minutes, and the rotation speed is 1200 rpm); at the above optimal temperature, discuss the reaction conditions of different reaction times of 3 minutes, 6 minutes, 9 minutes, and 12 minutes .

[0037] Since CsPbBr 3 The formation energy is very low, so rapid temperature rise is conducive to faster nucleation and growth, thereby obtaining better optical properties. During the experiment, it was found that when the temperature was lower than 140°C, the precursor did not react completely, and when the temperature reached 140°C, a bright...

Embodiment 2

[0039] Discussion on Precursor Ratio

[0040] First add 5 mL of octadecene solution to the reaction tube, and then accurately add different amounts of Cs 2 CO 3 , lead stearate, TBB and APTE in the reaction tube, so that the molar ratio Cs 2 CO 3 : lead stearate: TBB: APTE=1:1:3:1, other ratios such as 2:1:3:1, in the optimal reaction temperature and the time that embodiment 1 determines, explore different precursor ratios to impact on product performance.

[0041] By optimizing the ratio of different precursors, it was found that when Cs 2 CO 3 CsPbBr synthesized at 32.4mg, 38.7mg of lead stearate, 71.6mg of TBB and 280uL of APTES 3 @SiO 2 The effect is the best, and its dispersion and fluorescence properties are obviously better than other ratios. Such as Figure 4 As shown, when APTES is 280uL, CsPbBr 3 @SiO 2 There is no obvious precipitation, indicating that the particles are relatively small and uniform. In addition, the fluorescence performance under the ultr...

Embodiment 3

[0043] CbBr 3 @SiO 2 Microwave-assisted heating synthesis method of perovskite nanocrystalline composite:

[0044] Add 32.4mg Cs to the reaction tube sequentially 2 CO 3 , 38.7mg lead stearate, 71.6mg TBB, 5mL octadecene and 280uL APTES, then add a magnetic stirrer, and finally place the reaction tube in the reaction chamber of a microwave synthesizer, and react at 140°C for 6min to obtain CsPbBr 3 @SiO 2 Perovskite nanocrystalline composites;

[0045] CbBr 3 @SiO 2 The structural properties and their fluorescence properties are characterized as Figure 6 As shown, among them, Figure 6 (a) is CsPbBr 3 @SiO 2 XRD spectrum; Figure 6 (b) is CsPbBr 3 @SiO 2 Fluorescence spectrum (gained product CsPbBr 3 @SiO 2 Fluorescent picture under UV-365nm ultraviolet lamp irradiation); Figure 7 (a, b) is CsPbBr 3 @SiO 2 TEM and its HRTEM map; Figure 8 CsPbBr 3 @SiO 2 EDS diagram.

[0046] From Figure 6 (a) The XRD spectrum shows that 15°, 21°, 31°, 33°, 37° and 43...

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Abstract

The invention discloses silicon dioxide coated caesium-lead-bromine-perovskite nanocrystal compound and a microwave assisted heating synthesis method thereof. Through a microwave assisted heating way,1,3,5-tri(bromomethyl)benzene, 3-aminopropyl triethoxysilane, lead stearate and cesium carbonate are taken as precursors, and octadecene is taken as a solvent to synthesize CsPbBr3@SiO2 perovskite nanocrystal compound. Compared with CsPbBr3PNCs, the prepared CsPbBr3@SiO2 perovskite nanocrystal compound has very good light-emitting performance. The method has very good repeatability, and providesa brand-new idea for SiO2 coating of CsPbBr3PNCs.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to cesium lead bromide (CsPbBr) coated with silicon dioxide 3 @SiO 2 ) perovskite nanocrystalline composite and its microwave-assisted heating synthesis method. Background technique [0002] Lead-based perovskite nanocrystals (perovskite nanocrystals, PNCs) are a kind of ABX 3 Ionic compounds of chemical composition, where A + is a monovalent cation (such as CH 3 NH 3 + or Cs + ), B 2+ for Pb 2+ , X - is a halide ion (Cl - 、Br - , I - ). Since its development in 2014, the synthesis and application of lead-based PNCs has attracted widespread attention. In addition to the advantages of traditional quantum dots, lead-based PNCs also have the advantages of mild synthesis conditions (synthesis at room temperature), less light flicker, good defect tolerance, and less affected by particle size. In addition to the regulation of particle size, the emission wavelengt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/66C09K11/02B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C09K11/025C09K11/665
Inventor 陈碧桑
Owner MINNAN NORMAL UNIV
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