Method for synthesizing CsSnX3 perovskite quantum dots by microwave-assisted heating

A microwave-assisted, quantum dot technology, applied in the field of semiconductor and nanotechnology, can solve the problems of uneven heat transmission speed and distribution, temperature display accuracy error, low fluorescence yield of quantum dots, etc., to achieve short preparation cycle, heating and cooling The effect of high speed and high fluorescence quantum yield

Active Publication Date: 2017-09-26
HUIZHOU DESIKUN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the CsSnX prepared by this method 3 Low fluorescence yield of quantum dots (<1%)
This is because the traditional heating method of the heat injection method uses a heating mantle to heat, and uses heat conduction, heat convection, and heat radiation to transfer heat from the outside to the reaction solution. Due to the

Method used

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  • Method for synthesizing CsSnX3 perovskite quantum dots by microwave-assisted heating
  • Method for synthesizing CsSnX3 perovskite quantum dots by microwave-assisted heating
  • Method for synthesizing CsSnX3 perovskite quantum dots by microwave-assisted heating

Examples

Experimental program
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Effect test

Embodiment 1

[0022] In an inert atmosphere, the tin halide (SnX 2 ) Was placed in trioctyl phosphine (TOP), stirred, vacuumed at the same time and heated to 100 ℃, kept until SnX2 was completely dissolved to obtain a precursor solution with a molar concentration of 0.5M tin; the cesium carbonate (Cs 2 CO 3 ), oleic acid (OA) and oleylamine (OAm) in a molar ratio of 1:0.375:0.375, added to the mixed solvent of octadecene (ODE) and glycerol with a volume ratio of 1:3, and then placed in microwave heating In the device, stir, evacuate, heat up to 60°C, keep it warm until it is dissolved, and obtain a precursor solution with a molar concentration of 0.5M cesium; then pass inert gas into the cesium precursor solution, stop vacuuming, and continue to raise When the temperature reaches 150~190℃, quickly inject tin precursor solution, stop microwave heating after 1 min of reaction, and place in an ice water bath to quickly cool down; add methyl acetate or tert-butanol, centrifuge, and then wash with ...

Embodiment 2

[0026] In an inert atmosphere, the tin halide (SnX 2 ) Is placed in trioctyl phosphine (TOP), stirring, while vacuuming and heating to 150 ℃, heat preservation to SnX 2 Dissolve completely to obtain a precursor solution with a molar concentration of 1.5M tin; add cesium carbonate (Cs 2 CO 3 ), oleic acid (OA) and oleylamine (OAm) are added to the mixed solvent of octadecene (ODE) and silicon balls with a volume ratio of 1:5 in a molar ratio of 1:0.375:0.375, and then placed in the microwave In the heating device, stir, evacuate, and raise the temperature to 100°C, keep it warm until it is dissolved, and obtain a precursor solution with a molar concentration of 1.5M cesium; then pass inert gas into the cesium precursor solution, stop vacuuming, and continue Raise the temperature to 150~190℃, quickly inject tin precursor solution, stop microwave heating after 5 minutes of reaction, and place in an ice water bath to quickly cool down; add methyl acetate or tert-butanol, centrifuge, ...

Embodiment 3

[0030] In an inert atmosphere, the tin halide (SnX 2 ) Is placed in trioctyl phosphine (TOP), stirring, while vacuuming and heating to 120 ℃, heat preservation to SnX 2 Dissolve completely to obtain a precursor solution with a molar concentration of 0.8M tin; add cesium carbonate (Cs 2 CO 3 ), oleic acid (OA) and oleylamine (OAm) are added to the mixture of octadecene (ODE) and polar solvent (glycerol silica ball mixture) at a molar ratio of 1:0.375:0.375 with a volume ratio of 1:4 In the solvent, it is then placed in a microwave heating device, stirred, vacuumed, and heated to 90°C, kept until dissolved, to obtain a precursor solution with a molar concentration of 0.8M cesium; then pass inert gas into the cesium precursor solution, And stop vacuuming, and then continue to raise the temperature to 150~190℃, quickly inject tin precursor solution, stop microwave heating after 2 minutes of reaction, and place in an ice water bath to quickly cool down; add methyl acetate or tert-buta...

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Abstract

The invention discloses a method for synthesizing CsSnX3 perovskite quantum dots by microwave-assisted heating, and belongs to the field of semiconductor and nanotechnology. The method comprises the steps: adding cesium carbonate (Cs2CO3), oleic acid (OA) and oleylamine (OAm) according to the molar ratio of 1 to 0.375 to 0.375 to a mixed solvent mixed by octadecene (ODE) and a polar solvent with a volume ratio of (1:3) to (1:5), then placing into a microwave heating apparatus, stirring and vacuumizing, raising the temperature to be 60 to 100 DEG C, preserving heat to be dissolved, obtaining a cesium precursor solution with a molar concentration of 0.5 to 1.5M; introducing inert gas, raising the temperature to be 150 to 190 DEG C, injecting quickly a halide tin (SnX2) trioctylphosphine (TOP) solution, reacting for 1 to 5min, adding methyl acetate or tert-butanol after cooling, centrifuging, washing with n-hexane for 3 to 5 times, and obtaining CsSnX3 quantum dot powder after drying. According to the method for synthesizing the CsSnX3 perovskite quantum dots by microwave-assisted heating, the temperature distribution of the reaction temperature field is uniform and precisely controllable, the heating and cooling speed is fast, the preparation period is short and the yield is high; the quantum point has high crystallinity, less surface defects, uniform size distribution, high fluorescence quantum yield and high safety.

Description

Technical field [0001] The invention belongs to the field of semiconductor and nanotechnology, and specifically relates to the synthesis of CsSnX by microwave assisted heating 3 The method of perovskite quantum dots. Background technique [0002] Quantum dots (QD), also known as colloidal semiconductor nanocrystals (NCs, usually 2-20nm large), because of their unique properties such as quantum confinement effect and quantum size effect, they exhibit excellent optoelectronic properties and have a wide range of Application potential and prospects. Compared with traditional nanocrystals and organic dyes, quantum dot materials have a wide excitation region and a narrower emission spectrum. The fluorescence spectrum can be distributed in the entire visible light range, so it has stronger light absorption and stable light emission performance. The stability of the fluorescence intensity of quantum dots is also better than that of traditional organic fluorescent dyes, the fluorescence...

Claims

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Application Information

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IPC IPC(8): C09K11/66B82Y40/00
Inventor 田建军毕成浩郭瑞琪
Owner HUIZHOU DESIKUN CHEM CO LTD
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