CN110499150A - A kind of preparation method of the caesium lead bromine core-shell nano crystalline substance of coated with silica - Google Patents
A kind of preparation method of the caesium lead bromine core-shell nano crystalline substance of coated with silica Download PDFInfo
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- CN110499150A CN110499150A CN201910921039.XA CN201910921039A CN110499150A CN 110499150 A CN110499150 A CN 110499150A CN 201910921039 A CN201910921039 A CN 201910921039A CN 110499150 A CN110499150 A CN 110499150A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
A kind of preparation method of the caesium lead bromine core-shell nano crystalline substance of coated with silica of the invention belongs to the technical field of nano material preparation.First, cesium bromide and lead bromide are added to N, in dinethylformamide, again to middle addition oleic acid and oleyl amine, 110 DEG C are stirred and heated in oil bath pan, and stir 6 hours obtain clear yellow solution at this temperature, resulting yellow solution is added dropwise in the ammonia spirit that concentration is 2.8% and obtains precursor liquid；Then by its mixed liquor for being added dropwise to methyl silicate and toluene of resulting precursor liquid, magnetic agitation 2 hours at 30 DEG C obtain the core-shell nano crystalline substance of the coated with silica caesium lead bromine of favorable dispersibility.The present invention has the advantages that process simple, pattern of product and repeatability are high, and the sample phase purity of preparation is very high, good crystallinity, particle diameter distribution is uniform, quantum yield is high.
Description
Technical field
The invention belongs to the technical field of nano material preparation, in particular to the caesium lead bromine nucleocapsids of a kind of coated with silica
It is nanocrystalline and preparation method thereof.
Background technique
Metal halogen perovskite is led because of its excellent photoelectric properties and cheap cost in photoelectric device and solar energy
Domain is concerned.Especially organic metal halogen perovskite has caused in the successful application of photovoltaic device to inorganic halide in recent years
The nanocrystalline research of plain perovskite.As a kind of novel perovskite material, inorganic lead base CsPbX3(X=Cl, Br, I) halogen
Perovskite causes rapidly the concern of scientists.Especially caesium lead bromine is nanocrystalline has high luminescence generated by light quantum yield, narrow
The advantages that transmitting band and tunable fluorescence spectrum, has broader photovoltaic applications prospect.Although caesium lead bromine is in application aspect
With tempting development prospect, but it is more sensitive to oxygen and moisture at present, therefore there are still challenges in practical applications.
In order to improve the stability of caesium lead bromine, there is document to provide the method nanocrystalline using coated with silica caesium lead bromine at present,
For example, German chemical association magazine (Angewandte Chemie International Edition 2017.56.8134-
8138.) it is reported on: caesium lead bromine quantum dot being added to by silica/tri- using simple sol-gal process in toluene solution
In Al 2 O monomer, the silica/alumina monomer quantum dot of high stability and quantum yield is obtained；Advanced optical material
It is reported on magazine (Advanced Optical Materials 2018.3.1700997): by hot injection method by caesium lead bromine amount
Son point is embedded into anhydride silica ball, effectively improves the moisture resistance of quantum dot, enhances photostability.But it is above two
The sample that synthetic method is prepared is that multiple caesium lead bromines are coated in a silica core-shell is nanocrystalline.
Summary of the invention
The technical problem to be solved by the present invention is overcoming problem and shortage existing for background technique, a kind of titanium dioxide is provided
The caesium lead bromine core-shell nano crystalline substance and preparation method thereof of silicon cladding.
Specific technical solution of the invention is as follows:
A kind of preparation method of the caesium lead bromine core-shell nano crystalline substance of coated with silica, is carried out under air environment；It is first
First, the cesium bromide of molar ratio 1:1 and lead bromide are added in n,N-Dimethylformamide, then to middle addition oleic acid and oleyl amine,
Wherein, every 0.1mmol lead bromide uses 2.5mL n,N-Dimethylformamide, 0.15mL oleic acid and 0.45mL oleyl amine, in oil bath
110 DEG C are stirred and heated in pot, and stirs 6 hours obtain clear yellow solution at this temperature, resulting yellow is molten
Liquid, which is added dropwise in the ammonia spirit that concentration is 2.8%, obtains precursor liquid, and the volume ratio of the yellow solution and ammonium hydroxide is 1:
0.02；Then by its mixed liquor for being added dropwise to methyl silicate and toluene of resulting precursor liquid, the precursor liquid and silicic acid first
The volume ratio of ester and toluene is 0.2:0.005:10, and magnetic agitation 2 hours at 30 DEG C obtain the silica of favorable dispersibility
The core-shell nano for coating caesium lead bromine is brilliant.
In preparation process of the present invention, it is the nucleocapsid of each silica that obtained coated with silica caesium lead bromine is nanocrystalline
In only single caesium lead bromine it is nanocrystalline.
The utility model has the advantages that
The advantages of present invention preparation coated with silica caesium lead bromine nanometer crystal method is: the sample phase purity of preparation is very
Height, good crystallinity, particle diameter distribution are uniform, quantum yield is high；And this preparation method has process simple, pattern of product and can
The advantages that repeatability is high.With the nanocrystalline potentiality of large-scale production coated with silica caesium lead bromine.
Detailed description of the invention
Fig. 1 is the nanocrystalline transmission electron microscope picture of the coated with silica caesium lead bromine of the preparation of embodiment 1.
Fig. 2 is the nanocrystalline high resolution electron microscopy figure of the coated with silica caesium lead bromine of the preparation of embodiment 1.
Fig. 3 is the nanocrystalline transmission electron microscope picture of the caesium lead bromine of the preparation of embodiment 1.
Fig. 4 is the nanocrystalline high resolution electron microscopy figure of the caesium lead bromine of the preparation of embodiment 1.
Fig. 5 is the nanocrystalline fluorescence spectrum of the coated with silica caesium lead bromine of the preparation of embodiment 1.
Fig. 6 is the nanocrystalline absorption spectra of the coated with silica caesium lead bromine of the preparation of embodiment 1.
Specific embodiment
The present invention is more specifically described now in conjunction with the following example, unless otherwise specified, agents useful for same be it is commercially available can
The product of acquisition is purified not plus further and is used.
It is nanocrystalline that 1 synthetic silica of embodiment coats caesium lead bromine
It is to carry out in air that it is nanocrystalline, which to coat caesium lead bromine, for synthetic silica, and specific synthesis process is as follows: by 10mL's
N,N-Dimethylformamide is fitted into triangular flask, later successively by load weighted 0.0855g cesium bromide (0.4mmol) and
The lead bromide (0.4mmol) of 0.1476g is added in triangular flask, and the oleyl amine of the oleic acid and 1.8mL that then take 0.6mL is respectively dropped into
Into triangular flask, triangular flask is placed in oil bath pan and is stirred and heated to 110 DEG C, 6 hours is persistently stirred in this temperature, directly
To obtaining uniform yellow solution.It takes out 2mL and is added dropwise to and fill the ammonia spirit that concentration that 40 μ L are prepared in advance is 2.8%
In, obtain precursor liquid.The precursor liquid of 0.2mL is taken quickly to be added dropwise to the triangle for filling 5 μ L methyl silicates and 10mL toluene mixture liquid
In bottle, and sample is extracted after persistently stirring 2 hours under conditions of 30 DEG C, obtained solution is centrifuged 5 points with 9000rpm/min
Clock obtains the nanocrystalline of coated with silica caesium lead bromine after dry.
The nanocrystalline transmission electron microscope picture of coated with silica caesium lead bromine manufactured in the present embodiment is as shown in Figure 1, silica
Coating the nanocrystalline average length of caesium lead bromine is about 43nm.Fig. 2 is the nanocrystalline high-resolution electricity of coated with silica caesium lead bromine
Mirror picture shows that this is nanocrystalline with good crystallinity.Fig. 3 is the nanocrystalline transmission electron microscope picture of caesium lead bromine, and average-size is about
For 20nm.Fig. 4 is the nanocrystalline high resolution electron microscopy picture of caesium lead bromine, illustrates that the crystallinity of caesium lead bromine is very good.This shows dioxy
It is nanocrystalline later without influencing the nanocrystalline lattice of caesium lead bromine that SiClx coats caesium lead bromine.
The nanocrystalline optical property of 2 coated with silica caesium lead bromine of embodiment
The fluorescence and absorption spectra such as Fig. 5 of the nanocrystalline sample of coated with silica caesium lead bromine prepared by embodiment 1,6 show, by attached
Figure is it can be seen that sample has very high quantum yield and monodispersity.Fig. 5 is the nanocrystalline sample of coated with silica caesium lead bromine
Fluorescence spectrum.Fig. 6 is the absorption spectra of the nanocrystalline sample of coated with silica caesium lead bromine.
Claims (1)
1. a kind of preparation method of the caesium lead bromine core-shell nano crystalline substance of coated with silica, is carried out under air environment；Firstly,
The cesium bromide of molar ratio 1:1 and lead bromide are added in n,N-Dimethylformamide, then to middle addition oleic acid and oleyl amine,
In, every 0.1mmol lead bromide uses 2.5mL n,N-Dimethylformamide, 0.15mL oleic acid and 0.45mL oleyl amine, in oil bath pan
In be stirred and heated to 110 DEG C, and stir obtain clear yellow solution in 6 hours at this temperature, by resulting yellow solution
It is added dropwise in the ammonia spirit that concentration is 2.8% and obtains precursor liquid, the volume ratio of the yellow solution and ammonium hydroxide is 1:0.02；
Then by its mixed liquor for being added dropwise to methyl silicate and toluene of resulting precursor liquid, the precursor liquid and methyl silicate and first
The volume ratio of benzene is 0.2:0.005:10, and magnetic agitation 2 hours at 30 DEG C obtain the coated with silica caesium of favorable dispersibility
The core-shell nano of lead bromine is brilliant.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112808282A (en) * | 2021-01-20 | 2021-05-18 | 河南大学 | Cesium-lead-bromine perovskite @ silicon dioxide hollow mesoporous spherical core-shell structure, and preparation method and application thereof |
| CN115044366A (en) * | 2022-07-15 | 2022-09-13 | 广州医科大学 | Preparation method of exosome-modified perovskite quantum dot, product and application thereof |
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| CN105384189A (en) * | 2015-12-23 | 2016-03-09 | 济南大学 | Method for preparing caesium-lead halide nanorod and product obtained through method |
| CN107128967A (en) * | 2017-05-08 | 2017-09-05 | 厦门大学 | A kind of nanocrystalline synthetic method of full-inorganic CsPbX3 perovskites |
| CN108101103A (en) * | 2018-02-08 | 2018-06-01 | 河北工业大学 | A kind of caesium lead halogen Cs4PbX6Nanocrystalline synthetic method |
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2019
- 2019-09-26 CN CN201910921039.XA patent/CN110499150A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384189A (en) * | 2015-12-23 | 2016-03-09 | 济南大学 | Method for preparing caesium-lead halide nanorod and product obtained through method |
| CN107128967A (en) * | 2017-05-08 | 2017-09-05 | 厦门大学 | A kind of nanocrystalline synthetic method of full-inorganic CsPbX3 perovskites |
| CN108101103A (en) * | 2018-02-08 | 2018-06-01 | 河北工业大学 | A kind of caesium lead halogen Cs4PbX6Nanocrystalline synthetic method |
Non-Patent Citations (1)
| Title |
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| QIXUAN ZHONG ET AL.，: ""One-Pot Synthesis of Highly Stable CsPbBr3@SiO2 Core−Shell Nanoparticles"", 《ACS NANO》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112808282A (en) * | 2021-01-20 | 2021-05-18 | 河南大学 | Cesium-lead-bromine perovskite @ silicon dioxide hollow mesoporous spherical core-shell structure, and preparation method and application thereof |
| CN115044366A (en) * | 2022-07-15 | 2022-09-13 | 广州医科大学 | Preparation method of exosome-modified perovskite quantum dot, product and application thereof |
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