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A stable lead-free low bandgap all-inorganic perovskite a 2 pdx 6 Nanocrystal and its preparation method

A nanocrystal, low bandgap technology, applied in the field of preparation of new nanomaterials, can solve the problems of narrow visible light absorption range, narrow size distribution, poor stability, etc., and achieve the effects of good dispersion, uniform size and simple method.

Active Publication Date: 2020-05-19
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Since the existing non-lead perovskite nanocrystalline materials have problems such as poor stability or wide bandgap, and narrow visible light absorption range, the purpose of the present invention is to provide a stable, lead-free, low-bandgap perovskite A 2 wxya 6 A method for preparing nanocrystals. This anti-solvent synthesis method is simple, environmentally friendly, highly reproducible, and can be operated in an air atmosphere at room temperature; at the same time, the obtained nanocrystals have narrow size distribution, good dispersion, and stability. high advantage

Method used

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  • A stable lead-free low bandgap all-inorganic perovskite a <sub>2</sub> pdx <sub>6</sub> Nanocrystal and its preparation method
  • A stable lead-free low bandgap all-inorganic perovskite a <sub>2</sub> pdx <sub>6</sub> Nanocrystal and its preparation method
  • A stable lead-free low bandgap all-inorganic perovskite a <sub>2</sub> pdx <sub>6</sub> Nanocrystal and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A stable lead-free low bandgap all-inorganic perovskite Cs 2 PdBr 6 The preparation method of microcrystal, comprises the following steps:

[0040] Step 1, 0.851g CsBr, 0.532g PdBr 2 , 10mL HBr was added into the three-necked flask at the same time and mixed, then the system was heated and stirred at 85°C for 5min to ensure that the PdBr 2 and CsBr were all dissolved to obtain a clear and transparent solution;

[0041] Step 2, prepare 20mL DMSO-HBr mixed solution as an oxidant, wherein DMSO accounts for 10% of the total volume;

[0042] Step 3, warm up the clear solution in step 1 to 120 °C, then quickly add 20 mL of DMSO-HBr mixed solution, immediately generate a large amount of Cs 2 PdBr 6 Microcrystalline, after 30s of reaction, filter the product while it is hot, wash it with deionized water while filtering, and finally bake the product in an oven at 70°C for 30 minutes to obtain high-purity Cs 2 PdBr 6 Microcrystalline.

[0043] like figure 1 As shown in a...

Embodiment 2

[0045] Using the Cs prepared in Example 1 2 PdBr 6 Microcrystals are used as raw materials, which are dissolved in DMF to obtain a clear precursor solution, and then an appropriate amount of precursor solution is added to the anti-solvent to prepare Cs 2 PdBr 6 Nanocrystalline. The specific steps are:

[0046] Get the Cs prepared in 10mg embodiment 1 2 PdBr 6 Microcrystals were added to 2mL DMF, and then heated at 130°C for 1min to make Cs 2 PdBr 6 All the microcrystals were dissolved in DMF to obtain a clear precursor solution; finally, 200 μL of the precursor solution was quickly added to 2 mL of the anti-solvent propionic acid that was stirring, and a large amount of black precipitate was generated immediately, and after about 20 seconds, the stirring was stopped. The obtained nanocrystals can be directly used for characterization or testing of various other properties. The size of the obtained nanocrystals is uniform, and no large-scale morphology appears. In addi...

Embodiment 3

[0051] Using the Cs prepared in Example 1 2 PdBr 6 Microcrystals are used as raw materials, which are dissolved in DMF to obtain a clear precursor solution, and then an appropriate amount of precursor solution is added to the anti-solvent to prepare Cs 2 PdBr6 Nanocrystalline. The specific steps are:

[0052] Get the Cs prepared in 10mg embodiment 1 2 PdBr 6 Microcrystals were added to 2mL DMF, and then heated at 130°C to make Cs 2 PdBr 6 All the microcrystals were dissolved in DMF to obtain a clear precursor solution; then 200 μL of the precursor solution was quickly added to 2 mL of the anti-solvent isobutanol that was stirring, and a large amount of black precipitate was generated immediately, and after about 20 seconds, the stirring was stopped.

[0053] Figure 7a and Figure 7b Respectively the Cs synthesized in isobutanol in the present embodiment 3 2 PdBr 6 Morphology and size distribution of nanocrystals. It can be seen from the figure that Cs can be prepar...

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Abstract

The invention discloses a preparation method for stable full-inorganic perovskite A2PdX6 nanocrystalline with no lead and low band gap (A=Cs, Rb, K or multiple mixing; X=Cl, Br, I or multiple mixing thereof), the preparation method takes A2PdX6 micron-crystalline as a precursor material, and then the nanocrystalline is synthesized by using a rapid antisolvent method, the main synthesis process isas follows: Firstly, A2PdX6 micron-crystalline is synthesized by a solution method or a solid phase method; then the obtained A2PdX6 micron-crystalline is dissolved in a strong polar solvent under heating condition to obtain a clear and transparent precursor solution; after the precursor solution is cooled to room temperature, a certain amount of the precursor solution is rapidly added to the antisolvent under the stirring condition, and A2PdX6 nanocrystalline colloidal solution with a particle size about 3 nm is rapidly formed, the synthesis method provided by the invention is fast, simple, can be operated at normal temperature, has good reproducibility and is environmentally friendly; at the same time, the product has uniform size, good dispersibility, high stability and excellent photoelectric response; the preparation method can be used in fields such as light or photoelectrocatalysis, photodetectors, solar cells.

Description

technical field [0001] The invention belongs to the field of preparation of novel nanomaterials, in particular to a 2 wxya 6 Lead-free perovskite nanocrystalline material and its preparation method and application. Background technique [0002] In the past 4 years, lead halide methylamine (CH 3 NH 2 wxya 3 ) and cesium lead halide (CsPbX 3 ) as the representative perovskite nanocrystalline material, due to its adjustable band gap, large visible light absorption cross-section, high carrier mobility, long carrier diffusion path and simple and convenient solution phase preparation process, it has been widely accepted. Widespread concern. At the same time, they have shown potential application prospects in many fields such as solar cells, photodetectors, and photo(photoelectric) catalysis. However, the stability of the material and the environmental pollution caused by the toxicity of metal Pb limit the large-scale industrial application of this type of perovskite nanocry...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00B82Y40/00
CPCB82Y40/00C01G55/002C01P2002/34C01P2002/72C01P2002/84C01P2004/03C01P2004/04C01P2004/52C01P2004/64
Inventor 匡代彬周磊黄增光
Owner SUN YAT SEN UNIV
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