Method for preparing organic-inorganic hybrid perovskite material through gas-liquid or gas-solid two phase in-situ reaction

A perovskite material and in-situ reaction technology, applied in organic chemistry, organic chemical methods, amino compound preparation, etc., can solve the problems of high energy consumption, inability to completely convert lead halide PbX, cumbersome process, etc., and achieve film-forming properties Good, reduce the pre-preparation process, the effect of convenient operation

Active Publication Date: 2016-04-13
CONTEMPORARY AMPEREX TECH CO
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] In recent years, perovskite solar cells have become a research hotspot in the field of renewable energy. The traditional synthesis strategy of perovskite materials, whether it is a one-step method or a two-step continuous deposition method, needs to first synthesize the halide amine salt corresponding to lead halide perovskite. MAX, in the process of synthesizing MAX, the toxic solvent diethyl ether needs to be used, and steps such as rotary evaporation and vacuum drying are required. 2 Problems that cannot be completely converted (Yao Xin, Ding Yanli, Zhang Xiaodan, etc. A review of perovskite solar cells [J]. Acta Physica Sinica, 2015, (03): 145-152.)

Method used

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  • Method for preparing organic-inorganic hybrid perovskite material through gas-liquid or gas-solid two phase in-situ reaction
  • Method for preparing organic-inorganic hybrid perovskite material through gas-liquid or gas-solid two phase in-situ reaction
  • Method for preparing organic-inorganic hybrid perovskite material through gas-liquid or gas-solid two phase in-situ reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0037] This embodiment relates to a method in which hydroiodic acid (HI) and lead iodide are dissolved in DMF and then spin-coated and reacted with methylamine vapor in situ to prepare a perovskite film under a methylamine atmosphere. The method includes the following steps:

[0038] 1) Dissolve 0.461g of lead iodide and 0.132mL of hydroiodic acid solution in 1mL of DMF to obtain precursor solution A; the molar ratio of the above-mentioned lead iodide and hydroiodic acid is calculated as 1:1.

[0039] 2) The solution A obtained in step 1) was spin-coated onto the FTO substrate at 3500 rpm for 30 s, and the spin-coating was performed under a methylamine gas atmosphere, and dried at room temperature.

[0040] 3) The perovskite film can be obtained by annealing the substrate obtained in step 2) at 100°C for 5 minutes.

[0041] figure 1 It is the X-ray diffraction spectrum of Example 1, from which it can be drawn that the crystal form of the perovskite film obtained in Example 1 ...

Embodiment 2

[0045] This embodiment relates to a method for preparing a perovskite film by dissolving hydrobromic acid (HBr) and lead bromide in GBL and then reacting in situ with methylamine vapor in an atmosphere of methylamine. The method includes the following steps:

[0046] 1) Dissolve 0.369g of lead bromide and 0.121mL of HBr solution (molar concentration 8.65M) in 1mL of DMF to obtain precursor solution A; the molar ratio of lead bromide and hydrobromic acid is calculated as 1:1.05.

[0047] 2) The solution A obtained in step 1) was spin-coated onto the FTO substrate at 3500 rpm for 20 s, and the spin-coating was performed under a methylamine gas atmosphere, and dried at room temperature.

[0048] 3) The perovskite film can be obtained by annealing the substrate obtained in step 2) at 100°C for 5 minutes.

[0049] The XRD spectrum of perovskite obtained in this embodiment is shown in Figure 5 , indicating that a phase-pure, highly crystalline methylamine lead bromide perovskite t...

Embodiment 3

[0051] This embodiment relates to a kind of concentrated hydrochloric acid (HCl), lead chloride (PbCl 2 ) is dissolved in DMF and then spin-coated under a methylamine atmosphere and reacts with methylamine vapor in-situ to prepare a method for a perovskite film, the method comprising the steps of:

[0052] 1) Dissolve 0.222g of lead chloride and 0.082mL of HCl solution (molar concentration 12M) in 1mL of GBL to obtain precursor solution A; the molar ratio of the above lead chloride and concentrated hydrochloric acid is calculated as 1:0.95.

[0053]2) The solution A obtained in step 1) was spin-coated onto the FTO substrate at 3500 rpm for 10 s, and the spin-coating was performed under a methylamine gas atmosphere, and dried at room temperature.

[0054] 3) The perovskite film can be obtained by annealing the substrate obtained in step 2) at 100°C for 5 minutes.

[0055] The XRD spectrum of perovskite obtained in this embodiment is shown in Image 6 , indicating that a phase...

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Abstract

The invention provides a method for preparing an organic-inorganic hybrid perovskite material through a gas-liquid or gas-solid two phase in-situ reaction. Through gas-liquid one-step spin coating or gas-solid in-situ reaction continuous sedimentation, the organic-inorganic hybrid perovskite material is prepared. The method comprises mixing halogen acid HX and lead halide PbX2 according to a certain ratio, coating a substrate with the mixture in an organic amine atmosphere and carrying out annealing to obtain a perovskite film, or comprises mixing halogen acid HX and lead halide PbX2 according to a certain ratio, coating a substrate with the mixture, carrying out drying to obtain a precursor film and carrying out organic amine vapor treatment so that the high-quality perovskite spin-coated film is obtained through a gas-solid in-situ reaction. The perovskite film prepared through gas-liquid and gas-solid in-situ reaction methods has good crystallinity and the compact and flat surface. The method can be carried out at the normal temperature, is free of halogenated methylamine precursor preparation, can be operated conveniently, has a low cost and good film forming ability and is convenient for industrial large-scale production.

Description

technical field [0001] The invention relates to a gas-liquid or gas-solid two-phase in-situ reaction to prepare an organic-inorganic hybrid perovskite material, in particular to a gas-liquid one-step spin coating, or a gas-solid in-situ reaction continuous deposition method to prepare high-quality method for perovskite thin films. Background technique [0002] In recent years, perovskite solar cells have become a research hotspot in the field of renewable energy. The traditional synthesis strategy of perovskite materials, whether it is a one-step method or a two-step continuous deposition method, needs to first synthesize the halide amine salt corresponding to the lead halide perovskite. MAX, in the process of synthesizing MAX, the toxic solvent diethyl ether needs to be used, and steps such as rotary evaporation and vacuum drying are required. 2 Problems that cannot be completely converted (Yao Xin, Ding Yanli, Zhang Xiaodan, etc. A review of perovskite solar cells [J]. Ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C211/04C07C211/05
CPCC07B2200/13C07C209/00C07C211/04C07C211/05
Inventor 赵一新钱旭芳张太阳李戈郭男杰岳东亭阚淼贾爱华
Owner CONTEMPORARY AMPEREX TECH CO
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