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Cs2AgBiBr6 double perovskite and preparation method thereof

A double perovskite and anti-solvent technology, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of strong corrosion of the solution, low concentration of precursors, and impure synthetic products, etc., to achieve high solubility and improve the quality of precursors Concentration, the effect of avoiding component segregation

Active Publication Date: 2018-09-21
HUAZHONG UNIV OF SCI & TECH
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Problems solved by technology

[0005] Aiming at the above defects or improvement needs of the prior art, the present invention provides a Cs 2 AgBr 6 Double perovskite and its preparation method, thereby solving the existing Cs in the prior art 2 AgBr 6 In the acid solvent system, the concentration of the precursor is low, the solution is highly corrosive, resulting in low synthesis efficiency, and the technical problems of impure synthetic products in the organic solvent system

Method used

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  • Cs2AgBiBr6 double perovskite and preparation method thereof
  • Cs2AgBiBr6 double perovskite and preparation method thereof
  • Cs2AgBiBr6 double perovskite and preparation method thereof

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preparation example Construction

[0029] Such as figure 1 As shown, a Cs 2 AgBr 6 The preparation method of double perovskite, comprising:

[0030] (1) After mixing cesium bromide, silver bromide and bismuth tribromide according to the molar ratio of 2:1:X, they are dissolved in an organic solvent, the temperature during dissolution is 50°C-70°C, and the organic solvent is DMF, DMSO or Mix the solution in any ratio to obtain the precursor solution;

[0031](2) Add anti-solvent dropwise to the precursor solution. The anti-solvent is dichloromethane, chlorobenzene or turpentine permeate alcohol, and the solution precipitates a white precipitate, so that the volume ratio of the precursor solution and the anti-solvent is 1: Y, and the segregation crystals are removed. (white precipitate), at this moment, orange color appeared in the precipitate, and the dropwise addition was stopped immediately to obtain a solid-liquid mixture;

[0032] (3) After the solid-liquid mixture is centrifuged, get the supernatant liq...

Embodiment 1

[0036] a Cs 2 AgBr 6 The preparation method of double perovskite, comprising:

[0037] 1. Weigh 0.212g CsBr, 0.0939g AgBr and 0.224g BiBr 3 (the molar ratio is 2:1:1), dissolved in 5ml of DMF, heated and stirred at 60°C for about 2 hours to obtain a 0.1mol / L CABB precursor solution.

[0038] 2. Wash the glass bottles and centrifuge tubes with deionized water solution of detergent, acetone, isopropanol and ethanol for 10 minutes, and dry them in an oven.

[0039] 3. Take 5ml of precursor solution in a centrifuge tube, and then take 10ml of dichloromethane (the volume ratio of precursor to anti-solvent is 1:2).

[0040] 4. Add dichloromethane dropwise to the precursor solution, shake while dropping, and the solution precipitates a white precipitate. After continuous dropwise addition to 10ml of dichloromethane, the precipitate appeared orange, and the dropwise addition was stopped immediately.

[0041] 5. Centrifuge at 3000 rpm for 5 minutes, take the supernatant and put it...

Embodiment 2

[0046] a Cs 2 AgBr 6 The preparation method of double perovskite, comprising:

[0047] 1. Weigh 0.212g CsBr, 0.0939g AgBr and 0.448g BiBr 3 (the molar ratio is 2:1:2), dissolved in 5 ml of a 1:1 mixed solvent of DMF and DMSO, heated and stirred at 50°C for about 2 hours to obtain a CABB precursor solution.

[0048] 2. Wash the glass bottles and centrifuge tubes with deionized water solution of detergent, acetone, isopropanol and ethanol for 10 minutes, and dry them in an oven.

[0049] 3. Take 5ml of precursor solution in a centrifuge tube, and then take 7ml of chlorobenzene (the volume ratio of precursor to anti-solvent is 1:1.4).

[0050] 4. Add chlorobenzene dropwise to the precursor solution, oscillate while dropping, and the solution precipitates a white precipitate. After continuous dropwise addition to 7ml of chlorobenzene, the precipitate appeared orange, and the dropwise addition was stopped immediately.

[0051] 5. Centrifuge at 3000 rpm for 5 minutes, take the ...

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Abstract

The invention discloses Cs2AgBiBr6 double perovskite and a preparation method thereof. The preparation method is characterized in that a two-step crystallization process is introduced to avoid the component segregation phenomenon of Cs2AgBiBr6 perovskite in an organic solvent. The preparation method mainly comprises the following steps: titrating a precursor solution by using an anti-solvent, removing early crystallization by-products and taking clear liquid subjected to centrifugal separation as a crystal growth solution for the Cs2AgBiBr6 perovskite; then slowly synthesizing a Cs2AgBiBr6 perovskite material thorough the anti-solvent crystallization process. The preparation method of the Cs2AgBiBr6 double perovskite, disclosed by the invention, can effectively avoid the segregation phenomenon caused by different solubilities of components. Compared with acid as a solvent, the organic solvent has the advantages of greater solubility, lower requirements on sealing and corrosion resistance of containers; the synthesis efficiency can be significantly improved.

Description

technical field [0001] The invention belongs to the field of perovskite materials, more specifically, relates to a Cs 2 AgBr 6 Double perovskite and its preparation method. Background technique [0002] Currently Cs 2 AgBr 6 As a new type of semiconductor material, double perovskites have achieved excellent performance in the fields of radiation detection, photovoltaic cells, and photoelectric detection. The main synthesis method uses hydrobromic acid as a solvent to dissolve the precursor solution, and prepares Cs 2 AgBr 6 double perovskite. Since this method uses acid as a solvent, the strong corrosiveness of acid limits the selection of materials and substrate materials for the synthesis container, while Cs 2 AgBr 6 The solubility in acid is very low and the cooling process is slow, the material preparation process takes a long time and the production efficiency is low. [0003] Preparation of Cs by organic solvents such as DMF and DMSO 2 AgBr 6 The precursor so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/74
CPCC09K11/7435
Inventor 唐江牛广达尹力骁潘伟程巫皓迪
Owner HUAZHONG UNIV OF SCI & TECH
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