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Preparation method and application of lead-free A4MnBi2X12 perovskite material

A perovskite material, a4mnbi2x12 technology, is used in the preparation and application of new materials, which can solve the problems of difficult to guarantee stability, low luminous quantum efficiency, poor stability, etc., and achieve abundant reserves, environmental friendliness, and good thermal stability. Effect

Active Publication Date: 2020-02-11
SUN YAT SEN UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

Therefore, many researchers use elements such as Sn(II) and Ge(II) to replace lead, but both Sn and Ge are easily oxidized, and the stability is difficult to be guaranteed.
Manganese is an effective luminescent center, but most of the current manganese-based luminescent materials are based on organic-inorganic hybrid materials, and organic-inorganic hybrid materials have poor stability, while all-inorganic CsMnCl 3 The luminous quantum efficiency of the material is very low, considering that in CsMnCl 3 Introduce Bi (bismuth) as a photosensitizer to form a new structure of light-emitting materials

Method used

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  • Preparation method and application of lead-free A4MnBi2X12 perovskite material
  • Preparation method and application of lead-free A4MnBi2X12 perovskite material
  • Preparation method and application of lead-free A4MnBi2X12 perovskite material

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preparation example Construction

[0028] A kind of lead-free A described in the present invention 4 MnB 2x 12 The preparation method of perovskite material, the main steps are:

[0029] Mix halide metal salt, bismuth oxide or its corresponding bismuth salt (bismuth halide, bismuth acetate, bismuth nitrate, etc.), manganese halide / manganese monoxide / manganese acetate, and hydrohalic acid (HX), under high temperature The raw materials are dissolved by keeping warm in a polytetrafluoroethylene hydrothermal kettle, and then slowly lowered to room temperature, the single crystal is precipitated from the hydrohalic acid, filtered and washed to obtain the product A 4 MnB 2 x 12 .

[0030] Among them, the AX, Bi 2 o 3 、MnX 2 In A is Li, Na, K, Rb, Cs, and CH 3 NH 3 + CH 4 N 2 + , C 8 h 11 N + One or more mixtures of inorganic or organic cations, X is one or more mixtures of Cl, Br, I.

[0031] The synthesis method of the invention is simple and reproducible, and the obtained single crystal can be use...

Embodiment 1

[0033] A lead-free A 4 MnB 2 x 12 Perovskite materials (Cs 4 MnB 2 Cl 12 single crystal) preparation method, the main steps are:

[0034] Step 1, 672mg CsCl, 464mg Bi 2 o 3 , 125 mg MnCl 2 Add to 5mL hydrochloric acid, stir for 10 minutes to obtain the precursor;

[0035] Step 2: Transfer the precursor obtained in Step 1 to a polytetrafluoroethylene reactor and seal it; transfer the sealed reactor to an oven at 180°C and keep it warm for 30 minutes. Then slowly lower to room temperature, filter and remove the mother liquor to obtain a single crystal, wash the single crystal with a small amount of ethanol or concentrated hydrochloric acid, and then dry it in an oven at 70°C to obtain the target product Cs 4 MnB 2 Cl 12 single crystal.

[0036] like figure 1 As shown, the size of the obtained single crystal is about 4mm, and under the excitation of 365nm ultraviolet light, the single crystal emits very bright orange light. The crystal structure of the material was ...

Embodiment 2

[0039] A lead-free A 4 MnB 2 x 12 Perovskite materials (Cs 4 MnB 2 Cl 12 powder), the main steps are:

[0040] Step 1, 672mg CsCl, 464mg Bi 2 o 3 , 125 mg MnCl 2 Add to 5mL of hydrochloric acid, stir for 10 minutes to obtain powder precipitation;

[0041] In step 2, the precipitate obtained in step 1 is centrifuged or filtered, and dried to obtain Cs 4 MnB 2 Cl 12 powder.

[0042] Cs 4 MnB 2 Cl 12 It can be directly synthesized in hydrochloric acid at room temperature, such as Figure 5a As shown, the XRD of the powder is consistent with the single crystal XRD obtained in Example 1, indicating that the Cs directly synthesized by the normal temperature method 4 MnB 2 Cl 12 The powder phase is consistent with single crystal. Figure 5b It is a photo of the powder under ultraviolet light, and the luminescent color is orange.

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Abstract

The invention discloses a preparation method and application of a lead-free A4MnBi2X12 (A=Li, Na, K, Rb, Cs, CH3NH3<+>, CH4N2<+>, or C8H11N<+>; and X=Cl, Br, or I) double perovskite material. An A4MnBi2X12 single crystal is obtained by performing cooling crystallization in halogen acid by using AX, Bi2O3, and MnX2 as raw materials, and the single crystals with different sizes can be obtained by adjusting the cooling rate. The synthetic method has good repeatability and easy operation, the obtained single crystal has the characteristics of good crystallinity, no toxicity and stability, and thematerial obtained by regulating the type of halogen has excellent luminous properties, and can be used in the fields of scintillators, X-ray detection, luminescence, lighting and photocatalysis / photoelectrocatalysis.

Description

technical field [0001] The invention belongs to the field of preparation and application of novel materials, in particular to a kind of A 4 MnB 2 x 12 Preparation methods and applications of perovskite materials. Background technique [0002] In 2009, Kojima et al. used perovskite materials as the light-absorbing layer of solar cells for the first time. Due to the high carrier mobility, large extinction coefficient and low defect density of perovskite materials, in the past ten years, perovskite materials have been widely used in solar cells. It has excellent performance in fields such as batteries, lasers, photodetection, photo / photocatalysis, and water sensing. Perovskite nanocrystals have good luminescent properties, and the half-peak width is generally narrow, but perovskite nanocrystals are usually prepared by cumbersome thermal injection methods, which require high energy consumption and low yields. A large amount of ligands prevents the agglomeration of nanocrysta...

Claims

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Application Information

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IPC IPC(8): C09K11/74G01N23/00G01T1/20H01L33/50
CPCC09K11/7435G01T1/2012G01N23/00H01L33/504
Inventor 匡代彬魏俊华王旭东周磊廖金凤
Owner SUN YAT SEN UNIV
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