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Preparation method and product of Cs<3>Cu<2>X<5> (X=Cl, Br, I) nanocrystalline

A technology of nanocrystals and heat injection method, which is applied in chemical instruments and methods, copper compounds, inorganic chemistry, etc., can solve the problem of low quantum efficiency of luminescence, and achieve the effect of strong exciton-phonon coupling

Active Publication Date: 2020-06-30
HUAZHONG UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Substituting antimony (Sb) for lead to synthesize Cs 3 Sb 3 x 9 Nanocrystals, although the luminous quantum efficiency is as high as 46%, but the luminous quantum efficiency is still far lower than 100% of lead-containing halogen perovskite nanocrystals

Method used

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  • Preparation method and product of Cs&lt;3&gt;Cu&lt;2&gt;X&lt;5&gt; (X=Cl, Br, I) nanocrystalline
  • Preparation method and product of Cs&lt;3&gt;Cu&lt;2&gt;X&lt;5&gt; (X=Cl, Br, I) nanocrystalline
  • Preparation method and product of Cs&lt;3&gt;Cu&lt;2&gt;X&lt;5&gt; (X=Cl, Br, I) nanocrystalline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Taking X=I as an example, this embodiment may specifically include the following steps:

[0053] (1) Wash two flasks, one is used to synthesize cesium oleate. Get 1.628g of cesium carbonate (Cs 2 CO 3 ) was mixed with 20ml of octadecene (ODE) and 5ml of oleic acid (OA), so that the concentration of cesium oleate after complete reaction was about 0.4mmol / mL. In order to get rid of the air in the reaction bottle, vacuumize it at room temperature for 5 minutes, and then pass in nitrogen gas, so that the nitrogen gas is pumped and filled three times repeatedly. After the air in the reaction bottle is exhausted, fill with nitrogen, make the temperature of the reaction solution rise to 120°C and maintain it for one hour, cesium carbonate can be completely dissolved, and then raise the temperature to 150°C to make cesium carbonate and oleic acid Fully react to generate clear and transparent cesium oleate (CsOA);

[0054] (2) Another flask takes 0.19g cuprous iodide (CuI), ...

Embodiment 2

[0070] In this embodiment, zinc halide is used as an additive instead of indium halide in embodiment 1 for experimentation.

[0071]Taking X=I as an example, this embodiment may specifically include the following steps:

[0072] (1) Wash two flasks, one is used to synthesize cesium oleate. Get 1.628g of cesium carbonate (Cs 2 CO 3 ) was mixed with 20ml of octadecene (ODE) and 5ml of oleic acid (OA), so that the concentration of cesium oleate after complete reaction was about 0.4mmol / mL. In order to get rid of the air in the reaction bottle, vacuumize it at room temperature for 5 minutes, and then pass in nitrogen gas, so that the nitrogen gas is pumped and filled three times repeatedly. After the air in the reaction bottle is exhausted, fill with nitrogen, make the temperature of the reaction solution rise to 120°C and maintain it for one hour, cesium carbonate can be completely dissolved, and then raise the temperature to 150°C to make cesium carbonate and oleic acid Full...

Embodiment 3

[0077] In this embodiment, an experiment is carried out by changing the ratio of the amount of indium halide to cuprous halide in embodiment 1.

[0078] Taking X=I as an example, by adding 0.19g of copper iodide (CuI), 0.99g of indium iodide (InI 3 ), other conditions remain unchanged, and Cs can also be obtained 3 Cu 2 x 5 Nanocrystalline. The purification process of nanocrystals is the same as in Example 1. The fluorescence quantum yield and morphology of the obtained nanocrystalline product are basically consistent with those obtained in Example 1.

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Abstract

The invention belongs to the technical field of perovskite-like nanocrystals. The invention discloses a preparation method of Cs<3>Cu<2>X<5> nanocrystalline and a product. The preparation method comprises the steps that indium halide InX3 or zinc halide ZnX2 is additionally introduced into a precursor solution for preparing Cs<3>Cu<2>X<5> nanocrystalline through a thermal injection method, preparing the Cs<3>Cu<2>X<5> nanocrystalline through a thermal injection method, wherein X is selected from Cl, Br and I. According to the preparation method, a key precursor for regulating and controlling the growth of the nanocrystalline in the preparation method of the nanocrystalline is improved; indium halide or zinc halide is used as an additive in a precursor, and a copper element is used as a substitute of a lead element, so that the preparation of the lead-free metal halide light-emitting nanocrystal is completed, the preparation process is easy to implement, the cost is low, and meanwhile,the defects of the lead-containing halogen perovskite nanocrystal can be overcome.

Description

technical field [0001] The invention belongs to the field of preparation of perovskite-like nanocrystalline nanomaterials, more specifically, relates to a Cs 3 Cu 2 x 5 The preparation method and product of (X=Cl, Br, I) nanocrystals can produce perovskite-like nanocrystal nanomaterials without the toxic element lead by inhibiting the growth of all-inorganic metal halide nanocrystals. Background technique [0002] In recent years, researchers have made breakthroughs in the study of lead-containing halide perovskite nanocrystals, including organic-inorganic metal halide perovskite nanocrystals, such as MAPbBr 3 (MA is methylamine), all-inorganic metal halide perovskite nanocrystals, such as CsPbBr 3 Wait. Because lead-containing halogen perovskite nanocrystals have many excellent properties: such as high luminescence quantum efficiency (PLQY), the highest quantum yield reported so far can reach 100%, and the emission spectrum has a narrow half-peak width (FHWM). , high d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G3/00C09K11/02C09K11/61
CPCC01G3/006C01P2002/72C01P2002/85C01P2004/04C01P2004/64C09K11/025C09K11/616
Inventor 张建兵连霖源郑模艳张伟卓张道礼唐江张秀文
Owner HUAZHONG UNIV OF SCI & TECH
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