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Method of producing methylamine lead halide for perovskite solar cells

A lead halide methylamine, solar cell technology, applied in circuits, photovoltaic power generation, electrical components, etc., can solve the problems of difficulty in recycling organic solvents, difficulty in safety and environmental protection, and high production costs, and achieve easy expansion and industrialized production, and the process is simple. , The effect of process environmental protection and safety

Inactive Publication Date: 2017-02-15
TIANJIN VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fine chemical companies should develop green and environmentally friendly lead halide methylamine production processes according to market needs, in order to overcome the existing production methods of high production costs, unstable product quality, difficulty in recovering a large amount of organic solvents, prominent safety and environmental protection problems, and difficulty in large-scale production. production problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 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 formed lead chloride precipitate, and then vacuum distill and separate acetic acid and water to form crystals of ammonium lead chloride.

[0030] Mix the crystallization of lead ammonium chloride and solid paraformaldehyde powder 13.2g (0.44mol) evenly, and slowly heat the reaction at 120-160°C for 2 hours, so that the formaldehyde gas released by solid paraformaldehyde reacts with lead ammonium chloride to form chlorine Lead methylamine, further heated to 170-180 ° C until no obvious gas is released.

[0031] Immerse the reaction product with 150 mL of dehydrated dimethylformamide at room temperature for 12 hours until dissolved, and filter to remove insol...

Embodiment 2

[0033] 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, and then vacuum distill and separate acetic acid and water to generate ammonium lead bromide crystals.

[0034] Mix lead ammonium bromide crystals and solid paraformaldehyde powder 15g (0.50mol) evenly, and slowly heat the reaction at 120-160°C for 3 hours, so that the formaldehyde gas released by solid paraformaldehyde reacts with lead ammonium bromide to form lead bromide Methylamine, further heated to 170-180 ° C to react until no obvious gas is released.

[0035] Immerse the reaction product with 250 mL of dehydrated γ-butyrolactone at room temperature for 8 hours until dissolved, and filter to remove insoluble impurities to ...

Embodiment 3

[0037] 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.

[0038] Mix lead ammonium iodide crystals and solid paraformaldehyde powder 15g (0.50mol) evenly, and slowly heat the reaction at 120-160°C for 3 hours, so that the formaldehyde gas released by solid paraformaldehyde reacts with lead ammonium iodide to form lead iodide Methylamine, further heated to 170-180 ° C to react until no obvious gas is released.

[0039] Immerse the reaction product with 300 mL of dehydrated γ-butyrolactone at room temperature for 12 hours until dissolved, and filter to remove insoluble impurities to obtain a ...

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PUM

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Abstract

The invention relates to a method of producing methylamine lead halide for perovskite solar cells at low cost through solid phase reaction of formaldehyde and ammonium lead halide. Halogen acid, ammonium halide, lead acetate and acetic acid are mixed according to the mole ratio of (2.1-2.1):(1.1-1.2):1:(20-40), reflux reaction is carried out after the mixture is heated to 100-120 DEG C, acetic acid and water are separated through vacuum distillation, and an ammonium halide lead crystal is generated. The ammonium halide lead crystal and paraformaldehyde are mixed according to the mole ratio of 1:(2.1-2.5), are slowly heated at 120-160 DEG C to react for 1-6h, and are further heated to 170-180 DEG C to react until there is no obvious gas emission. The reaction product is re-crystallized with polarity organic solvent, washed with fatty alcohol and vacuum-dried to get refined methylamine lead halide. The yield was 95-99.2%, and the content is 99.0-99.5%. The production technology is simple, environment-friendly and safe. There is no need for annealing treatment after coating. The methylamine lead halide can be directly used as a light absorption layer of a solar cell.

Description

technical field [0001] The invention relates to a low-cost production method for producing lead halide methylamine for perovskite solar cells by using formaldehyde and lead ammonium halide solid-phase chemical reaction, belonging 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 light-absorbing layer is generally 200-600nm, and its main function is to absorb sunlight and generate electron-hole pairs,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L51/42H01L51/46
CPCH10K85/00H10K30/00Y02E10/549Y02P70/50
Inventor 王少杰赵燕禹李建生刘炳光刘希东卢俊锋
Owner TIANJIN VOCATIONAL INST
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