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Preparation method of color-adjustable small-size Mn: CsPbCl3 nanocrystal

A nanocrystal, small size technology, applied in nanotechnology, nano optics, nanotechnology, etc., can solve the problems of inability to obtain small size doped nanocrystals, large nanocrystal size, uncontrollable size, etc., and achieve good monodispersity. , the reaction operation is simple, the effect of reducing production costs

Inactive Publication Date: 2018-09-28
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this high-temperature synthetic method makes the size of the nanocrystals larger and uncontrollable, and it is impossible to obtain small-sized doped nanocrystals; Dissolve in DMF under the action of oleylamine and other ligands to form a mixed solution, and then inject it into the acetone solution together with the manganese dichloride solution dissolved in DMF, and stir vigorously
This method has mild reaction conditions, but the reaction time is too long (40h), the manganese-doped fluorescence is yellow-orange light and the fluorescence efficiency is low, which has certain limitations in application.

Method used

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  • Preparation method of color-adjustable small-size Mn: CsPbCl3 nanocrystal
  • Preparation method of color-adjustable small-size Mn: CsPbCl3 nanocrystal
  • Preparation method of color-adjustable small-size Mn: CsPbCl3 nanocrystal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] First, weigh 2 mmol of cesium carbonate, 2.5 mL of oleic acid, and 17.5 mL of octadecene in a three-necked flask, vacuumize at 120°C, heat up to 150°C under nitrogen protection, dissolve to form a 0.2M cesium oleate solution, and drop to Set aside at room temperature.

[0027] Then, weigh 0.6mmol of lead chloride, 1.5mL of oleic acid, 1.5mL of oleylamine, and 6mL of octadecene in a three-necked flask, vacuumize at 120°C, and add 1.5mL of trioctylphosphine under the protection of nitrogen. Dissolve at 150°C to form a mixed solution, lower the ice-water bath to room temperature, inject 0.6mL cesium oleate solution, and react for 1 hour to obtain CsPbCl 3 Perovskite nanocrystal seeds, and then heated to 60 ° C for 10 minutes to obtain 2nm CsPbCl 3 Perovskite nanocrystals.

[0028] Finally, 2nm CsPbCl 3 The mother liquor of perovskite nanocrystals is directly put into a centrifuge for 8000rpm5min centrifugal purification, the supernatant is discarded, and the obtained 0....

Embodiment 2

[0030] First, weigh 2 mmol of cesium carbonate, 2.5 mL of oleic acid, and 17.5 mL of octadecene in a three-necked flask, vacuumize at 120°C, heat up to 150°C under nitrogen protection, dissolve to form a 0.2M cesium oleate solution, and drop to Set aside at room temperature.

[0031] Then, weigh 0.6mmol of lead chloride, 1.5mL of oleic acid, 1.5mL of oleylamine, and 6mL of octadecene in a three-necked flask, vacuumize at 120°C, and add 1.5mL of trioctylphosphine under the protection of nitrogen. Dissolve at 150°C to form a mixed solution, lower the ice-water bath to room temperature, inject 0.6mL cesium oleate solution, and react for 1 hour to obtain CsPbCl 3 Perovskite nanocrystal seeds, and then heated up to 140°C for 10 minutes to obtain 3nm CsPbCl 3 Perovskite nanocrystals.

[0032] Finally, 3nm CsPbCl 3The mother liquor of perovskite nanocrystals is directly put into a centrifuge for 8000rpm5min centrifugal purification, the supernatant is discarded, and the obtained 0...

Embodiment 3

[0034] First, weigh 2 mmol of cesium carbonate, 2.5 mL of oleic acid, and 17.5 mL of octadecene in a three-necked flask, vacuumize at 120°C, heat up to 150°C under nitrogen protection, dissolve to form a 0.2M cesium oleate solution, and drop to Set aside at room temperature.

[0035] Then, weigh 0.6mmol of lead chloride, 1.5mL of oleic acid, 1.5mL of oleylamine, and 6mL of octadecene in a three-necked flask, vacuumize at 120°C, and add 1.5mL of trioctylphosphine under the protection of nitrogen. Dissolve at 150°C to form a mixed solution, lower the ice-water bath to room temperature and inject 0.6mL cesium oleate solution to react for 1 hour to obtain nanocrystalline seeds, put the mother liquor of perovskite nanocrystals directly into a high-speed centrifuge for centrifugal purification, and precipitate with 1mL n-hexane Dispersed and injected into octadecene at 120°C to obtain 6.8nm CsPbCl 3 Perovskite nanocrystals.

[0036] Finally, the 6.8nm CsPbCl 3 The mother liquor o...

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Abstract

The invention discloses a preparation method of a color-adjustable small-size Mn: CsPbCl3 nanocrystal and belongs to the technical field of semiconductor nanomaterial preparation. The preparation method comprises weighing lead chloride, oleic acid, oleylamine and octadecene, putting the materials into a three-necked flask, carrying out vacuum-pumping at 120 DEG C, adding trioetylphosphine into thematerials in the nitrogen gas protective atmosphere at 150 DEG C to obtain a mixed solution, cooling the mixed solution to the room temperature, pouring a cesium oleate solution into the mixed solution for a reaction at the room temperature for 1h to obtain a CsPbCl3 nanocrystal seed, preparing lead bismuth chloride perovskite with different sizes from the CsPbCl3 nanocrystal seed, carrying out purification, adding a manganese salt into the perovskite, and carrying out grinding to obtain Mn: CsPbCl3 nanocrystals in different colors. The preparation method can adjust the amaranth of the Mn: CsPbCl3 nanocrystal to red color. The color-adjustable small-size Mn: CsPbCl3 nanocrystal has the controllable size and high fluorescence efficiency. The preparation method has simple processes, utilizes easily available raw materials, realizes large-scale synthesis and has a wide product application prospect.

Description

technical field [0001] The invention belongs to the technical field of semiconductor nanomaterial preparation, and relates to a small-sized Mn:CsPbCl with adjustable color 3 Methods of preparing nanocrystals. Background technique [0002] After the semiconductor material is gradually reduced from the bulk phase to a certain critical size (1-20 nanometers), the volatility of the carriers becomes significant, and the movement will be limited, resulting in an increase in kinetic energy. The corresponding electronic structure is continuous from the bulk phase to The energy level structure becomes a quasi-split discontinuity, a phenomenon known as the quantum size effect. The more common semiconductor nanoparticles, that is, quantum dots, mainly include II-VI, III-V and IV-VI groups. These types of quantum dots are well obeyed by the quantum size effect, and their properties change regularly with the size, for example, the absorption and emission wavelengths change with the siz...

Claims

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Application Information

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IPC IPC(8): C01G21/00B82Y40/00B82Y20/00C09K11/66
Inventor 解仁国李思汪大洋
Owner JILIN UNIV
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