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Preparation method of tetraethoxysilane-coated perovskite nanocrystals

A technology of ethyl orthosilicate and perovskite, which is applied in the fields of nanotechnology, nanotechnology, nano-optics for materials and surface science, and can solve the problems of unstable nanocrystals, easy decomposition and deterioration, and limited wide application.

Active Publication Date: 2021-04-20
WENZHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Despite the high quantum efficiency of nanocrystals synthesized by thin-film method, CsPbX 3 Nanocrystals are extremely unstable when exposed to air and water, and are easy to decompose and deteriorate, which seriously limits their wide application.
Thin films protect perovskite nanocrystals better than solutions but still weaker than stable powder structures

Method used

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  • Preparation method of tetraethoxysilane-coated perovskite nanocrystals
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  • Preparation method of tetraethoxysilane-coated perovskite nanocrystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: CsPbBr 3 Preparation of NCs

[0034] (1-1) Preparation of the precursor: a 100ml three-necked flask was filled with CsCO 3 0.5g, ODE (1-octadecene) 15ml, OA (oleic acid) 3ml, raise the temperature to 120°C and keep it for 60min, then raise the temperature to 150°C for use; the whole process is under N 2 Under the atmosphere.

[0035] (1-2) Preparation of perovskite nanocrystals:

[0036] PbBr was charged into another three-necked flask 2 0.3mmol and ODE (1-octadecene) 15ml, raise the temperature to 120°C and keep it for 60min, then add 0.5ml OA (oleic acid) and 0.5ml OAm (oleylamine), and raise the temperature to 150°C ℃, after the solid is completely dissolved, quickly inject 0.5ml of the precursor solution into the mixed solution, react for 10s and put it in ice water to cool to room temperature; the whole process is under N 2 Under the atmosphere.

[0037] (1-3) Purification treatment of perovskite nanocrystals:

[0038] Centrifuge the cooled perovski...

Embodiment 2-6

[0039] Example 2-6: Preparation of perovskite nanocrystals coated with orthosilicate

[0040] Get the perovskite CsPbX that embodiment 1 prepares 3 Nanocrystalline dispersion 2, add different volumes of ethyl orthosilicate to it respectively, so that the volume of orthosilicate accounts for the volume of perovskite CsPbX 3 25% (embodiment 2), 33% (embodiment 3), 50% (embodiment 4), 67% (embodiment 5), 75% (embodiment 6) of the dispersion liquid volume of nanocrystal, stir 3min to make After mixing evenly, dry in an oven at 60°C for 10 hours to obtain perovskite nanocrystals QDs@0.25TEOS (Example 2), QDs@0.33TEOS (Example 3), and QDs@0.5TEOS coated with orthosilicate (Example 4), QDs@0.67TEOS (Example 5), QDs@0.75TEOS (Example 6).

[0041] figure 1 It is the X-ray diffraction (XRD) pattern of a series of perovskite nanocrystals coated with tetraethyl orthosilicate prepared in Example 2-6, wherein S1 is QDs@0.25TEOS, S2 is QDs@0.33TEOS, and S3 is QDs@0.5TEOS, S4 is QDs@0.67T...

Embodiment 11

[0053] Embodiment 11: Stability experiment

[0054] The perovskite CsPbBr that 2mL embodiment 1 prepares 3 The nanocrystal dispersion 2 was transferred to a cuvette, and the fluorescence intensity at this time was measured. Then place the cuvette in an ultrasonic cleaning machine for 30 minutes to measure the fluorescence intensity after ultrasonication. For comparison of fluorescence intensity, see Figure 7-a .

[0055] With the CsPb that embodiment 4 obtains 2 x 5 Transfer 0.2 g of sample powder @50% TEOS to a cuvette, add 2 ml of ultrapure water, and measure the fluorescence intensity at this time. Then place the cuvette in an ultrasonic cleaning machine for 30 minutes to measure the fluorescence intensity after ultrasonication. For comparison of fluorescence intensity, see Figure 7-b .

[0056] With the CsPb that embodiment 5 obtains 2 x 5 Transfer 0.2 g of sample powder @67% TEOS to a cuvette, add 2 ml of ultrapure water, and measure the fluorescence intensity...

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Abstract

The invention discloses a preparation method of tetraethoxysilane-coated perovskite nanocrystals, which comprises the following steps: (1) obtaining a dispersion liquid of perovskite CsPbX3 nanocrystals, X represents halogen, the concentration of the perovskite CsPbX3 nanocrystals in the dispersion liquid is 1-5wt%, and a solvent is n-hexane and / or toluene; and (2) adding tetraethoxysilane into the dispersion liquid of the perovskite CsPbX3 nanocrystals in the step (1) to enable the volume ratio of the dispersion liquid of the perovskite CsPbX3 nanocrystals to the tetraethoxysilane to be 100:(10-90), fully conducting mixing, and conducting drying in a drying oven to obtain the tetraethoxysilane-coated perovskite nanocrystals. The preparation method is short in preparation time, raw materials are easy to obtain, batch production is easy, and the prepared tetraethoxysilane-coated perovskite nanocrystalline has the outstanding advantages of being good in optical performance, good in light stability and adjustable in component.

Description

technical field [0001] The invention relates to a perovskite nanocrystal coated with tetraethyl orthosilicate and a preparation method thereof, belonging to the field of research on nanocrystal coating. Background technique [0002] Due to the advantages of all-inorganic lead-cesium halide perovskite nanocrystals with tunable wavelength, wide absorption range, tunable band gap, and high quantum efficiency, they have attracted extensive attention. CaB 3 The preparation methods of nanocrystals include solution hot injection synthesis and ion exchange. CN201710783608.X discloses a water-soluble CsPbX 3 The preparation method of perovskite nano crystals is to disperse them in an organic solvent for stable protection, and obtain polymer ions after centrifugation. Obtaining perovskite particles that can emit light and have high quantum efficiency has great application value in biological applications, display and other fields. CN201910202479.X discloses a small grain CsPbX ind...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/66C01G21/00B82Y20/00B82Y30/00B82Y40/00
Inventor 向卫东周宇峰梁晓娟
Owner WENZHOU UNIVERSITY
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