Preparation method for methylammonium iodide

A technology of methyl ammonium iodide and methylamine, which is applied in the field of preparation of methyl ammonium iodide, can solve the problems of poor performance of perovskite films, reduced iodine content, low density of defect states, etc., so as to improve the purity and defect. The effect of low density of states and large crystal size

Active Publication Date: 2017-11-10
BEIJING INSTITUTE OF TECHNOLOGYGY
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Problems solved by technology

[0004] In order to solve the problem that the iodine element content in the methyl ammonium iodide prepared by the existing conventional technology is relatively high, resulting in the poor performance of the prepared perovskite film, the purpose of the present invention is to provide a preparation method of high-purity ammonium iodide Method, the method is mainly to use the alcohol solution of organic amine that can provide alkaline environment to recrystallize the crude product under the protection of nitrogen, thereby greatly reducing the content of iodine element in the prepared methyl ammonium iodide; in addition, using this method The perovskite film prepared by the method described in the invention as a precursor has a large crystal size, low density of defect states, and low density, and the electrical performance of the solar cell prepared by the perovskite film is significantly improved

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  • Preparation method for methylammonium iodide
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  • Preparation method for methylammonium iodide

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[0027] Fabrication of perovskite solar cells: SnO 2 The solution was spin-coated on a clean ITO conductive glass substrate at 3000rpm, spin-coated for 30s, and then spin-coated SnO 2 The final ITO conductive glass was annealed at 150°C for 30 minutes to form SnO on the ITO conductive glass. 2 Electron transport layer; the perovskite precursor solution was spin-coated on SnO at 4000rpm 2 On the electron transport layer, spin-coat for 25s, and then anneal the ITO conductive glass spin-coated perovskite precursor solution at 65°C for 1min, then anneal at 100°C for 2min. 2 A perovskite film is formed on the electron transport layer; the spiro-OMeTAD solution is spin-coated on the perovskite film at 3000rpm for 30s to form a hole transport layer on the perovskite film; Gold is evaporated on it as an electrode to obtain a flat heterojunction perovskite solar cell;

[0028] The SnO 2 Solution preparation: SnO with a mass fraction of 15% 2 The stock solution of the aqueous soluti...

Embodiment 1

[0033] (1) The hydriodic acid that the mass fraction is 30% methylamine aqueous solution and the mass fraction is 57% is mixed, and the mol ratio of methylamine and hydrogen iodide in the mixed solution is 1:1.2; Under nitrogen protection, mix The solution was placed in an ice-water bath and reacted in the dark for 5 hours to obtain an aqueous solution of methylammonium iodide;

[0034] (2) using a rotary evaporator to remove the solvent water in the methyl ammonium iodide aqueous solution by rotary evaporation at 40° C. to obtain the methyl ammonium iodide crystal crude product;

[0035] (3) Under the protection of nitrogen, first add the crude methylammonium iodide crystals to 12.5mmol / L methylamine ethanol solution, and heat to 90°C, after the crude methylammonium iodide crystals are completely dissolved, a mixed solution is obtained Add diethyl ether to the mixed solution until the crystals just precipitate, stop heating, cool to the crystals no longer precipitate, filter ...

Embodiment 2

[0038] (1) The hydriodic acid that the mass fraction is 30% methylamine aqueous solution and the mass fraction is 57% is mixed, and the mol ratio of methylamine and hydrogen iodide in the mixed solution is 1:1.2; Under nitrogen protection, mix The solution was placed in an ice-water bath and reacted in the dark for 5 hours to obtain an aqueous solution of methylammonium iodide;

[0039] (2) using a rotary evaporator to remove the solvent water in the methyl ammonium iodide aqueous solution by rotary evaporation at 40° C. to obtain the methyl ammonium iodide crystal crude product;

[0040] (3) Under the protection of nitrogen, first add the crude methylammonium iodide crystals to 12.5mmol / L methylamine ethanol solution, and heat to 90°C, after the crude methylammonium iodide crystals are completely dissolved, a mixed solution is obtained Add diethyl ether to the mixed solution until the crystals just precipitate, stop heating, cool to the crystals no longer precipitate, filter ...

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Abstract

The invention relates to a preparation method for methylammonium iodide, belonging to the technical fields of organic-inorganic hybrid materials and photoelectric materials. According to the method in the invention, under the protection of nitrogen, a crude product is purified by using an alcoholic solution of organic amine capable of providing an alkaline environment; the alcoholic solution of organic amine facilitates disproportionation of I2 to produce iodide ions and effectively inhibits generation of I2, so the content of elemental iodine in the prepared methyl ammonium iodide is greatly reduced; a perovskite film prepared by using the methyl ammonium iodide as a precursor has large crystal size, low defect state density and long carrier life; and a solar cell prepared from the perovskite film has photoelectric conversion efficiency.

Description

technical field [0001] The invention relates to a method for preparing methylammonium iodide, which belongs to the technical field of organic-inorganic hybrid materials and photoelectric materials. Background technique [0002] With the progress and development of human society, human demand for energy has increased significantly. The use of a large amount of fossil energy has caused serious environmental pollution. Moreover, fossil energy is non-renewable and increasingly exhausted, making the energy crisis a problem facing all mankind. Solar energy is a clean and safe renewable energy. Effective use of solar energy is of great significance to alleviate the energy crisis, protect the earth's environment, and further promote economic development. [0003] Organic-inorganic hybrid perovskite solar cells have attracted widespread attention from researchers all over the world due to their low preparation cost and simple preparation process. Their superior photoelectric properti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C211/04C07C209/84
CPCC07C209/00C07C209/84C07C211/04
Inventor 陈棋周晨晓张德良李煜璟
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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