Preparation method of stable lead-free all-inorganic double perovskite A2BB'X6 nanocrystals

A double perovskite, nanocrystal technology, applied in inorganic chemistry, nanotechnology, chloride preparation, etc., can solve the problems of low stability, narrow size distribution of nanocrystals, good dispersibility, etc., and achieve high stability and method. Simple, good dispersion effect

Active Publication Date: 2018-04-20
SUN YAT SEN UNIV
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  • Description
  • Claims
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Problems solved by technology

[0006] In order to overcome the low stability problem in the existing lead-free perovskite nanocrystalline materials, the object of the present invention is to provide a stable lead-free double perovskite A 2 BB’X 6 The preparation...

Method used

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  • Preparation method of stable lead-free all-inorganic double perovskite A2BB'X6 nanocrystals
  • Preparation method of stable lead-free all-inorganic double perovskite A2BB'X6 nanocrystals
  • Preparation method of stable lead-free all-inorganic double perovskite A2BB'X6 nanocrystals

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Embodiment 1

[0034] A stable lead-free double perovskite A 2 BB’X 6 A method for preparing nanocrystals, comprising the steps of:

[0035] Step 1, 45mg BiBr 3 , 17mg AgNO 3 , 0.1mL HBr, 1mL oleic acid, 1mL oleylamine and 4mL octadecene were mixed simultaneously, heated and stirred under vacuum at 120°C for 1h to ensure that the water and gas in the system were removed, and then heated under N 2 Heated to 200°C under protection to obtain a clear and transparent solution.

[0036] Step 2, 0.814g Cs 2 CO 3 , 40mL of octadecene and 2.5mL of oleic acid were added to a 100mL three-neck flask at the same time, and then stirred under vacuum at 120°C for 1h to make Cs 2 CO 3 Fully react with oleic acid to obtain a clear and transparent octadecene solution of cesium oleate; 0.8mL of the cesium oleate solution obtained is quickly injected into the precursor solution prepared in step 1), and after reacting for 5s, the system ice bath is cooled to room temperature.

[0037] Step 3, centrifuge at...

Embodiment 2

[0041] Synthesize Cs using the preparation method described 2 AgBr 6 Nanocrystals, and then washed with a low-polarity solvent to remove the ligands on the surface of the nanocrystals, applied to the photocatalytic reduction of CO 2 .

[0042] To the 4mLCs prepared in embodiment 1 2 AgBr 6 Add 2 mL of absolute ethanol to the nanocrystal dispersion, shake and wash the mixed system for 30 s, and then centrifuge at 12,000 rpm for 5 min to obtain a yellow precipitate in the lower layer. The washing process is repeated twice. Finally, the surface ligand was washed and treated with Cs 2 AgBr 6 Nanocrystalline.

[0043] The Cs obtained in this example 2 AgBr 6 Nanocrystals were at 55% relative humidity, 70mW·cm -2 The stability test was carried out under the light conditions and the high temperature environment of 100 ℃.

[0044] pass Figure 5 The XRD results show that Cs 2 AgBr 6 The nanocrystals are stable for more than 90 days at 55% relative humidity. At 70mW·cm -...

Embodiment 3

[0047] A stable lead-free double perovskite A 2 BB’X 6 A method for preparing nanocrystals, comprising the steps of:

[0048] Step 1, 45mg BiBr 3 , 17mg AgNO 3 , 0.1mL HBr, 1mL oleic acid, 1mL oleylamine and 4mL octadecene were mixed simultaneously, heated and stirred under vacuum at 120°C for 0.5h to ensure that the water and gas in the system were removed, and then heated under N 2 Heated to 200°C under protection to obtain a clear and transparent solution.

[0049] Step 2, 0.814g Cs 2 CO 3 , 40mL of octadecene and 2.5mL of oleic acid were added to a 100mL three-neck flask at the same time, and then stirred under vacuum at 120°C for 1h to make Cs 2 CO 3 Fully react with oleic acid to obtain a clear and transparent octadecene solution of cesium oleate. Take 0.8 mL of the obtained cesium oleate solution and quickly inject it into the precursor solution prepared in step 1), and after reacting for 5 seconds, quickly cool the system down to room temperature in an ice bath...

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Abstract

The invention discloses a preparation method of stable lead-free all-inorganic double perovskite A2BB'X6 nanocrystals. The method adopts a thermal injection technology to synthesize the nanocrystals,and concretely comprises the following steps: mixing a metal precursor salt, a reaction solvent oleic acid, oleylamine, octadecene and other raw materials, carrying out vacuum heating and stirring ata certain temperature for a certain period of time, rising the temperature to a suitable reaction temperature under the protection of N2, rapidly injecting the obtained hot oleate solution of A into areaction system, and then rapidly cooling the system to room temperature by using ice bath to finally obtain the A2BB'X6 perovskite nanocrystals having a uniform size. The method has the advantages of simplicity, convenient, good reappearance and environmental protection, and the obtained product has the advantages of uniform size, good dispersion, high stability and excellent photocatalytic performance, and can be applied to the fields of photocatalysis, photodetectors, laser, solar cells and the like.

Description

technical field [0001] The invention belongs to the field of preparation and photoelectric application of novel nanomaterials, and specifically relates to a 2 BB’X 6 Preparation method of lead-free double perovskite nanocrystalline material. Background technique [0002] Since 2014, perovskite nanocrystalline materials represented by lead methylamine halide and lead cesium halide have been widely used due to their tunable band gap, high exciton binding energy, high carrier mobility, and easy and convenient solution phase. The preparation process has received extensive attention. At the same time, they have shown potential application prospects in many fields such as light-emitting diodes (LEDs), solar cells, photodetectors, and lasers. However, the toxicity and environmental pollution of metal Pb elements limit the industrial application of this type of perovskite nanocrystalline materials in the future, so non-toxic elements such as Sn, Bi, Sb, etc. are used to partially...

Claims

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Application Information

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IPC IPC(8): C01B9/02C01B9/04C01B9/06C01G29/00B82Y40/00B01J27/138C07C9/04C07C1/02C01B32/40
CPCB01J27/138B01J35/0013B01J35/004B01J35/006B82Y40/00C01B9/02C01B9/04C01B9/06C01G29/006C01P2002/72C01P2004/04C01P2004/51C01P2004/64C07C1/02C07C9/04C07C2527/138
Inventor 匡代彬周磊陈白雪徐杨帆苏成勇
Owner SUN YAT SEN UNIV
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