CN105331362B - A kind of preparation method of the inorganic halogen perovskite fluorescence quantum of the big yield of room temperature - Google Patents
A kind of preparation method of the inorganic halogen perovskite fluorescence quantum of the big yield of room temperature Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of the inorganic halogen perovskite fluorescence quantum of the big yield of room temperature, the luminescent quantum dot is CsPbX3, X=A in formulaxB1‑x, 0≤X≤1, A and B are any one in Cl, Br, I.This method comprises the following steps：Lead halide and caesium halide are dissolved in dimethylformamide first, and add surfactant oleyl amine and oleic acid, stirring obtains precursor solution after being completely dissolved, then precursor solution is instilled in poor solvent with 0.08~0.13mL/s speed, at the uniform velocity stirs and produce inorganic halogen perovskite fluorescence quantum CsPbX3.The present invention is carried out at normal temperatures, it is not necessary to protective gas, and equipment is simple, is produced on a large scale, by selecting halogen and adjusting its ratio, can be obtained total visible light wave band and be lighted.Inorganic halogen perovskite fluorescence quantum halfwidth made from the preparation method of the present invention is 16~39nm, and fluorescence quantum efficiency can stablize placement more than March close to 90%, available for fields such as solar cell, laser, photo-detector, light emitting diodes.
Description
Technical field
The present invention relates to a kind of preparation method of the inorganic halogen perovskite fluorescence quantum of the big yield of room temperature, belong to photoelectron
Technical field of material.
Background technology
Ca-Ti ore type semiconductor, especially Ca-Ti ore type Organic leadP halide (CH3NH3PbX3, X=F, Cl, Br, I) and because of it
Cost is low, efficiency high, energy gap is adjustable, has latent in fields such as solar cell, laser, photo-detector, light emitting diodes
Application value (J.Burschka, N.Pellet, S.-J.Moon, R.Humphry-Baker, P.Gao,
M.K.Nazeeruddin,M.Gratzel,Nature 2013,499,316).In area of solar cell, only triennium, with
The photoelectric transformation efficiency of solar cell based on the material has exceeded 20% (N.-G.Park, The Journal of
Physical Chemistry Letters 2013,4,2423)。
However, Ca-Ti ore type Organic leadP halide limits it in optoelectronic areas to the extreme sensitivity of air and moisture
Using.CH3NH3Extremely unstable under air condition, the degraded of Organic leadP perovskite is rapid.Protesescu et al. is noted using heat
Enter method, the halogen of different proportion is dissolved in octadecylene, and add surfactant oleic acid and oleyl amine, in argon gas and the ring of high temperature
Oleic acid caesium is injected under border, the inorganic lead halide (CsPbX of Ca-Ti ore type is obtained3), CsPbX3Not only it is likewise supplied with organic perovskite
Advantage, the problem of also overcoming unstable in air and steam well.But because of its harsh preparation requirement, such as high temperature is lazy
Property atmosphere etc. adds cost, reduces materials synthesis efficiency；In addition, there is also ask for the extensive preparation of hot injection method
Topic, can reduce product quality and monodispersity (L.Protesescu, S.Yakunin, M.I.Bodnarchuk, F.Krieg,
R.Caputo,C.H.Hendon,R.X.Yang,A.Walsh,M.V.Kovalenko,Nano Letters 2015,6,3692)。
The content of the invention
For deficiency of the prior art, the invention provides a kind of inorganic halogen perovskite fluorescent quantum of the big yield of room temperature
The preparation method of point, stable using product made from the preparation method, reaction is simple, quick, and is produced on a large scale.
Technical scheme is as follows：A kind of preparation side of the inorganic halogen perovskite fluorescence quantum of the big yield of room temperature
Method, is comprised the following steps that：Lead halide and caesium halide are dissolved in dimethylformamide (DMF) first, and add surfactant
Oleyl amine and oleic acid, stirring obtain precursor solution after being completely dissolved, then by precursor solution with 0.08~0.13mL/s speed
Degree is instilled in poor solvent, is at the uniform velocity stirred and is produced inorganic halogen perovskite fluorescence quantum CsPbX3, X=A in formulaxB1-x, 0
≤ X≤1, described A and B are selected from any of Cl, Br, I；Wherein, the mol ratio of caesium, lead and halogen is 1:1:3.
Any one of described poor solvent in toluene, n-hexane, normal heptane, normal octane, n-decane and chloroform.
Described mixing speed is 600~1200r/min.
Preferably, in the embodiment of the present invention, described lead halide or caesium halide contains lead chloride or chlorination
During caesium, cosolvent dimethyl sulfoxide (DMSO) is added in precursor solution, promotes the dissolving of lead chloride or cesium chloride.
The crystal structure of quantum dot prepared by the present invention is perovskite structure, and preparation is carried out at normal temperatures, it is not necessary to protected
Gas is protected, equipment is simple, is produced on a large scale, by selecting halogen and adjusting its ratio, total visible light wave band hair can be obtained
Light.I ratio is higher in raw material, and emission wavelength is longer；Cl content is higher in raw material, and emission wavelength is shorter；When halogen is pure
During Br, green light.Inorganic halogen perovskite fluorescence quantum halfwidth made from the inventive method is 16-39nm, fluorescent quantum
Efficiency can stablize placement more than March close to 90%.Quantum dot excellent performance prepared by the present invention, available for solar-electricity
The fields such as pond, laser, photo-detector, light emitting diode.
Brief description of the drawings
Fig. 1 is the UV absorption visible spectrum and fluorescence spectra of obtained perovskite quantum dot in embodiment 1.
Fig. 2 is the UV absorption visible spectrum and fluorescence spectra of obtained perovskite quantum dot in embodiment 2.
Fig. 3 is the UV absorption visible spectrum and fluorescence spectra of obtained perovskite quantum dot in embodiment 3.
Fig. 4 is the UV absorption visible spectrum and fluorescence spectra of obtained perovskite quantum dot in embodiment 4.
Fig. 5 is the UV absorption visible spectrum and fluorescence spectra of obtained perovskite quantum dot in embodiment 5.
Fig. 6 is the UV absorption visible spectrum and fluorescence spectra of obtained perovskite quantum dot in embodiment 6.
Fig. 7 is the UV absorption visible spectrum and fluorescence spectra of obtained perovskite quantum dot in embodiment 7.
Embodiment
The present invention is described in further detail with accompanying drawing with reference to embodiments.
Embodiment 1
(a) 0.0556g PbCl are weighed2, 0.0738g PbBr2, 0.0269g CsCl, 0.0341g CsBr, (mol ratio is
Cs:Pb:Cl:Br=1:1:1.5:1.5) it is dissolved in 10mL DMF, and adds 1mL oleic acid and 0.5mL oleyl amines.Because PbCl2
With CsCl compared with indissoluble solution, therefore add 3mL dimethyl sulfoxide (DMSO)s (DMSO) hydrotropy.
(b) after stirring and dissolving 10min, measure 2mL precursor solution and instilled with 0.1mL/s speed in 10mL toluene,
And keep 1000 revs/min of speed persistently to stir.Luminescent quantum dot is formed in 5s clocks.All operating process are normal in normal temperature
Pressure is carried out, it is not necessary to protective gas.As shown in figure 1, the luminescent quantum dot maximum emission wavelength prepared is 455nm, crystal knot
Structure is perovskite structure, and halfwidth is 16nm, and fluorescence quantum efficiency is 37%.
Embodiment 2
(a) 0.0371g PbCl are weighed2, 0.0984g PbBr2, 0.018g CsCl, 0.0454g CsBr, (mol ratio is
Cs:Pb:Cl:Br=1:1:1:2) it is dissolved in 10mL DMF, and adds 1mL oleic acid and 0.5mL oleyl amines.Because PbCl2With
CsCl adds 3mL dimethyl sulfoxide (DMSO)s (DMSO) hydrotropy compared with indissoluble solution.
(b) after stirring and dissolving 10min, measure 2mL precursor solution and instilled with 0.08mL/s speed in 10mL toluene,
And keep 1000 revs/min of speed persistently to stir.Luminescent quantum dot is formed in 5s clocks.All operating process are normal in normal temperature
Pressure is carried out, it is not necessary to protective gas.As shown in Fig. 2 the luminescent quantum dot maximum emission wavelength prepared is 478nm, crystal knot
Structure is perovskite structure, and halfwidth is 18nm, and fluorescence quantum efficiency is 62%.
Embodiment 3
(a) 0.0681g PbBr is weighed2, 0.1476g CsBr, (mol ratio is Cs:Pb:Br=1:1:3) it is dissolved in
In 10mL DMF, and add 1mL oleic acid and 0.5mL oleyl amines.
(b) after stirring and dissolving 10min, measure 2mL precursor solution and instilled with 0.13mL/s speed in 10mL toluene,
And keep 1000 revs/min of speed persistently to stir.Luminescent quantum dot is formed in 1s clocks.All operating process are normal in normal temperature
Pressure is carried out, it is not necessary to protective gas.As shown in figure 3, the luminescent quantum dot maximum emission wavelength prepared is 513nm, crystal knot
Structure is perovskite structure, and halfwidth is 20nm, and fluorescence quantum efficiency is 88%.
Embodiment 4
(a) 0.0984g PbBr are weighed2, 0.0615g PbI2, 0.0454g CsBr, 0.0277g CsI, (mol ratio is
Cs:Pb:Br：I=1:1:2:1) it is dissolved in 10mL DMF, and adds 1mL oleic acid and 0.5mL oleyl amines.
(b) after stirring and dissolving 10min, measure 2mL precursor solution and 10mL toluene is instilled with 0.1mL each second speed
In, and keep 600 revs/min of speed persistently to stir.Luminescent quantum dot is formed in 5s clocks.All operating process are in normal temperature
Carried out under normal pressure, it is not necessary to protective gas.As shown in figure 4, the luminescent quantum dot maximum emission wavelength prepared is 548nm, crystal
Structure is perovskite structure, and halfwidth is 26nm, and fluorescence quantum efficiency is 78%.
Embodiment 5
(a) 0.0738g PbBr are weighed2, 0.0922g PbI2, 0.034g CsBr, 0.0416g CsI, (mol ratio is Cs:
Pb:Br：I=1:1:1.5:1.5) it is dissolved in 10mL DMF, and adds 1mL oleic acid and 0.5mL oleyl amines.
(b) after stirring and dissolving 10min, measure 2mL precursor solution and 10mL toluene is instilled with 0.1mL each second speed
In, and keep 1200 revs/min of speed persistently to stir.Luminescent quantum dot is formed in 5s clocks.All operating process are normal
Carried out under normal temperature and pressure, it is not necessary to protective gas.As shown in figure 5, the luminescent quantum dot maximum emission wavelength prepared is 600nm, it is brilliant
Body structure is perovskite structure, and halfwidth is 38nm, and fluorescence quantum efficiency is 72%.
Embodiment 6
(a) 0.044g PbBr are weighed2, 0.1106g PbI2, (mol ratio is Cs to 0.0292g CsBr, 0.0561g CsI:
Pb:Br:I=1:1:1.2:1.8) it is dissolved in 10mL DMF, and adds 1mL oleic acid and 0.5mL oleyl amines.
(b) after stirring and dissolving 10min, measure 2mL precursor solution and 10mL chloroforms are instilled with 0.1mL each second speed
In, and keep 1000 revs/min of speed persistently to stir.Luminescent quantum dot is formed in 5s clocks.All operating process are normal
Carried out under normal temperature and pressure, it is not necessary to protective gas.As shown in fig. 6, the luminescent quantum dot maximum emission wavelength prepared is 628nm, it is brilliant
Body structure is perovskite structure, and halfwidth is 39nm, and fluorescence quantum efficiency is 75%.
Embodiment 7
(a) 0.0382g PbBr are weighed2, 0.1030g PbI2, (mol ratio is Cs to 0.0227g CsBr, 0.0544g CsI:
Pb:Br：I=1:1:1:2) it is dissolved in 10mL DMF, and adds 1mL oleic acid and 0.5mL oleyl amines.
(b) after dissolving 10min, measure 2mL precursor solution and 10mL n-hexanes are instilled with 0.1mL each second speed
In, and keep 1000 revs/min of speed persistently to stir.Luminescent quantum dot is formed in 5s clocks.All operating process are normal
Carried out under normal temperature and pressure, it is not necessary to protective gas.As shown in fig. 7, the luminescent quantum dot maximum emission wavelength prepared is 640nm, it is brilliant
Body structure is perovskite structure, and halfwidth is 35nm, and fluorescence quantum efficiency is 70%.
Claims (4)
1. a kind of preparation method of the inorganic halogen perovskite fluorescence quantum of the big yield of room temperature, it is characterised in that specific steps are such as
Under：Lead halide and caesium halide are dissolved in dimethylformamide first, and add surfactant oleyl amine and oleic acid, stirring is complete
Precursor solution is obtained after dissolving, then instills precursor solution in poor solvent with 0.08~0.13mL/s speed, it is even
Speed, which stirs, produces inorganic halogen perovskite fluorescence quantum CsPbX3, X=A in formulaxB1-x, 0≤X≤1, described A and B are selected
From any of Cl, Br, I；Wherein, the mol ratio of caesium, lead and halogen is 1:1:3.
2. preparation method according to claim 1, it is characterised in that described poor solvent is selected from toluene, n-hexane, just
Any one in heptane, normal octane, n-decane and chloroform.
3. preparation method according to claim 1, it is characterised in that described mixing speed is 600~1200r/min.
4. preparation method according to claim 1, it is characterised in that described lead halide or caesium halide contain lead chloride or
During cesium chloride, cosolvent dimethyl sulfoxide (DMSO) is added in described precursor solution.
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| CN104388089A (en) * | 2014-11-04 | 2015-03-04 | 北京理工大学 | High-fluorescence-quantum-yield hybridized perovskite quantum dot material and preparation method thereof |
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