CN112961675B - Method for improving stability of perovskite quantum dots through sol-gel passivation - Google Patents
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Abstract
The invention discloses a method for improving the stability of perovskite quantum dots by sol-gel passivation, which adopts a ligand-assisted redeposition technology and takes APTES and oleic acid as ligands to prepare heterogeneous all-inorganic perovskite quantum dots; then TEOS is added to wrap a layer of silicon dioxide on the surface of the quantum dot to prepare SiO 2 @CsPbX 3 Fluorescent powder; and introducing the all-inorganic perovskite quantum dots into the silica gel matrix by using TEOS as a precursor and ethanol as a solvent through a sol-gel wet chemical process, and doping perovskite into the silica gel matrix, thereby preparing the perovskite quantum dots with high stability. The APTES serving as a ligand can effectively control the particle size of the perovskite quantum dots and passivate the surfaces of the quantum dots, and siloxane on the APTES can be gradually hydrolyzed along with the stirring of the solution to generate a layer of silicon dioxide on the surfaces of the quantum dots, so that the purposes of blocking water and oxygen in the air and protecting the quantum dots are achieved.
Description
Technical Field
The invention belongs to the technical field of perovskite quantum dots, and particularly relates to a method for improving the stability of perovskite quantum dots through sol-gel passivation.
Background
The semiconductor quantum dots have excellent photoelectric properties such as high fluorescence quantum efficiency, narrow light-emitting peak, adjustable emission spectrum and the like, and are widely applied to the fields of light-emitting diodes, biological imaging, photodetectors and the like. In recent years, perovskite quantum dots, an emerging quantum dot material, have attracted extensive attention. Besides the advantages, the perovskite quantum dot has the advantages of better photoelectric transmission performance, larger emission spectrum adjustment range, wider color gamut, simple synthesis method, low cost, room-temperature synthesis and the like, so that the perovskite quantum dot has a very good application prospect in the field of novel photoelectric devices.
The application of perovskite quantum dots is severely limited by its stability. The perovskite quantum dot is a typical ionic crystal and has a huge specific surface area, which causes that the perovskite quantum dot is very sensitive to environmental changes, such as oxygen and water vapor in air, high temperature and other factors can cause that the structure of the perovskite quantum dot is damaged, and further the luminescence of the perovskite quantum dot is severely quenched. In addition, perovskite quantum dots have an "anion exchange effect" in that when perovskite solutions containing different halogen anions are mixed, the anions are rapidly exchanged (within seconds or even immediately) and evenly distributed in all quantum dots. The energy level structure of the perovskite can be directly regulated and controlled by the anion formed by the perovskite, so that the perovskite originally having different emission spectra after anion exchange is averaged to be only provided with one luminescence peak, which limits the application of the perovskite in the aspects of multicolor display and illumination. In summary, improving the stability of perovskite quantum dots is particularly important for their wide application.
Silica is an inorganic substance having excellent optical properties, and is very useful for photoelectric devices due to its long-term chemical and physical stability. Therefore, many researchers can improve the stability of the perovskite quantum dots by adopting a silica-coated method, for example, zhang et al synthesizes the all-inorganic perovskite quantum dots coated with silica by adopting APTES as a ligand, and the all-inorganic perovskite quantum dots have good stability in the air. They also adopt a mode of combining a silicon dioxide substrate with a polymer to synthesize flexible all-inorganic perovskite quantum dot/silicon dioxide soft gel in situ. The prepared gel can ensure that the perovskite quantum dots can be uniformly distributed in the gel, has high transparency, and has good stability to water and polar solvents. Huang et al use silica spheres to coat organic-inorganic hybrid perovskite quantum dots to better improve the stability of the quantum dots compared to uncoated quantum dots.
Disclosure of Invention
The invention aims to provide a method for improving the stability of a perovskite quantum dot by sol-gel passivation, which adopts a ligand assisted redeposition technology and takes APTES and oleic acid as ligands to prepare different types of all-inorganic perovskite quantum dots; then TEOS is added to coat a layer of silicon dioxide on the surface of the quantum dot to prepare SiO 2 @CsPbX 3 A fluorescent powder; and then, taking ethyl orthosilicate as a precursor and ethanol as a solvent, introducing the all-inorganic perovskite quantum dots into the silica gel matrix by adopting a sol-gel wet chemical process, and doping perovskite into the silica gel matrix, thereby preparing the composite gel glass doped with the stable perovskite quantum dot material.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method of improving the stability of perovskite quantum dots by sol-gel passivation, the method comprising the steps of:
(1) Preparing a precursor solution: weighing CsX (X = Cl, br, I) and PbX in certain ratio 2 Dissolving in N, N-Dimethylformamide (DMF), stirring uniformly to prepare a precursor, then adding ligand APTES and oleic acid into the precursor, and performing ultrasonic oscillation to obtain a clear and transparent precursor solution;
(2)SiO 2 @CsPbX 3 preparation of colloidal solution: under the condition of violent stirring, taking the precursor solution, adding the precursor solution into a toluene solution, and adding a proper amount of TEOS to obtain SiO with different colors of fluorescence 2 @CsPbX 3 A colloidal solution;
(3)SiO 2 @CsPbX 3 preparing fluorescent powder: centrifuging the obtained product, discarding supernatant, retaining bottom precipitate, and vacuum drying to obtain SiO with different colors and fluorescence 2 @CsPbX 3 Fluorescent powder;
(4) Preparing perovskite doped composite gel glass: respectively measuring TEOS and ethanol in a certain proportion, placing in a clean beaker for ultrasonic oscillation, and then adding SiO 2 @CsPbX 3 Mixing fluorescent powder, adding GPTMS and APTES, and magnetically stirring for several hours. After the TEOS is fully hydrolyzed and condensed, pouring a proper amount of solution into a transparent plastic culture dish, standing for several days at room temperature, and obtaining the CsPbX without obvious weight loss of the sample 3 Doped composite gel glass.
Further, the mole ratio of tetraethyl orthosilicate to 3-glycidyltrimethoxysilane (3-aminopropyl) triethoxysilane in the step 4) is 7.
Further, step 3) centrifugation is carried out for 5 minutes at a rotating speed of 7000 r/min.
And (5) adding different amounts of fluorescent powder in the step (4) to obtain the composite gel glass with different doping concentrations.
CsPbX prepared by the above preparation method 3 The doped composite gel glass has good optical transparency, improves the stability of perovskite quantum dots, can improve the stability of the quantum dots by introducing the perovskite quantum dots into a silicon dioxide gel system, brings some new optical characteristics to the gel glass, and expands the application of the gel glass in the optical field.
Drawings
FIG. 1 is SiO 2 @CsPbBr 3 Picture of doped composite gel glass.
FIG. 2 is SiO 2 @CsPbBr 3 TEM image of colloidal solution;
FIG. 3 is SiO 2 @CsPbBr 3 XRD pattern of the composite gel glass;
FIG. 4 is SiO 2 @CsPbBr 3 PL plots for colloidal solutions, phosphors, and composite gel glasses.
Detailed Description
In order to facilitate an understanding of the present invention, the following examples are provided to further illustrate the present invention, but are not intended to limit the scope of the present invention.
Example 1
Weighing CsBr and PbBr 2 Dissolving in N, N-Dimethylformamide (DMF), stirring to obtain precursor, adding ligand APTES and oleic acid into the precursor, and ultrasonic oscillating to obtain clear and transparent precursor solution. Finally stirring vigorouslyAdding the precursor solution into toluene solution, and adding appropriate amount of TEOS to obtain green fluorescent SiO 2 @CsPbBr 3 A colloidal solution. Centrifuging the obtained product at 7000r/min for 5 min, discarding supernatant, retaining bottom precipitate, and vacuum drying to obtain green fluorescent SiO 2 @CsPbBr 3 And (4) fluorescent powder. Respectively measuring ethyl silicate and ethanol, placing the ethyl silicate and the ethanol in a clean beaker for ultrasonic oscillation, and then adding SiO 2 @CsPbBr 3 And (3) uniformly mixing the fluorescent powder, and finally, sequentially adding GPTMS and APTES and magnetically stirring for a plurality of hours, wherein the molar ratio of TEOS to GPTMS to APTES is 7. After the TEOS is fully hydrolyzed and condensed, pouring a proper amount of solution into a transparent plastic culture dish, standing for several days at room temperature, and obtaining CsPbBr without obvious weight loss of the sample 3 Doped composite gel glass.
Example 2
Weighed CsCl and PbCl 2 Dissolving in N, N-Dimethylformamide (DMF), stirring to obtain precursor, adding ligand APTES and oleic acid into the precursor, and ultrasonic oscillating to obtain clear and transparent precursor solution. Finally, under the condition of violent stirring, the precursor is added into a toluene solution, and a proper amount of TEOS is added to obtain SiO with blue fluorescence 2 @CsPbCl 3 A colloidal solution. Centrifuging the obtained product at 7000r/min for 5 min, discarding supernatant, retaining bottom precipitate, and vacuum drying to obtain blue fluorescent SiO 2 @CsPbCl 3 And (3) fluorescent powder. Respectively measuring ethyl silicate and ethanol, placing the ethyl silicate and the ethanol in a clean beaker for ultrasonic oscillation, and then adding SiO 2 @CsPbCl 3 And (3) uniformly mixing the fluorescent powder, and finally, sequentially adding GPTMS and APTES and magnetically stirring for a plurality of hours, wherein the molar ratio of TEOS to GPTMS to APTES is 7. After the TEOS is fully hydrolyzed and condensed, pouring a proper amount of solution into a transparent plastic culture dish, standing for several days at room temperature, and obtaining the CsPbCl without obvious weight loss of the sample 3 Doped composite gel glass.
Example 3
Weighed CsI and PbI 2 Dissolving in N, N-Dimethylformamide (DMF), stirring to obtain precursor, and adding ligand APTES and oleic acidAnd in the precursor, performing ultrasonic oscillation to obtain a clear and transparent precursor solution. Finally, under the condition of intense stirring, the precursor is added into toluene solution, and a proper amount of TEOS is added to obtain SiO with red fluorescence 2 @CsPbBr 3 A colloidal solution. Centrifuging the obtained product at 7000r/min for 5 min, discarding supernatant, retaining bottom precipitate, and vacuum drying to obtain red fluorescent SiO 2 @CsPbI 3 And (3) fluorescent powder. Respectively measuring ethyl silicate and ethanol, placing the ethyl silicate and the ethanol in a clean beaker for ultrasonic oscillation, and then adding SiO 2 @CsPbI 3 And (3) uniformly mixing the fluorescent powder, and finally, sequentially adding GPTMS and APTES and magnetically stirring for a plurality of hours, wherein the molar ratio of TEOS to GPTMS to APTES is 7. After the TEOS is fully hydrolyzed and condensed, pouring a proper amount of solution into a transparent plastic culture dish, standing for several days at room temperature, and obtaining the CsPbI without obvious weight loss of the sample 3 Doped composite gel glass.
And (3) performance characterization:
FIG. 1 is SiO 2 @CsPbBr 3 Picture of doped composite gel glass. The figure shows that the gel glass is relatively transparent and has no cracks completely, which indicates that the quantum dots are successfully doped into the gel glass.
FIG. 2 is SiO 2 @CsPbBr 3 TEM image of colloidal solution. As can be seen from the figure, the quantum dots are spherical and have good dispersibility, the average is about 4-5 nm, and the outer layer has amorphous SiO 2 And (5) network connection.
FIG. 3 is SiO 2 @CsPbBr 3 XRD pattern of composite gel glass. XRD analysis showed diffraction peaks at 15.2 °,21.6 °,26.5 °,30.6 °,34.4 °,37.8 °,43.9 °, and 46.7 °, corresponding to (100), (110), (111), (200), (210), (211), (220), and (300) crystal planes, and it can be seen that SiO was present 2 @CsPbBr 3 Quantum dots are cubic phase structures (PDF # 54-0752), similar to those described in other literature.
FIG. 4 is SiO 2 @CsPbBr 3 PL profiles of colloidal solution, phosphor and composite gel glass. The emission wavelengths of the three are all about 510 nm, and no obvious movement exists.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (3)
1. A method for improving the stability of perovskite quantum dots by sol-gel passivation is characterized by comprising the following steps:
1) Preparing a precursor solution: weighing CsX and PbX 2 Dissolving in N, N-dimethylformamide, and stirring to obtain precursor, wherein X is Cl, br or I; then adding (3-aminopropyl) triethoxysilane and oleic acid into the precursor, and performing ultrasonic oscillation to obtain precursor liquid;
2)SiO 2 @CsPbX 3 preparation of colloidal solution: adding the precursor solution into a toluene solution, continuously stirring, and adding tetraethyl orthosilicate to obtain SiO with color fluorescence 2 @CsPbX 3 A colloidal solution;
3)SiO 2 @CsPbX 3 preparing fluorescent powder: centrifuging the obtained product by a centrifugal machine, discarding supernatant, retaining bottom precipitate, and vacuum drying to obtain SiO 2 @CsPbX 3 Fluorescent powder;
4) Preparing perovskite doped composite gel glass: respectively measuring tetraethyl orthosilicate and ethanol, placing the tetraethyl orthosilicate and the ethanol in a clean beaker for ultrasonic oscillation, and then adding SiO 2 @CsPbX 3 Uniformly mixing fluorescent powder; then sequentially adding 3-glycidyltrimethoxysilane and (3-aminopropyl) triethoxysilane; pouring tetraethyl orthosilicate into a culture dish after sufficient hydrolysis and polycondensation, standing, and obtaining the composite gel glass containing stable perovskite quantum dots after no obvious weight loss, wherein the molar ratio of tetraethyl orthosilicate to 3-glycidyltrimethoxysilane (3-aminopropyl) triethoxysilane is 7.
2. The method of sol-gel passivation for improving the stability of perovskite quantum dots according to claim 1, wherein: and 3) centrifuging for 5 minutes at the rotating speed of 7000 r/min.
3. A composite gel glass containing stable perovskite quantum dots prepared by the method of any one of claims 1-2.
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CN107446572A (en) * | 2017-09-01 | 2017-12-08 | 中国科学院长春光学精密机械与物理研究所 | Synthetic silica coats the application of the method for organic inorganic calcium perovskite like structure quantum dot and its quantum dot of synthesis |
CN110790489A (en) * | 2019-11-28 | 2020-02-14 | 福建工程学院 | Preparation method of low-dimensional material doped non-hydrolytic gel glass |
CN110872510A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院大连化学物理研究所 | Red and green light perovskite quantum dot stable fluorescent powder based on silicon dioxide coating and preparation |
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CN106634961A (en) * | 2016-12-19 | 2017-05-10 | 中央民族大学 | Organic-inorganic hybrid perovskite quantum dot and preparation method thereof |
CN107446572A (en) * | 2017-09-01 | 2017-12-08 | 中国科学院长春光学精密机械与物理研究所 | Synthetic silica coats the application of the method for organic inorganic calcium perovskite like structure quantum dot and its quantum dot of synthesis |
CN110872510A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院大连化学物理研究所 | Red and green light perovskite quantum dot stable fluorescent powder based on silicon dioxide coating and preparation |
CN110790489A (en) * | 2019-11-28 | 2020-02-14 | 福建工程学院 | Preparation method of low-dimensional material doped non-hydrolytic gel glass |
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