CN110607172B - Preparation method of perovskite/titanium dioxide composite nanocrystal - Google Patents

Preparation method of perovskite/titanium dioxide composite nanocrystal Download PDF

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CN110607172B
CN110607172B CN201910789106.7A CN201910789106A CN110607172B CN 110607172 B CN110607172 B CN 110607172B CN 201910789106 A CN201910789106 A CN 201910789106A CN 110607172 B CN110607172 B CN 110607172B
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perovskite
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titanium dioxide
oleic acid
octadecene
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CN110607172A (en
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唐孝生
卞瑶
杜鹃
张孟
叶怀宇
孙立东
张国旗
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Southwest University of Science and Technology
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Abstract

The invention provides a preparation method of a perovskite/titanium dioxide composite nanocrystal, which comprises the following steps: 1) Mixing cesium carbonate, an octadecene solution and oleic acid, and reacting to obtain a cesium oleate precursor solution; 2) Mixing lead halide, octadecene solution, oleic acid and oleylamine, and quickly reacting the obtained mixed solution with the cesium oleate precursor solution to obtain a perovskite quantum dot solution; 3) Purifying the perovskite quantum dot solution by using toluene to obtain a perovskite toluene solution; 4) And mixing the perovskite toluene solution with the titanium dioxide nanotube to obtain the perovskite/titanium dioxide composite nanocrystal. Compared with the prior art, the perovskite/titanium dioxide composite nanocrystal prepared by adopting the simple liquid phase synthesis method successfully excites two-photon random laser, and provides a new opportunity for frequency rising conversion.

Description

Preparation method of perovskite/titanium dioxide composite nanocrystal
Technical Field
The invention relates to application of a perovskite material in the field of laser, in particular to a preparation method of a perovskite/titanium dioxide composite nanocrystal.
Background
Nanometer laser has attracted more and more attention in recent years, and is widely applied to the fields of super-resolution biomedical imaging, ultra-high density data storage, integrated optical chips and the like. The two-photon pumping laser does not need phase matching and plays an important role in the fields of three-dimensional material manufacturing and biology.
Nanocrystal Quantum Dots (QDs) derive low dimensional properties with significant advantages due to size effects, quantum confinement effects, macroscopic quantum tunneling and surface effects, such as narrow emission peaks and simple synthesis methods, with tremendous potential in low-threshold laser applications.
Nanocrystalline Quantum Dots (QDs) have significant advantages such as narrow emission peak and simple synthesis method, especially inorganic perovskite quantum dots not only provide high photoluminescence quantum yield (PLQY) and narrow full width at half maximum (FWHM), but also can achieve full coverage of visible light of the emission spectrum by adjusting the composition of halide elements. These properties give them great potential in low threshold laser applications. However, csPbX 3 The further development of perovskite quantum dot-based optoelectronic devices has been hindered by the purification difficulty of quantum dots. Although the quantum dots are buried in silicon dioxide before the collection and purification are achieved, the thickness of the shell is difficult to control, and the quality of the cavity of a general laser is high.
Disclosure of Invention
The invention aims to solve the problems and provides CsPbBr 3 /TiO 2 The preparation method of the nano composite material is characterized by comprising the following steps:
1) Mixing cesium carbonate, an octadecene solution and oleic acid, and reacting to obtain a cesium oleate precursor solution;
2) Mixing lead halide, octadecene solution, oleic acid and oleylamine, and quickly reacting the obtained mixed solution with the cesium oleate precursor solution to obtain a perovskite quantum dot solution;
3) Purifying the perovskite quantum dot solution by using toluene to obtain a perovskite toluene solution;
4) And mixing the perovskite toluene solution with the titanium dioxide nanotube to obtain the perovskite/titanium dioxide composite nanocrystal.
Preferably, in the step 1), the mass volume ratio of the cesium carbonate to the oleic acid is 50-150mg:0.6ml; the mass concentration of the cesium carbonate in the oleic acid and octadecene solution is 20-30mg/L.
Preferably, in the step 1), the reaction is carried out under a protective gas condition; the reaction temperature is 100-150 ℃, and the reaction time is 40-90min.
Preferably, in the step 2), the mass concentration of the lead halide in the octadecene solution is 1-15mg/ml; the volume ratio of the oleic acid to the oleylamine is 1-2; the volume percentage of the oleic acid in the octadecene is 5-15%; the volume percentage content of the potassium oleate precursor solution in the octadecene is 8-12%.
Preferably, in the step 2), the lead halide, the octadecene solution, the oleic acid and the oleylamine are mixed specifically as follows: under the condition of protective gas, lead halide and octadecene are mixed, heated and kept warm, then heated to 150-170 ℃, and oleic acid and oleylamine are added.
Preferably, the temperature for heat preservation is 110-130 ℃, and the time for heat preservation is 30-60min.
Preferably, the reaction is carried out under the condition of protective gas; the reaction temperature is 150-170 ℃, and the rapid reaction time is 5-15s.
Preferably, said step 2) comprises an ice bath after the rapid reaction.
Preferably, in step 4), the TiO is 2 The mass concentration of the nano tube in the perovskite toluene solution is 2-3mg/mL.
Preferably, in the step 4), the perovskite toluene solution and the titanium dioxide nanotubes are mixed and then ultrasonically vibrated for 0.5 to 1 hour.
Preferably, the perovskite/titanium dioxide composite nanocrystal prepared by the preparation method is prepared.
Preferably, the perovskite/titanium dioxide composite nanocrystal is applied to the preparation of solar cells, light emitting diodes or lasers.
Has the advantages that:
the invention adopts a simple liquid phase synthesis method, the preparation process is simple, the titanium dioxide nanotube array can collect quantum dots and enhance the scattering effect of light, the prepared perovskite/titanium dioxide composite nanocrystal successfully excites two-photon random laser, and a lower laser threshold value and a better quality factor are measured at room temperature. The random laser of the perovskite/titanium dioxide composite nano-crystal is successfully realized without an additional resonant cavity, and a new possibility is provided for frequency rising conversion.
Drawings
FIG. 1 shows CsPbBr provided in example 1 of the present invention 3 /TiO 2 Schematic diagram of the preparation process of the composite nanocrystal.
FIG. 2 shows CsPbBr provided in embodiment 1 of the present invention 3 /TiO 2 Scanning electron microscope pictures of composite nanocrystals.
FIG. 3 shows CsPbBr provided in embodiment 1 of the present invention 3 /TiO 2 X-ray diffraction patterns of the composite nanocrystals.
FIG. 4 shows CsPbBr provided in embodiment 1 of the present invention 3 /TiO 2 Scanning electron microscope pictures and energy dispersion spectra of the composite nanocrystals.
FIG. 5 shows CsPbBr provided in embodiment 1 of the present invention 3 /TiO 2 Fluorescence (PL), absorption (Abs), and fluorescence lifetime (lifetime) profiles of the composite nanocrystals.
FIG. 6 shows CsPbBr provided in embodiment 1 of the present invention 3 /TiO 2 A spontaneous amplified emission (ASE) spectrum of the composite nanocrystal.
FIG. 7 shows CsPbBr provided in embodiment 1 of the present invention 3 /TiO 2 Laser test (sizing) patterns of composite nanocrystals.
Detailed Description
The embodiments herein and the various features and relevant details of the embodiments described below in connection with the specific examples are explained more fully with reference to the non-limiting embodiments that are illustrated in the accompanying drawings and detailed in the following description. Descriptions of well-known components and processing techniques are omitted so as to not unnecessarily obscure the embodiments herein. Conventional processes well known in the semiconductor art may be used in fabricating the structure. The examples used herein are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples herein should not be construed as limiting the scope of the embodiments herein.
Example 1 provides aCsPbBr 3 /TiO 2 The preparation method of the composite nanocrystal comprises the following steps:
(1) To a concentration of 25mg/L Cs 2 CO 3 Adding 0.6ml of oleic acid into the octadecylene solution, heating for one hour at 120 ℃ under the atmosphere of nitrogen, and obtaining Cs 2 CO 3 And (3) completely reacting with oleic acid to obtain a cesium oleate precursor solution, wherein the mass volume ratio of cesium carbonate to oleic acid is 100mg:0.6ml;
(2) 69mg of PbBr 2 Adding into 5ml octadecene solution, heating to 120 deg.C under nitrogen, maintaining for one hour, heating to 150 deg.C, and injecting 0.5ml oleic acid and 0.5ml oleylamine to PbBr 2 Completely dissolving, then injecting 0.4mL of a precursor of cesium oleate, and quickly reacting for 10s under the nitrogen condition;
(3) Taking out the reaction solution, carrying out ice bath to completely stop the reaction to obtain CsPbBr 3 A quantum dot solution;
(4) Centrifuging and purifying with toluene, collecting supernatant after three times of centrifuging and purifying to obtain CsPbBr 3 Toluene solution.
(5) 2ml of CsPbBr was taken 3 Toluene solution, 5mg TiO 2 Subjecting the nanotube to ultrasonic oscillation for 0.5h to obtain CsPbBr 3 /TiO 2 A composite nanocrystal.
As shown in FIG. 1, is CsPbBr 3 /TiO 2 The preparation process of the composite nanocrystal is schematically shown in FIG. 1 (a), which shows TiO 2 Schematic of nanotube arrays, FIG. 1 (b-c) CsPbBr 3 /TiO 2 The preparation process of the nano material is shown schematically; FIG. 1 (d) is a CsPbBr-filled cell 3 TiO of quantum dot 2 A schematic diagram of nanotubes; FIG. 1 (e) shows CsPbBr 3 /TiO 2 Optical pictures of toluene solution. FIG. 2 (a) shows CsPbBr with a resolution of 100nm as shown in the scanning electron microscope of FIG. 2 3 Quantum dot/TiO 2 Scanning electron microscope pictures of nanotube composite crystals, FIG. 2 (b) is CsPbBr filled 3 Of a single TiO compound 2 High resolution transmission electron microscopy images of nanotubes with a resolution of 200nm. Scanning electron microscopy and high resolution transmission electron microscopy accurately demonstrate CsPbBr 3 The quantum dots are uniformly dispersed in TiO 2 In the nanotubes. FIG. 3 shows CsPbBr 3 /TiO 2 X-ray diffraction patterns of the composite nanocrystals. FIG. 4 shows CsPbBr 3 /TiO 2 Scanning electron microscope pictures and energy dispersion spectra of the composite nanocrystals. FIG. 5 shows CsPbBr 3 /TiO 2 Fluorescence (PL), absorption (Abs), and fluorescence lifetime (lifetime) profiles of the composite nanocrystals. FIG. 6 shows CsPbBr 3 /TiO 2 A spontaneous amplified emission (ASE) spectrum of the composite nanocrystal. FIG. 7 shows CsPbBr 3 /TiO 2 Laser test (sizing) patterns of composite nanocrystals. Due to TiO 2 The nano tube has a function of collecting light to a certain extent, photons of a laser light source are subjected to continuous random scattering among quantum dots in the nano tube, and a part of the photons returns to an original light path incident point, so that a closed loop is formed, and when the optical gain is larger than the loss, laser oscillation occurs at the resonant frequency of a corresponding feedback circuit. By adjusting the pumping energy to be 5.34mJ/cm 2 Slowly increases to 18.05mJ/cm 2 The emission intensities at different excitation energies are shown in fig. 7. When the energy of the pump light is low, the material fluoresces at 532nm, and the half-peak width is about 17nm. The increase of the light energy density of the pump also brings about the increase of the luminous intensity, and the luminous peak becomes narrower. Once the energy density reaches a fixed value, a spike begins to appear around 537 nm. Again, the intensity of these peaks increases with increasing pump source energy, and these luminescence peaks are called CsPbBr 3 /TiO 2 A laser peak of stimulated emission.
The composite nanocrystal prepared by the embodiment shows a quite low two-photon excitation pumping laser threshold value of 9.54mJ/cm 2 The half-peak width of the laser emission was 0.49nm, and the quality factor was 1084. These interesting findings indicate that such low cost perovskite-based stochastic laser devices can be achieved by simple methods.
Example 2 provides another CsPbCl 3 /TiO 2 The preparation method of the composite nanocrystal comprises the following steps:
(1) To a concentration of 25mg/L Cs 2 CO 3 Adding 1.0ml of oleic acid into the octadecene solution, and heating the mixture for a small time at 120 ℃ in a nitrogen atmosphereWhile, cs 2 CO 3 And (3) completely reacting with oleic acid to obtain a cesium oleate precursor solution, wherein the mass volume ratio of cesium carbonate to oleic acid is 100mg:0.6ml;
(2) 40mg of PbCl was added 2 Adding into 5ml octadecene solution, heating to 110 deg.C under nitrogen, maintaining for 30min, heating to 160 deg.C, and adding 0.5ml oleic acid and 1ml oleylamine to PbCl 2 Completely dissolving, then injecting 0.6mL of precursor solution of cesium oleate, and quickly reacting for 10s under the nitrogen condition;
(3) Taking out the reaction solution, and carrying out ice bath to completely stop the reaction to obtain CsPbCl 3 A quantum dot solution;
(4) Centrifuging and purifying with toluene, collecting supernatant after three times of centrifuging and purifying to obtain CsPbCl 3 Toluene solution.
(5) 2ml of CsPbCl was taken 3 Toluene solution, 4mg TiO 2 Subjecting the nanotube to ultrasonic oscillation for 50min to obtain CsPbCl 3 /TiO 2 A composite nanocrystal.
The preparation method is simple and environment-friendly, and the obtained red perovskite quantum dots can be applied to photoelectric devices such as light emitting diodes, photoelectric detectors, lasers, solar cells and the like.
It should be noted that the drawings provided in this embodiment are only for schematically illustrating the basic idea of the present invention, and the drawings only show the components related to the present invention rather than being drawn according to the number, shape and size of the components in actual implementation, and the type, quantity and proportion of each component in actual implementation may be arbitrarily changed, and the layout of the components may be more complicated.
The foregoing is a further description of the invention with reference to preferred embodiments, and the examples described are some, but not all, examples of the invention. It will be apparent to those skilled in the art that various modifications, additions, substitutions, and other embodiments can be made without departing from the spirit and scope of the invention.

Claims (10)

1. A preparation method of perovskite/titanium dioxide composite nanocrystals is characterized by comprising the following steps:
1) Mixing cesium carbonate, octadecene solution and oleic acid, and reacting to obtain cesium oleate precursor solution;
2) Mixing lead halide, octadecene solution, oleic acid and oleylamine, and quickly reacting the obtained mixed solution with the cesium oleate precursor solution to obtain a perovskite quantum dot solution;
3) Purifying the perovskite quantum dot solution by using toluene to obtain a perovskite toluene solution;
4) Mixing the perovskite toluene solution with a titanium dioxide nanotube to obtain a perovskite/titanium dioxide composite nanocrystal;
in step 4), the TiO is 2 The mass concentration of the nano tube in the perovskite toluene solution is 2-3mg/mL;
in the step 4), the perovskite toluene solution and the titanium dioxide nano tube are mixed and then subjected to ultrasonic oscillation for 0.5-1h.
2. The method for preparing perovskite/titanium dioxide composite nanocrystals according to claim 1, wherein in step 1), the mass-to-volume ratio of cesium carbonate to oleic acid is 50-150mg:0.6ml; the mass concentration of the cesium carbonate in the oleic acid and octadecene solution is 20-30mg/L.
3. A process for preparing the perovskite/titania composite nanocrystal according to claim 1, wherein in step 1), the reaction is carried out under a protective gas condition; the reaction temperature is 100-150 ℃, and the reaction time is 40-90min.
4. The method for preparing the perovskite/titanium dioxide nanocomposite nanocrystal as claimed in claim 1, wherein in the step 2), the mass concentration of the lead halide in the octadecene solution is 1-15mg/ml; the volume ratio of the oleic acid to the oleylamine is 1-2; the volume percentage of the oleic acid in the octadecene is 5-15%; the volume percentage content of the potassium oleate precursor solution in the octadecene is 8-12%.
5. The method for preparing the perovskite/titanium dioxide composite nanocrystal according to claim 1, wherein in the step 2), the lead halide, the octadecene solution, the oleic acid and the oleylamine are mixed specifically as follows:
under the condition of protective gas, lead halide and octadecene are mixed, heated and kept warm, then heated to 150-170 ℃, and oleic acid and oleylamine are added.
6. The method for preparing the perovskite/titanium dioxide composite nanocrystal as claimed in claim 5, wherein the temperature is kept at 110-130 ℃ for 30-60min.
7. The process for preparing perovskite/titania composite nanocrystals according to claim 1, wherein in step 2), the reaction is carried out under a protective gas; the reaction temperature is 150-170 ℃, and the rapid reaction time is 5-15s.
8. The method for preparing the perovskite/titanium dioxide composite nanocrystal as claimed in claim 1, wherein the step 2) comprises an ice bath after the rapid reaction.
9. A perovskite/titania composite nanocrystal obtained by the production method as claimed in any one of claims 1 to 8.
10. Use of the perovskite/titania composite nanocrystal of claim 9 in the preparation of a solar cell, a light emitting diode or a laser.
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CN108193253A (en) * 2018-01-19 2018-06-22 河南工业大学 A kind of full-inorganic perovskite Nanocomposites H-TiO2Based nanotube array and its preparation method and application
CN108774511A (en) * 2018-05-31 2018-11-09 兰州大学 The preparation of full-inorganic perovskite quantum dot/mesoporous MOF-5 composite luminescent materials and application in the led

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CN108193253A (en) * 2018-01-19 2018-06-22 河南工业大学 A kind of full-inorganic perovskite Nanocomposites H-TiO2Based nanotube array and its preparation method and application
CN108774511A (en) * 2018-05-31 2018-11-09 兰州大学 The preparation of full-inorganic perovskite quantum dot/mesoporous MOF-5 composite luminescent materials and application in the led

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