CN110699067B - Silica-coated palladium-doped inorganic perovskite quantum dot and preparation method thereof - Google Patents

Silica-coated palladium-doped inorganic perovskite quantum dot and preparation method thereof Download PDF

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CN110699067B
CN110699067B CN201910993715.4A CN201910993715A CN110699067B CN 110699067 B CN110699067 B CN 110699067B CN 201910993715 A CN201910993715 A CN 201910993715A CN 110699067 B CN110699067 B CN 110699067B
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王向华
徐志梁
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Abstract

The invention discloses a palladium-doped inorganic perovskite quantum dot wrapped by silicon dioxide and a preparation method thereof, wherein the blue light quantum dot is CsPb x Pd 1‑x Br y Cl 3‑y @SiO 2 Quantum dots of CsPbBr 3 Quantum dot outer wrapping SiO 2 Layer formation of CsPbBr 3 @SiO 2 Quantum dot reaction with CsPdCl 3 Mixing the quantum dots and doping palladium ions to obtain the quantum dots. According to the palladium-doped inorganic perovskite quantum dot wrapped by silicon dioxide, through wrapping of the silicon dioxide and doping of palladium ions, CsPbBr is remarkably improved 3 The quantum dots have the fluorescence quantum efficiency in the blue light range, have stable performance and have wide application prospect in the fields of optoelectronic devices and solar cells.

Description

Silica-coated palladium-doped inorganic perovskite quantum dot and preparation method thereof
Technical Field
The invention relates to an inorganic perovskite quantum dot, and belongs to the field of novel nano material preparation.
Background
The all-inorganic perovskite quantum dot material is composed of inorganic nanocrystals, and is more stable compared with organic and inorganic hybrid perovskite materials. As a material in a nanocrystalline form, the material can also be prepared into a core-shell structure by using a colloid chemical method, so that the performance of the material is improved. The photoelectric conversion efficiency of the solar cell prepared by using the all-inorganic perovskite quantum dot material can exceed 10% [ references 1 and 2 ]]The fluorescence quantum efficiency of the all-inorganic perovskite green light quantum dot is close to 100%. The method shows that the all-inorganic perovskite quantum dot material has wide application prospect in the fields of solar cells, luminescent and display devices and the like. Wherein CsPbX 3 The (X ═ Cl, Br, I) quantum dots can be prepared by adopting a low-cost solution preparation process, and the forbidden band width of the quantum dots can cover the whole visible spectrum range based on chemical element replacement and quantum size effect.
However, CsPbX is currently available 3 (X ═ Cl, Br, I) quantum dotsThe problem of low fluorescence quantum efficiency in the blue range (PLQY) is prevalent. Such as CsPbCl 3 PLQY of perovskite blue light quantum dot is 5%, and CsPbCl is mostly adopted in the prior art 3 Br element is introduced into the nanocrystal to improve the PLQY of blue light, but the effect is still not ideal, and the PLQY is only 15% at about 460nm, so a method for further improving the fluorescence quantum efficiency of blue light quantum dots needs to be found.
The improvement of the fluorescence quantum efficiency of blue light quantum dots by doping metal elements, particularly transition metal elements, is an effective approach reported in recent years. In 2017, Menghong topic was assigned to CsPbBr 3 3-valent aluminum ions are introduced into the quantum dots to obtain blue light quantum dots with peak positions of 456nm, and PLQY reaches 42%. 2018, Sunzhong Tao group passed in CsPbCl 3 Positive 2-valent nickel ions are introduced into the quantum dots to obtain blue light quantum dots with peak positions of 410-. In 2019, the topic group of the field Jianjun passes CsPbBr x Cl 3-x 2-valent copper ions are introduced into the quantum dots to obtain blue light quantum dots with peak positions of 450-460nm, and PLQY reaches about 85%. Because the improvement of the performance of the quantum dot material benefits from the diffusion of anions and cations in the preparation process of the quantum dot, the performance of the device is difficult to avoid reduction caused by the diffusion of elements when the quantum dot material is applied to the device as an optical film. In addition, the diffusion process tends to cause the nanocrystals to grow, causing a significant red-shift in the spectrum.
Reference documents:
1.Xiang,W.C.and W.Tress"Review on Recent Progress of All-Inorganic Metal Halide Perovskites and Solar Cells."Advanced Materials:28.
2.Swarnkar,A.,et al.(2016)."Quantum dot-induced phase stabilization of alpha-CsPbI3 perovskite for high-efficiency photovoltaics."Science 354(6308):92-95.
disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a palladium-doped inorganic perovskite quantum dot wrapped by silicon dioxide and a preparation method thereof, aiming at fully obtaining the advantages brought by element doping and quantum confinement effect and simultaneously inhibiting the material performance degradation caused by the diffusion of anions and cations in the use process of the material.
In order to realize the purpose, the invention adopts the following technical scheme:
the invention discloses a palladium-doped inorganic perovskite quantum dot wrapped by silicon dioxide, which is characterized in that: the quantum dots are CsPb x Pd 1-x Br y Cl 3-y @SiO 2 Quantum dots of Cs 4 PbBr 6 Quantum dot outer wrapping SiO 2 Layer formation of CsPbBr 3 @SiO 2 Quantum dot, and CsPdCl 3 Mixing the quantum dots and doping palladium ions to obtain the quantum dots.
Further, the CsPb x Pd 1-x Br y Cl 3-y @SiO 2 The quantum dots are blue light quantum dots, and CsPbBr is regulated and controlled 3 @SiO 2 Quantum dots and CsPdCl 3 The mixing ratio of the quantum dots, namely the value of x is regulated to regulate the emission peak of the blue quantum dots.
Further, x is more than or equal to 0.05 and less than or equal to 0.5.
The invention also discloses a preparation method of the palladium-doped inorganic perovskite quantum dot wrapped by the silicon dioxide, which comprises the following steps: first, Cs is synthesized by a thermal injection method 4 PbBr 6 And CsPdCl 3 Quantum dots; then on Cs 4 PbBr 6 Outer wrapping SiO 2 Layer, CsPbBr is obtained 3 @SiO 2 Quantum dots; finally, CsPbBr is added 3 @SiO 2 Quantum dots and CsPdCl 3 Mixing the quantum dots to obtain the silica-coated palladium-doped inorganic perovskite quantum dot CsPb x Pd 1-x Br y Cl 3-y @SiO 2 。
Compared with the prior art, the invention has the beneficial effects that:
1. the palladium-doped inorganic perovskite quantum dots wrapped by the silicon dioxide further improve the effectiveness of palladium ion doping by wrapping the silicon dioxide: in the blue light wave band with the wavelength less than 480nm, the PLQY still exceeds 80 percent, and the color saturation and the energy efficiency can be simultaneously improved when the PLQY is applied to a display.
2. The silicon dioxide wrapping layer can effectively inhibit the growth of the quantum dots, improve the chemical stability of the quantum dots and enhance the quantum confinement effect.
3. The preparation method of the quantum dot is simple, and relatively stable Cs is utilized 4 PbBr 6 The intermediate avoids the destructive effect of polar molecules on the luminescent nanocrystal in the preparation process, and has good repeatability.
Drawings
FIG. 1 shows CsPbBr in different mixing ratios obtained in the example of the present invention y Cl 3-y The fluorescence quantum efficiency of the quantum dots is shown in the figure, and the excitation wavelength is 365 nm.
FIG. 2 shows CsPbBr in different mixing ratios obtained in the embodiment of the present invention y Cl 3-y @SiO 2 The fluorescence quantum efficiency of the quantum dots is 365 nm.
FIG. 3 shows CsPb in different mixing ratios obtained in the example of the present invention x Pd 1-x Br y Cl 3-y The fluorescence quantum efficiency of the quantum dots is 365 nm.
FIG. 4 shows CsPb in different mixing ratios obtained in the example of the present invention x Pd 1-x Br y Cl 3-y @SiO 2 The fluorescence quantum efficiency of the quantum dots is 365 nm.
Detailed Description
The following examples are given for the detailed implementation and the specific operation based on the technical solution of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
This example prepares CsPb as follows x Pd 1-x Br y Cl 3-y @SiO 2 Quantum dot:
(1) preparation of the precursor
0.319g of Cs 2 CO 3 Adding into 15mL ODE solution, adding 1.5mL oleic acid, introducing nitrogen, heating and stirring at 150 deg.C until Cs 2 CO 3 Completely dissolving to obtain precursor solution, and heating at 100 deg.C before use.
(2)CsPbBr 3 @SiO 2 The preparation of (1):
0.1468g of PbBr 2 Adding into 20mL ODE solution, vacuum drying at 100 deg.C for 20min, adding 2mL oleic acid and 2mL oleylamine, stirring to PbBr 2 Completely dissolving; heating to 140 deg.C, rapidly injecting 4.2mL of precursor solution, reacting for 10s, rapidly cooling in ice water bath for 1min, centrifuging at 8000rpm for 5min, removing supernatant, adding 5mL of n-heptane into the residual precipitate, centrifuging at 5000rpm for 3min to obtain supernatant as Cs 4 PbBr 6 A solution;
in 5mL of Cs 4 PbBr 6 Adding TMOS (tetramethoxysilane) 20 μ L and deionized water 200 μ L into the solution, shaking at 2800rpm for 5min, standing for 12h, centrifuging at 5000rpm for 3min to obtain supernatant CsPbBr 3 @SiO 2 A quantum dot solution;
(3)CsPdCl 3 preparing quantum dots: 0.08g of PdCl 2 Adding into 20mL of ODE solution, drying at 120 ℃ for 1h in vacuum, adding 2mL of oleic acid and 2mL of oleylamine, and stirring until PdCl 2 Completely dissolving; then heating to 140 ℃, quickly injecting 2mL of precursor solution, reacting for 5s, quickly cooling in ice-water bath for 1min, centrifuging at 8000rpm for 5min, removing supernatant, adding 5mL of n-heptane into the residual precipitate, centrifuging at 5000rpm for 3min, and obtaining supernatant which is CsPdCl 3 A quantum dot solution.
(4) Mixing
Reacting CsPbBr 3 @SiO 2 Quantum dot solution and CsPdCl 3 Mixing the quantum dot solution according to the required proportion, shaking uniformly, standing for 1min to obtain the palladium-doped inorganic perovskite quantum dot (CsPb) wrapped by silicon dioxide x Pd 1-x Br y Cl 3-y @SiO 2 ) The solution of (1). By regulating and controlling the mixing ratio, namely regulating and controlling the value of x, the blue light quantum dots with different emission peaks can be obtained. This example CsPbBr @ SiO 2 And CsPdCl 3 The mixing volume ratio of (1) to (4) is 1:4, 1:1.4, 1:1, 1:0.8, 1:0.6 and 1:0.5 respectively.
For comparison, this example also prepared the following quantum dot solutions:
CsPbBr 3 quantumPreparing dots: 0.2g of PbBr 2 Adding into 20mL ODE solution, vacuum drying at 120 deg.C for 1h, adding 2mL oleic acid and 2mL oleylamine, stirring to PbBr 2 Completely dissolving; heating to 165 deg.C, rapidly injecting 2mL of precursor solution, reacting for 5s, rapidly cooling in ice water bath for 1min, centrifuging at 8000rpm for 5min, removing supernatant, adding 5mL of n-heptane into the rest precipitate, centrifuging at 5000rpm for 3min to obtain supernatant CsPbBr 3 A quantum dot solution.
CsPbCl 3 Preparing the quantum dots: 0.14g of PbCl was added 2 Adding into 20mL ODE solution, vacuum drying at 120 deg.C for 1h, adding 2mL oleic acid and 2mL oleylamine, and stirring to PbCl 2 Completely dissolving; heating to 140 deg.C, rapidly injecting 2mL of precursor solution, reacting for 5s, rapidly cooling in ice water bath for 1min, centrifuging at 8000rpm for 5min, removing supernatant, adding 5mL of n-heptane into the rest precipitate, centrifuging at 5000rpm for 3min to obtain supernatant CsPbCl 3 A quantum dot solution.
Mixing CsPbBr 3 Quantum dot solution and CsPbCl 3 Mixing the quantum dot solutions according to different proportions, shaking uniformly, and standing for 1min to obtain CsPbBr y Cl 3-y A solution of quantum dots. This example CsPbBr 3 Quantum dot solution and CsPbCl 3 The volume ratio of the quantum dot solution is 1:0.8, 1:0.7, 1:0.6, 1:0.5 and 1:0.3 respectively.
Reacting CsPbBr 3 @SiO 2 Quantum dot solution and CsPbCl 3 Mixing the quantum dot solution according to different proportions, shaking uniformly, standing for 1min to obtain CsPbBr y Cl 3-y @SiO 2 A solution of quantum dots. This example CsPbBr 3 @SiO 2 Quantum dot solution and CsPbCl 3 The volume ratio of the quantum dot solution is 1:0.6, 1:0.5 and 1:0.4 respectively.
Mixing CsPbBr 3 Quantum dot solution and CsPdCl 3 Mixing the quantum dot solution according to different proportions, shaking uniformly, and standing for 1min to obtain CsPb x Pd 1-x Br y Cl 3-y A solution of quantum dots. This example CsPbBr 3 Quantum dot solution and CsPdCl 3 The mixture volume ratio of the quantum dots is 1:4,1:3、1:2、1:0.8、1:0.6、1:1.55、1:0.5、1:0.3。
FIGS. 1,2, 3 and 4 show CsPbBr in different mixing ratios y Cl 3-y Quantum dots, CsPbBr y Cl 3-y @SiO 2 、CsPb x Pd 1-x Br y Cl 3-y Quantum dot, CsPb x Pd 1-x Br y Cl 3-y @SiO 2 The excitation wavelength of the fluorescence quantum efficiency graph of the quantum dots is 365 nm. From the figure, it can be seen that the fluorescence quantum efficiency of the palladium-doped blue quantum dots coated by the silicon dioxide is remarkably improved compared with that of other quantum dots.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Claims (3)

1. A palladium-doped inorganic perovskite quantum dot wrapped by silicon dioxide is characterized in that: the quantum dots are CsPb x Pd 1-x Br y Cl 3-y @SiO 2 Quantum dots, x is more than or equal to 0.05 and less than or equal to 0.5, and is in Cs 4 PbBr 6 Quantum dot outer wrapping SiO 2 Layer formation of CsPbBr 3 @SiO 2 Quantum dot, and CsPdCl 3 Mixing the quantum dots and carrying out palladium ion doping to obtain the quantum dot.
2. The silica-coated palladium-doped inorganic perovskite quantum dot of claim 1, wherein: the CsPb x Pd 1-x Br y Cl 3-y @SiO 2 The quantum dots are blue light quantum dots, and CsPbBr is regulated and controlled 3 @SiO 2 Quantum dots and CsPdCl 3 The mixing ratio of the quantum dots, namely the value of x is regulated to regulate the emission peak of the blue quantum dots.
3. A preparation method of the silica-coated palladium-doped inorganic perovskite quantum dot as claimed in any one of claims 1 to 2, which is characterized by comprising the following steps: first by hot injectionSynthetic Cs 4 PbBr 6 And CsPdCl 3 Quantum dots; then in Cs 4 PbBr 6 Wrapping SiO outside 2 Layer, CsPbBr is obtained 3 @SiO 2 Quantum dots; finally, CsPbBr is added 3 @SiO 2 Quantum dots and CsPdCl 3 Mixing the quantum dots to obtain the silica-coated palladium-doped inorganic perovskite quantum dot CsPb x Pd 1-x Br y Cl 3-y @SiO 2 。
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