a mapbx 3 Preparation method of perovskite nanocluster

Abstract

The invention discloses a preparation method of MAPbX3 perovskite nanocluster, belonging to the technical field of preparation of semiconductor nanomaterial. The method comprises the following steps of: adding a methylamine halide solution into a N2 protected lead halide solution; and reacting for 1 minute at a temperature of 0-25 DEG to obtain the MAPbX3 perovskite nanocluster. The nanocluster prepared in the invention has very sharp and symmetric absorption and fluorescence peaks and shows perfect luminescent property and fluorescence quantum efficiency; the whole reaction is easy to operate while the conditions are mild; large-scale synthesis can be implemented; the MAPbX3 perovskite nanocluster has huge application prospect in the fields such as biological fluorescent markers, LEDs and solar cells.

Description

technical field

[0001] The invention belongs to the technical field of semiconductor nanomaterial preparation, and relates to a method for preparing MAPbX in large quantities. 3 (X = Cl, Br, I) Synthesis of perovskite nanoclusters. Background technique

[0002] When the material size of a macroscopic bulk phase semiconductor is gradually reduced to a situation related to the electronic wave function of the material, significant electronic fluctuation changes appear, and the electronic structure of the semiconductor changes, from the original continuous energy band structure to split The energy level state and the energy level structure that changes with the size will affect the optical properties of the material accordingly. This phenomenon is called the quantum size effect. The more common semiconductor nanoparticles, that is, quantum dots, mainly include II-VI, III-V and IV-VI groups. These types of quantum dots are well obeyed by the quantum size effect, and their prope...

Examples

Embodiment 1

[0021] First, a solution of methylamine chloride (MACl) was prepared. Take 120mmol (12mL) of methylamine solution, 44mmol (3.8mL) of hydrochloric acid solution and 50mL of ethanol in a three-necked flask, and react at room temperature for 2 hours under nitrogen protection. The whole solution is colorless and transparent, and then the solution is rotary evaporated under the conditions of -0.1MPa and 45°C, and white crystals will be precipitated in the bottle, which is chloromethylamine. , rotary steaming again. Repeat this three times to wash and purify the chloromethylamine powder, and finally place it in a vacuum oven at 60°C for purification and set aside. Take 0.5mmol (0.0337g) of chloromethylamine (MACl) solid powder and dissolve it in 5mL of ethanol to prepare a 0.1M chloromethylamine (MACl) solution.

[0022] Then take 0.05mmol of lead chloride solid powder, 0.12mL of oleylamine, 0.1mL of oleic acid, 0.1mL of tri-n-octylphosphine and 4mL of dodecane into the three-neck...

Embodiment 2

[0024] First, a methylamine bromide (MABr) solution is prepared. Take 120mmol (12mL) of methylamine solution, 44mmol (5mL) of hydrobromic acid solution and 50mL of ethanol in a three-necked flask, and react at room temperature for 2 hours under nitrogen protection. The whole solution is colorless and transparent, and then the solution is rotary evaporated under the conditions of -0.1MPa and 45°C, and white crystals will be precipitated in the bottle, which is methyl bromide, and methyl bromide is dissolved in 50mL of ethanol , rotary steaming again. Repeat this three times to wash and purify the methyl bromide powder, and finally place it in a vacuum oven at 60°C for purification and set aside. Take 0.5mmol (0.056g) of methylamine bromide (MABr) solid powder and dissolve it in 5mL of ethanol to prepare a 0.1M methylamine bromide (MABr) solution.

[0025] Then take 0.05mmol of lead bromide solid powder, 0.12mL of oleylamine, 0.1mL of oleic acid and 4mL of dodecane into a thre...

Embodiment 3

[0028] First, a solution of methylamine iodide (MAI) was prepared. Take 120mmol (12mL) of methylamine solution, 44mmol (11mL) of hydriodic acid solution and 40mL of ethanol in a three-necked flask, and react at room temperature for 2 hours under nitrogen protection. The whole solution is colorless and transparent, and then the solution is rotary evaporated at -0.1MPa and 45°C, and white crystals will precipitate in the bottle, which is methyl iodide. Dissolve methyl iodide in 50mL of ethanol , rotary steaming again. Repeat this three times to wash and purify the methyl iodide powder, and finally place it in a vacuum oven at 60°C for purification and set aside. Take 0.5 mmol (0.079 g) of methyl iodide (MAI) solid powder and dissolve it in 5 mL of ethanol to prepare a 0.1 M methyl iodide (MAI) solution.

[0029] Then take 0.05mmol of lead iodide solid powder, 0.12mL of oleylamine, 0.1mL of oleic acid and 4mL of dodecane into the three-neck flask, vacuumize at 50°C for 30 minutes...

technical field

[0001] The invention belongs to the technical field of semiconductor nanomaterial preparation, and relates to a method for preparing MAPbX in large quantities. 3 (X = Cl, Br, I) Synthesis of perovskite nanoclusters. Background technique

[0002] When the material size of a macroscopic bulk phase semiconductor is gradually reduced to a situation related to the electronic wave function of the material, significant electronic fluctuation changes appear, and the electronic structure of the semiconductor changes, from the original continuous energy band structure to split The energy level state and the energy level structure that changes with the size will affect the optical properties of the material accordingly. This phenomenon is called the quantum size effect. The more common semiconductor nanoparticles, that is, quantum dots, mainly include II-VI, III-V and IV-VI groups. These types of quantum dots are well obeyed by the quantum size effect, and their prope...

Examples

Embodiment 1

[0021] First, a solution of methylamine chloride (MACl) was prepared. Take 120mmol (12mL) of methylamine solution, 44mmol (3.8mL) of hydrochloric acid solution and 50mL of ethanol in a three-necked flask, and react at room temperature for 2 hours under nitrogen protection. The whole solution is colorless and transparent, and then the solution is rotary evaporated under the conditions of -0.1MPa and 45°C, and white crystals will be precipitated in the bottle, which is chloromethylamine. , rotary steaming again. Repeat this three times to wash and purify the chloromethylamine powder, and finally place it in a vacuum oven at 60°C for purification and set aside. Take 0.5mmol (0.0337g) of chloromethylamine (MACl) solid powder and dissolve it in 5mL of ethanol to prepare a 0.1M chloromethylamine (MACl) solution.

[0022] Then take 0.05mmol of lead chloride solid powder, 0.12mL of oleylamine, 0.1mL of oleic acid, 0.1mL of tri-n-octylphosphine and 4mL of dodecane into the three-neck...

Embodiment 2

[0024] First, a methylamine bromide (MABr) solution is prepared. Take 120mmol (12mL) of methylamine solution, 44mmol (5mL) of hydrobromic acid solution and 50mL of ethanol in a three-necked flask, and react at room temperature for 2 hours under nitrogen protection. The whole solution is colorless and transparent, and then the solution is rotary evaporated under the conditions of -0.1MPa and 45°C, and white crystals will be precipitated in the bottle, which is methyl bromide, and methyl bromide is dissolved in 50mL of ethanol , rotary steaming again. Repeat this three times to wash and purify the methyl bromide powder, and finally place it in a vacuum oven at 60°C for purification and set aside. Take 0.5mmol (0.056g) of methylamine bromide (MABr) solid powder and dissolve it in 5mL of ethanol to prepare a 0.1M methylamine bromide (MABr) solution.

[0025] Then take 0.05mmol of lead bromide solid powder, 0.12mL of oleylamine, 0.1mL of oleic acid and 4mL of dodecane into a thre...

Embodiment 3

[0028] First, a solution of methylamine iodide (MAI) was prepared. Take 120mmol (12mL) of methylamine solution, 44mmol (11mL) of hydriodic acid solution and 40mL of ethanol in a three-necked flask, and react at room temperature for 2 hours under nitrogen protection. The whole solution is colorless and transparent, and then the solution is rotary evaporated at -0.1MPa and 45°C, and white crystals will precipitate in the bottle, which is methyl iodide. Dissolve methyl iodide in 50mL of ethanol , rotary steaming again. Repeat this three times to wash and purify the methyl iodide powder, and finally place it in a vacuum oven at 60°C for purification and set aside. Take 0.5 mmol (0.079 g) of methyl iodide (MAI) solid powder and dissolve it in 5 mL of ethanol to prepare a 0.1 M methyl iodide (MAI) solution.

[0029] Then take 0.05mmol of lead iodide solid powder, 0.12mL of oleylamine, 0.1mL of oleic acid and 4mL of dodecane into the three-neck flask, vacuumize at 50°C for 30 minutes...

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