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Method for producing halogenated caesium lead material for perovskite solar cell

A cesium lead halide, solar cell technology, applied in the direction of circuits, photovoltaic power generation, electrical components, etc., can solve the problems of difficult recovery of organic solvents, unstable product quality, difficult safety and environmental protection, etc., to achieve easy expansion and industrial production, improve The effect of environmental stability and simple process

Inactive Publication Date: 2017-02-22
TIANJIN VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the breakthrough of perovskite solar cell technology and adapting to the development of the broad application market in the future, it is necessary to supply specialized raw materials for perovskite solar cells to overcome the existing production methods of high production costs, unstable product quality, and a large number of organic materials. Difficulty in solvent recovery, outstanding safety and environmental protection issues, and difficulties in large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add respectively 51.1g (0.42mol) of hydrochloric acid, 11.8g (0.22mol) of ammonium chloride, 76.3g (0.2mol) of lead acetate trihydrate and 240g (4mol) of acetic acid in a glass reactor with a mass percentage concentration of 30%. , mix the above materials evenly, heat to reflux at 100-120°C to completely dissolve the resulting lead chloride precipitate, then vacuum distill and separate acetic acid and water until crystals of ammonium lead chloride are precipitated, cool and centrifuge to separate ammonium lead chloride Crystallized and washed with C1-C4 fatty alcohol.

[0033] Mix the obtained lead ammonium chloride crystals, 34.2g (0.105mol) of cesium carbonate and 121.2g (2mol) of isopropanol evenly, and slowly heat the reaction at 80-85°C for 2h, so that cesium carbonate and lead ammonium chloride can be reacted and converted It is cesium lead chloride, and the by-product ammonium carbonate is decomposed and volatilized until no gas is released in the reactant.

[0...

Embodiment 2

[0036] 79.1g (0.44mol) of hydrobromic acid, 21.6g (0.22mol) of ammonium bromide, 76.3g (0.2mol) of lead acetate trihydrate and 360g (6mol) of acetic acid were added to the glass reactor with a mass percent concentration of 45%. ), mix the above materials evenly, heat to reflux at 100-120°C to completely dissolve the resulting lead bromide precipitate, then vacuum distill and separate acetic acid and water to generate lead ammonium bromide crystals, cool and centrifuge to separate lead ammonium bromide crystallized and washed with absolute ethanol.

[0037] Mix the obtained lead ammonium bromide crystals, 35.8 g (0.11 mol) of cesium carbonate and 184 g (4 mol) of absolute ethanol, and slowly heat the reaction at 70-80° C. for 2 hours to convert cesium carbonate and lead ammonium bromide into cesium lead bromide, and decompose and volatilize the by-product ammonium carbonate until no gas is released from the reactant.

[0038] Cool the reaction product to 50-60°C, add 10 g of γ...

Embodiment 3

[0040] 102.3g (0.44mol) of hydroiodic acid, 21.6g (0.22mol) of ammonium iodide, 76.3g (0.2mol) of lead acetate trihydrate and 480g (8mol) of acetic acid were added to the glass reactor with a mass percent concentration of 55%. ), mix the above materials evenly, heat to reflux at 100-120°C to completely dissolve the resulting lead iodide precipitate, then vacuum distill and separate acetic acid and water to generate ammonium lead iodide crystals, cool and centrifuge to separate lead ammonium iodide crystallized and washed with absolute ethanol.

[0041] Mix the resulting lead ammonium iodide crystals, 35.8 g (0.11 mol) of cesium carbonate and 222.3 g (3 mol) of n-butanol, and slowly heat the reaction at 90-110° C. for 4 hours to convert cesium carbonate and lead ammonium iodide into cesium lead iodide, and decompose and volatilize the by-product ammonium carbonate until no gas is released from the reactant.

[0042] Cool the reaction product to 50-60°C, add 10 g of dimethyl su...

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Abstract

The invention relates to a method for producing a halogenated caesium lead material that is obtained based on solid-liquid two-phase chemical reaction of a halogenated ammonium lead material and cesium carbonate and has advantages of low production cost, high stability and easy dispersion. A halogenated ammonium lead, cesium carbonate, and C1-C4 fatty alcohol are mixed uniformly according to a molar ratio 1 to 0.5-0.55 to 10-20; while heating is carried out slowly at a temperature of 70 to 110 DEG C, reaction is carried out for 2 to 6 hours, so that the cesium carbonate reacts with the halogenated ammonium lead material to obtain a halogenated caesium lead material and ammonium carbonate as a by product decomposes and volatilizes; and a reaction product is cooled to be reach a temperature of 50 to 60 DEG C, a polar solvent as a cosolvent of a halogenated caesium lead crystal and silicone oil as a surface treating agent are added, a supernatant solution is stirred continuous for 6 to 12 hours, thereby forming a halogenated caesium lead crystal particle with characteristics of uniform particle diameter and surface hydrophobicity. The method provided by the invention has characteristics of simple process and secure environment protection and is easy to expanded produce and industrial produce. The product obtained by using the method can be used as a material for a light absorption layer of a perovskite solar cell and a material of a hole transport layer.

Description

technical field [0001] The invention relates to a production method of cesium lead halide for perovskite solar cells, in particular to a method for producing cesium lead halide with high stability and easy dispersibility at low cost by using ammonium lead halide and cesium carbonate for solid-liquid two-phase chemical reaction The method belongs to the field of new energy and new materials. [0002] technical background [0003] Solar cells based on organometallic halide perovskite structured light-absorbing materials are called perovskite solar cells. At present, their photoelectric conversion efficiency has exceeded 28%, and it is expected to reach 50% in the future, which will subvert the existing solar cell technology. Mainstream products in the market. Perovskite solar cells are usually composed of five parts: transparent conductive glass, dense layer, perovskite light absorbing layer, hole transport layer, and metal back electrode. The thickness of the perovskite ligh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L51/42H01L51/48
CPCH10K30/00Y02E10/549
Inventor 胡兴兰刘炳光李建生王少杰王璐瑶韩秋坡凌小芳
Owner TIANJIN VOCATIONAL INST
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