CN107384386A - A kind of perovskite CsPbX3The synthetic method of quantum wire - Google Patents

A kind of perovskite CsPbX3The synthetic method of quantum wire Download PDF

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CN107384386A
CN107384386A CN201710472597.3A CN201710472597A CN107384386A CN 107384386 A CN107384386 A CN 107384386A CN 201710472597 A CN201710472597 A CN 201710472597A CN 107384386 A CN107384386 A CN 107384386A
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quantum wire
lead
cspbx
presoma
perovskite
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CN107384386B (en
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曹万强
方凡
刘培朝
李阳
王仁龙
梅�明
张慧婕
曾媛媛
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Hubei University
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Hubei University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
    • C09K11/664—Halogenides
    • C09K11/665—Halogenides with alkali or alkaline earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The invention discloses a kind of perovskite CsPbX3The synthetic method (wherein X=Cl, Br, I) of quantum wire, its step are：The presoma of caesium is prepared with cesium salt, oleic acid, octadecylene；The presoma of lead and halogen is prepared with lead salt and haloid, oleic acid, oleyl amine and 5ml octadecylene；The presoma of caesium, lead, halogen is distributed in non-polar solven, adds 5% to 30% polar solvent of the amount of non-polar solven, it is agitated to can obtain CsPbX3Quantum wire.It is the difference of the group orientation and part carried using polar solvent, synthesizes perovskite CsPbX3Quantum wire.The CsPbX that the present invention obtains3Perovskite quantum wire；Its wavelength covers 380nm-700nm, a width of 18-40nm 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 perovskite CsPbX3The synthetic method of quantum wire
Technical field
The present invention relates to nano material synthesis technical field, and in particular to a kind of perovskite CsPbX3(X=Cl, Br, I) is measured The synthetic method of sub-line.
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.
Quantum wire can be regarded as a kind of continuity of zero-dimensional quantum dots as a kind of one-dimensional material.Except with quantum dot Some basic characteristics outside, also make quantum wire in area source, display, solar energy with other properties, the performance Field of batteries is with a wide range of applications.At present, CsPbX3Perovskite quantum wire is only in high―temperature nuclei, and see reference document Zhang, D.；Eaton,S.W.；Yu,Y.；Dou,L.；Yang,P.,Solution‐Phase Synthesis of Cesium Lead Halide Perovskite Nanowires.Journal of the American Chemical Society 2015,137,9230-3. and Bekenstein, Y.；Koscher,B.A.；Eaton,S.W.；Yang,P.；Alivisatos, A.P.,Highly Luminescent Colloidal Nanoplates of Perovskite Cesium Lead Halide and Their Oriented Assemblies.Journal of the American Chemical Society 2015, 137,16008‐11.
CsPbX3Perovskite quantum wire is synthesizing then blank out close to room temperature, and the application to quantum wire brings certain tired Difficulty, exploitation room temperature synthesis CsPbX3Perovskite quantum wire has obvious process meaning to development and application.
The content of the invention
It is an object of the invention to provide a kind of CsPbX3The new synthetic method of quantum wire, it is catalyzed using being used as containing polar solvent Agent, reduce CsPbX in traditional octadecylene or paraffin systems3The synthesis temperature of quantum wire, make presoma rapid at room temperature Reaction generation CsPbX3Quantum wire, wherein X=Cl, Br, I.The CsPbX3Quantum dot wavelength covers 380nm-700nm, transmitting half Peak width is 18-40nm.The method reaction temperature is low, and raw material is cheap, and aggregate velocity is fast, simple to operate, is adapted to extensive batch raw Production.
A kind of CsPbX3The preparation method of quantum wire, specifically includes following steps；
A) cesium salt, oleic acid (OA), octadecylene (ODE) are added in three-necked flask, leads to nitrogen after vacuumizing 30min at 90 DEG C Gas, it is heated to the 100-150 DEG C of presoma until forming caesium；
B) lead salt and haloid, oleic acid (OA), oleyl amine (OLA) and 5ml octadecylene (ODE) are added separately to three mouthfuls of burnings In bottle, lead to nitrogen after 30min is vacuumized at 90 DEG C, then heat up 100-180 DEG C, obtain the presoma of lead and halogen；
C) presoma of caesium, lead, halogen is distributed in non-polar solven, add the amount of non-polar solven 5% arrives 30% polar solvent, it is agitated to can obtain CsPbX3Quantum wire, wherein X=Cl, Br, I；
Described cesium salt is Cs2CO3, one or more in CsCl；
The lead salt is PbCl2、PbBr2、PbI2, one or more in PbO；
The haloid is halogen-containing lead salt, or without halogen lead salt；
Described non-polar solven is hexane, toluene or the mixed solvent containing above-mentioned solvent；
Described polar solvent is ethanol, propyl alcohol, butanol, acetone or the mixed solvent containing above-mentioned solvent；
The present invention can be applied in display or solar cell or laser device.
The technological core of the invention is, as catalyst, will be dispersed in nonpolar using with orientation polar solvent Presoma catalytic ionization synthesizes CsPbX in room temperature orientation solvent3Quantum wire.It is the group carried using polar solvent The difference of orientation and part, synthesis perovskite CsPbX3Quantum wire
Agitated obtained CsPbX3Perovskite quantum wire；Its wavelength covers 380nm-700nm, a width of 18- of transmitting half-peak 40nm.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.
Brief description of the drawings
The CsPbX of Fig. 1 different components3Quantum wire fluorescence emission spectrogram of compound；
CsPbBr in Fig. 2 embodiments 13Quantum wire high power transmission electron microscope picture
Embodiment
Embodiment 1：
Prepare CsPbBr3Quantum wire
1. synthesize Cs, Pb, Br 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's and Br Presoma.
2. prepare CsPbBr3Quantum wire
The presoma of 0.1ml Cs presomas, 1.5ml Pb and Br is dispersed in 10ml non-polar solven hexanes, then Take 0.5ml polar solvent acetone soln to be rapidly injected in hexane, that is, obtain CsPbBr3Quantum wire.
Embodiment 2：
Prepare CsPbBr1.5I1.5Quantum wire
1. synthesize Cs, Pb, Br, I 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's and Br Presoma.
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, before obtains Pb and I Drive body.
2. prepare CsPbBr1.5I1.5Quantum wire
0.1ml Cs presomas, 0.75ml Pb and Br presoma, 0.75ml Pb and I presoma are dispersed in In 10ml non-polar solven hexane solvents, then take 0.5ml polar solvent acetone soln to be rapidly injected in hexane, that is, obtain CsPbBr1.5I1.5Quantum wire.
Embodiment 3：
Prepare CsPbI3Quantum wire
1. synthesize Cs, Pb, I 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, before obtains Pb and I Drive body.
2. prepare CsPbI3Quantum wire
The presoma of 0.1ml Cs presomas, 1.5ml I is dispersed in 10ml non-polar solven hexane solvents, then taken 0.5ml polar solvent acetone soln is rapidly injected in hexane, that is, obtains CsPbI3Quantum wire.
Embodiment 4：
Prepare CsPbCI3Quantum wire
1. synthesize Cs, Pb, Cl 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 PbCl2, 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's and Cl Presoma.
2. prepare CsPbCI3Quantum wire
The presoma of 0.1ml Cs presomas, 1.5ml Pb and Cl is dispersed in 10ml non-polar solven hexane solvents In, then take 0.5ml polar solvent acetone soln to be rapidly injected in hexane, that is, obtain CsPbCI3Quantum wire.

Claims (2)

  1. A kind of 1. perovskite CsPbX3The synthetic method of quantum wire, it is characterised in that comprise the following steps：
    A) cesium salt, oleic acid (OA), octadecylene (ODE) are added in three-necked flask, leads to nitrogen after vacuumizing 30min at 90 DEG C, then It is heated to the 100-150 DEG C of presoma until forming caesium；
    B) lead salt and haloid, 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 the presoma of lead and halogen；
    C) presoma of caesium, lead, halogen is distributed in non-polar solven, adds 5% to the 30% of the amount of non-polar solven Polar solvent, it is agitated to can obtain CsPbX3Quantum wire, wherein X=Cl, Br, I；
    Described cesium salt is Cs2CO3, one or more in CsCl；
    The lead salt is PbCl2、PbBr2、PbI2, one or more in PbO；
    The haloid is halogen-containing lead salt, or without halogen lead salt；
    Described non-polar solven is hexane, toluene or the mixed solvent containing above-mentioned solvent；
    Described polar solvent is ethanol, propyl alcohol, acetone or the mixed solvent containing above-mentioned solvent.
  2. A kind of 2. perovskite CsPbX according to claim 13Synthesize perovskite CsPbX prepared by quantum wire synthetic method3 Synthesize quantum wire, it is characterised in that apply in display or solar cell or laser device.
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108217718A (en) * 2018-03-13 2018-06-29 南方科技大学 A kind of ABX3Nanocrystalline synthetic method of perovskite and products thereof and purposes
CN108585031A (en) * 2018-05-15 2018-09-28 宁波工程学院 CsPb0.922Sn0.078I3The method of perovskite nanobelt and the controlledly synthesis nanobelt
CN109231262A (en) * 2018-10-24 2019-01-18 华中科技大学 A kind of direct synthesis of cubic phase CsPbI3The method of nano wire
CN109736073A (en) * 2019-01-10 2019-05-10 陕西科技大学 A kind of height mould proof terylene and preparation method thereof quantum-dot modified using tin based perovskites
CN109775750A (en) * 2019-02-11 2019-05-21 陕西科技大学 A kind of solwution method prepares full-inorganic perovskite CsPbBr3The method and up-conversion luminescent material of nano wire
WO2020077905A1 (en) * 2018-10-15 2020-04-23 武汉华星光电半导体显示技术有限公司 Quantum dot preparation method and quantum dot
CN111204797A (en) * 2020-01-17 2020-05-29 南京工业大学 Morphology-controllable all-inorganic CsPbBr3Preparation method of perovskite nanocrystal
CN111892081A (en) * 2020-06-29 2020-11-06 南京理工大学 CsPbI3Mixed phase perovskite film and controllable preparation method thereof
CN112897577A (en) * 2021-01-31 2021-06-04 福建工程学院 Method for regulating and controlling nonlinear optical amplitude limiting performance of perovskite quantum dots
CN114276800A (en) * 2021-11-27 2022-04-05 苏州大学 Methylamine metal halide perovskite quantum dot, solar cell and preparation method of methylamine metal halide perovskite quantum dot
CN114956164A (en) * 2022-07-05 2022-08-30 电子科技大学 Cubic alpha-CsPbI 3 Rapid synthesis of rod-shaped delta-CsPbI by inducing lattice distortion 3 Method (2)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106379932A (en) * 2016-08-19 2017-02-08 湖北大学 A method of synthesizing a perovskite CsPbX3 quantum dot at room temperature

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106379932A (en) * 2016-08-19 2017-02-08 湖北大学 A method of synthesizing a perovskite CsPbX3 quantum dot at room temperature

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108217718A (en) * 2018-03-13 2018-06-29 南方科技大学 A kind of ABX3Nanocrystalline synthetic method of perovskite and products thereof and purposes
CN108585031A (en) * 2018-05-15 2018-09-28 宁波工程学院 CsPb0.922Sn0.078I3The method of perovskite nanobelt and the controlledly synthesis nanobelt
WO2020077905A1 (en) * 2018-10-15 2020-04-23 武汉华星光电半导体显示技术有限公司 Quantum dot preparation method and quantum dot
CN109231262A (en) * 2018-10-24 2019-01-18 华中科技大学 A kind of direct synthesis of cubic phase CsPbI3The method of nano wire
CN109736073A (en) * 2019-01-10 2019-05-10 陕西科技大学 A kind of height mould proof terylene and preparation method thereof quantum-dot modified using tin based perovskites
CN109775750A (en) * 2019-02-11 2019-05-21 陕西科技大学 A kind of solwution method prepares full-inorganic perovskite CsPbBr3The method and up-conversion luminescent material of nano wire
CN109775750B (en) * 2019-02-11 2021-05-04 陕西科技大学 Solution method for preparing all-inorganic perovskite CsPbBr3Method for preparing nanowires and up-conversion luminescent material
CN111204797A (en) * 2020-01-17 2020-05-29 南京工业大学 Morphology-controllable all-inorganic CsPbBr3Preparation method of perovskite nanocrystal
CN111892081A (en) * 2020-06-29 2020-11-06 南京理工大学 CsPbI3Mixed phase perovskite film and controllable preparation method thereof
CN112897577A (en) * 2021-01-31 2021-06-04 福建工程学院 Method for regulating and controlling nonlinear optical amplitude limiting performance of perovskite quantum dots
CN114276800A (en) * 2021-11-27 2022-04-05 苏州大学 Methylamine metal halide perovskite quantum dot, solar cell and preparation method of methylamine metal halide perovskite quantum dot
CN114956164A (en) * 2022-07-05 2022-08-30 电子科技大学 Cubic alpha-CsPbI 3 Rapid synthesis of rod-shaped delta-CsPbI by inducing lattice distortion 3 Method (2)

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