CN106379932B - A kind of synthetic method of perovskite CsPbX3 quantum dots at room temperature - Google Patents

A kind of synthetic method of perovskite CsPbX3 quantum dots at room temperature Download PDF

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Publication number
CN106379932B
CN106379932B CN201610694070.0A CN201610694070A CN106379932B CN 106379932 B CN106379932 B CN 106379932B CN 201610694070 A CN201610694070 A CN 201610694070A CN 106379932 B CN106379932 B CN 106379932B
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quantum dot
solution
source
cspbx
room temperature
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CN106379932A (en
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曹万强
方凡
刘培朝
曾媛媛
张慧婕
李阳
王仁龙
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Hubei University
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Hubei University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G21/00Compounds of lead
    • C01G21/006Compounds containing, besides lead, two or more other elements, with the exception of oxygen or hydrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/84Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a kind of CsPbX at room temperature3The simple method for synthesizing of (X=Br, I) quantum dot, it is characteristic of the invention that:Catalyst is used as using a kind of organic solvent containing chlorine element, makes caesium source and the reaction of lead source that can not be reacted at room temperature, synthesizes CsPbX3Quantum dot, its step are:Prepare caesium source presoma;Prepare lead source presoma;Caesium source presoma is dissolved into the organic solvent containing chlorine element;At room temperature by lead source presoma with 10:1 to 3:1 ratio injection, it is agitated to can obtain CsPbX3Quantum dot;The quantum dot wavelength covers 450nm-760nm, a width of 25-40nm of transmitting half-peak.The invention advantage is:Reaction temperature is low, and raw material is cheap, and aggregate velocity is fast, simple to operate, is adapted to large-scale mass production.

Description

A kind of synthetic method of perovskite CsPbX3 quantum dots at room temperature
Technical field
The present invention relates to photoelectric display illumination technical field of nano material, and in particular to a kind of perovskite CsPbX3(X= Br, I) synthetic method of quantum dot at room temperature.
Background technology
Quantum dot, also referred to as semiconductor nano, by hundreds of to thousands of former molecular inorganic cores, outside cladding Organic ligand, particle diameter is generally in 2-15nm.Because quantum dot can pass through the sized controllable tune realized to its emission spectrum Section, the spectral emissions of whole visible region can be obtained by the size and chemical constituent that change quantum dot, in LED illumination The fields such as display, solar cell, biological fluorescent labelling show huge potentiality and application value.Especially shown in illumination Aspect, have the characteristics that small volume, cost are low, luminous efficiency is high, long lifespan and energy consumption are low, therefore in cost-effective, environment Received significant attention in terms of protection.Due to CsPbX in traditional octadecylene or paraffin systems3Quantum dot synthesizes, caesium source and lead source Reaction needs a higher temperature to form CsPbX3Quantum dot, the preparation to quantum dot bring efficiency low cost is high to be stranded It is difficult.
The content of the invention
It is an object of the invention to provide a kind of CsPbX3The new synthetic method of quantum dot, using the organic solvent containing chlorine element As catalyst, CsPbX in traditional octadecylene or paraffin systems is reduced3The synthesis temperature of quantum dot.Make at room temperature without The caesium source of method reaction and the reaction of lead source, synthesize CsPbX3Quantum dot, wherein X=Br, I..The CsPbX3Quantum dot wavelength covers 450nm-760nm, launch a width of 25-40nm of half-peak, the method reaction temperature is low, and raw material is cheap, and aggregate velocity is fast, operation letter It is single, it is adapted to large-scale mass production.
A kind of CsPbX3The preparation method of quantum dot, specifically includes following steps;
A) caesium source, oleic acid (OA), octadecylene (ODE) are added in three-necked flask, leads to nitrogen after vacuumizing 30min at 90 DEG C Gas, 100-150 DEG C is heated to until forming settled solution 1;
B) lead source and halogen source, oleic acid (OA), oleyl amine (OLA) and 5ml octadecylene (ODE) are added separately to three-necked flask In, lead to nitrogen after 30min is vacuumized at 90 DEG C, then heat up 100-180 DEG C, obtain settled solution 2;
C) at room temperature, or with temperature take appropriate solution 1 to be dissolved into the solvent containing chlorine element, reinject appropriate solution 2, it is agitated to obtain CsPbX3Quantum dot;
Or take appropriate solution 2 to be dissolved into the solvent containing chlorine element (such as chloroform), and appropriate solution 1 is reinjected, it is agitated Obtain CsPbX3Quantum dot;
Described caesium source is Cs2CO3, one or more in CsCl.
Described lead source is PbCl2、PbBr2、PbO、PbI2In one or more;
The described solvent containing chlorine element is dichloromethane, chloroform, tetrachloromethane or the mixing containing above-mentioned solvent Solvent;
Described solution 1 and the ratio of solution 2 are adjustable, from 1:3 to 1:10, and order can overturn;
The method of the present invention is keeping CsPbX3While the excellent optical property of quantum dot, simplify its synthesis step, Difficulty reduces.
The technological core of the invention is that organic solvent containing chlorine element is used as catalyst, and caesium source is dissolved in into solvent In, then the lead source prepared and halogen source are rapidly injected, synthesize CsPbX in room temperature3Quantum dot.
Brief description of the drawings
Fig. 1 is the CsPbBr in embodiment 13Quantum dot uv-visible absorption spectra and fluorescence emission spectrogram of compound;
CsPbBr in Fig. 2 embodiments 13Quantum dot high power transmission electron microscope picture
Embodiment
Embodiment 1:
Prepare CsPbBr3Quantum dot
1. synthesize Cs presomas and Pb presoma
By 0.25mmol CsCO3, 0.25ml oleic acid (OA), 4ml octadecylene (ODE) add in three-necked flask, 90 DEG C vacuumize logical nitrogen after 30min, are heated to 150 DEG C until forming colourless solution, i.e. Cs presomas.
By 0.188mmol PbBr2, 0.5ml oleic acid (OA), 0.5ml oleyl amine (OLA) and 5ml octadecylene (ODE) It is added separately in three-necked flask, leads to nitrogen after 30min is vacuumized at 90 DEG C, then be warming up to 150 DEG C, obtains Pb forerunner Body.
2. prepare CsPbBr3Quantum dot
0.1ml Cs presomas are dissolved in 3ml chloroform, then take 1.5ml Pb presoma to be rapidly injected this In solution, that is, obtain CsPbBr3Quantum dot.
Embodiment 2:
Prepare CsPbI3Quantum dot
1. synthesize Cs presomas and Pb presoma
By 0.25mmol CsCO3, 0.25ml oleic acid (OA), 4ml octadecylene (ODE) add in three-necked flask, 90 DEG C vacuumize logical nitrogen after 30min, are heated to 150 DEG C until forming colourless solution, i.e. Cs presomas.
By 0.188mmol PbI2, 0.5ml oleic acid (OA), 0.5ml oleyl amine (OLA) and 5ml octadecylene (ODE) It is added separately in three-necked flask, leads to nitrogen after 30min is vacuumized at 90 DEG C, then be warming up to 150 DEG C, obtains Pb forerunner Body.
2. prepare CsPbI3Quantum dot
0.1ml Cs presomas are dissolved in 3ml chloroform, then take 1.5ml Pb presoma to be rapidly injected this In solution, that is, obtain CsPbI3Quantum dot.

Claims (1)

  1. A kind of 1. perovskite CsPbX3The synthetic method of quantum dot at room temperature, it is characterised in that comprise the following steps:
    A) caesium source, oleic acid (OA), octadecylene (ODE) are added in three-necked flask, leads to nitrogen after vacuumizing 30min at 90 DEG C, then 100-150 DEG C is heated to until forming colourless solution 1;
    B) lead source and halogen source, oleic acid (OA), oleyl amine (OLA) and 5ml octadecylene (ODE) are added separately in three-necked flask, Lead to nitrogen after 30min is vacuumized at 90 DEG C, then heat up 100-180 DEG C, obtain settled solution 2;
    C) at room temperature, or with temperature take solution 1 to be dissolved into the organic solvent containing chlorine element, reinject solution 2, stir and produce To CsPbX3Quantum dot, wherein X=Br, I;
    Or take solution 2 to be dissolved into the organic solvent containing chlorine element, solution 1 is reinjected, stirring obtains CsPbX3Quantum dot, Wherein X=Br, I;
    Described caesium source is Cs2CO3, one or more in CsCl;
    The lead source is PbCl2、PbBr2、PbI2, one or more in PbO;
    The halogen source is the halogen in lead source, if lead source is free of halogen, you can replaced with halogen-containing compound, such as NH4X;
    The described solvent containing chlorine element is dichloromethane, chloroform, tetrachloromethane or the mixed solvent containing above-mentioned solvent;
    Described solution 1 and the ratio of solution 2 are 1:3 to 1:10, or 3:1 to 10:1.
CN201610694070.0A 2016-08-19 2016-08-19 A kind of synthetic method of perovskite CsPbX3 quantum dots at room temperature Expired - Fee Related CN106379932B (en)

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CN107195789B (en) * 2017-06-01 2019-05-21 吉林大学 A kind of preparation method of inorganic mixed halogen perovskite thin film and its application in terms of preparing solar battery
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CN109092336A (en) * 2018-07-18 2018-12-28 河南工业大学 A kind of full-inorganic perovskite composite Ti O2Nano wire and preparation method thereof
CN109456763B (en) * 2018-10-15 2020-11-24 厦门大学 Synthesis method of lead-iodine perovskite quantum dots
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CN110184054B (en) * 2019-06-14 2022-05-17 纳晶科技股份有限公司 Preparation method of perovskite quantum dots
CN111892081A (en) * 2020-06-29 2020-11-06 南京理工大学 CsPbI3Mixed phase perovskite film and controllable preparation method thereof

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CN104934304B (en) * 2015-06-04 2018-04-27 苏州大学 A kind of method that mixed solvent induction regulating controlling by under room temperature obtains black cubic system perovskite thin film
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CN105331362B (en) * 2015-12-07 2017-08-04 南京理工大学 A kind of preparation method of the inorganic halogen perovskite fluorescence quantum of the big yield of room temperature
CN105733574B (en) * 2016-01-31 2018-06-12 南京理工大学 A kind of method that low temperature solution polycondensation prepares perovskite quantum dot
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