CN111892518A - Short-chain inorganic acid ester passivation material and application thereof - Google Patents
Short-chain inorganic acid ester passivation material and application thereof Download PDFInfo
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- CN111892518A CN111892518A CN202010528514.XA CN202010528514A CN111892518A CN 111892518 A CN111892518 A CN 111892518A CN 202010528514 A CN202010528514 A CN 202010528514A CN 111892518 A CN111892518 A CN 111892518A
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Abstract
The invention provides a short-chain inorganic acid ester passivation material, which comprises an extremely short alkyl chain segment, wherein the alkyl chain segment comprises a special functional group A and a functional group B, the functional group A is at least one of sulfate, bisulfate, sulfite, bisulfite, nitrite, nitrate, sulfonate, phosphate and hydrogen phosphate, and the functional group B is an amino group. The short-chain inorganic acid ester provided by the invention interacts with defects and has a good passivation effect on the surface of the perovskite quantum dot.
Description
Technical Field
The invention relates to a short-chain inorganic acid ester passivation material and application of the material to passivation of perovskite quantum dots, and belongs to the technical field of photoelectric materials and devices.
Background
Perovskite materials are a class having ABX3The A site of the organic/inorganic metal halide perovskite is usually cesium (Cs)+) Methylamine (CH)3NH3 +,MA+) Formamidine (CH (NH)2)+,FA+) Isovalent cation, B is Pb2+、Sn2+、Cu2+Divalent cations, X being a halogen anion such as Cl－、Br－、I－And the like. The B site and X site ions are coordinated to form an octahedron structure, the octahedron structures form a basic framework of the perovskite in a form of common vertex, and A site cations are filled in the middle positions of the octahedron structure to maintain the structure stability and the charge balance. When the perovskite size is reduced to at or below its exciton bohr radius, strong quantum confinement effects occur and are therefore referred to as perovskite quantum dots.
The smaller the size of the quantum dot is, the ratio of the surface area to the volume is increased, and ions on the surface of the perovskite fall off to generate lead ions which are not fully coordinated to form charged defects, so that the material is further degraded and the photoelectric performance is reduced. The passivation of these surface lead ions by using some materials with special properties is one of the important means for improving the photoelectric properties of perovskite quantum dots. The naked lead ions are combined with the passivation material, so that non-radiative recombination generated by excitons induced by the lead ions is avoided, and the photoelectric property of the quantum dots can be effectively improved. In recent years, a lot of work has been reported on reducing surface defects of different passivation materials, such as quaternary ammonium bromide, organic-inorganic hybrid ion pairs, organic polymers and the like, and effectively improving the performance of perovskite photoelectric devices.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects existing on the surface of the perovskite in the prior art and providing a short-chain inorganic acid ester passivation material and application thereof.
The invention provides a short-chain inorganic acid ester passivation material, which comprises an extremely short alkyl chain segment, wherein the alkyl chain segment comprises a special functional group A and a functional group B, the functional group A is at least one of sulfate, bisulfate, sulfite, bisulfite, nitrite, nitrate, sulfonate, phosphate and hydrogen phosphate, and the functional group B is amino.
The amphoteric short carbon chain compound provided by the invention can reduce the defect state density through the interaction of the electronegative functional group A and the lead ions which are not fully coordinated in the perovskite quantum dots; the functional group B can be protonated into positively charged ammonium cations to fill the perovskite surface cation vacancies. The material has obvious promotion effect on the fluorescence intensity and the service life of the perovskite quantum dots. The perovskite quantum dot prepared from the short-chain inorganic acid ester passivation material has good application prospect in the fields of light-emitting diodes, solar cells, photoelectric detectors, thin film transistors, lasers and the like.
As a further technical scheme of the invention, the structural general formula of the short-chain inorganic acid ester passivation material is shown as follows:
wherein R is (CH)2)nN is more than or equal to 1 and less than or equal to 6, n is an integer, and X is at least one of sulfate ester group, bisulfate ester group, sulfite ester group, bisulfite ester group, nitrite ester group, nitrate ester group, sulfonate ester group, phosphate ester group and hydrogen phosphate ester group.
The invention also provides an application of the short-chain inorganic acid ester passivation material, and the short-chain inorganic acid ester passivation material passivates perovskite quantum dots.
According to the application of the short-chain inorganic acid ester passivation material provided by the invention, the short-chain inorganic acid ester passivation material is directly added into a perovskite precursor solution to be used as an additive for passivating defects.
The short-chain inorganic acid ester passivation material is directly added into the perovskite quantum dots to be used as a post-treatment additive, can be effectively attached to the surfaces of the perovskite quantum dots and passivate defects, obtains the perovskite quantum dots with high fluorescence intensity and good stability, and has good application prospect in the field of perovskite photoelectric devices.
The invention further provides perovskite quantum dots based on short-chain inorganic acid ester passivation materials, wherein the perovskite quantum dots comprise all-inorganic perovskite quantum dots and organic-inorganic hybrid perovskite quantum dots.
The invention further provides a mode for passivating the perovskite quantum dots by using the short-chain inorganic acid ester passivating material, which specifically comprises the following steps:
s1, dissolving short-chain inorganic acid ester passivation material, metal source halide and organic/inorganic source halide in a polar solvent according to different stoichiometric ratios, and uniformly stirring to prepare perovskite quantum dot precursor solution;
s2, dripping the perovskite quantum dot precursor solution prepared in the step S1 into toluene, and then centrifuging, and taking supernatant, namely the perovskite quantum dot after the material is passivated.
The metal source halide is at least one of lead halide and stannous halide; the organic/inorganic source halide is at least one of cesium halide, formamidine hydrohalide and methylamine hydrohalide.
The perovskite quantum dots can be applied to light emitting diodes, solar cells, photodetectors, thin film transistors and lasers.
The polar solvent is DMF. The molar ratio of the metal source halide to the organic/inorganic source halide is 1:1, the addition amount of the short-chain inorganic acid ester passivation material is x mg/mL, wherein x is more than or equal to 0 and less than or equal to 1.
Compared with the prior art, the invention adopting the technical scheme has the following technical effects:
(1) the amphoteric short alkyl chain passivation material provided by the invention can passivate quantum dot defects, is combined with free metal ions to reduce quenching of excitons, and improves the fluorescence intensity, fluorescence life and stability of quantum dots;
(2) the perovskite quantum dot passivated by the short-chain inorganic acid ester has the advantages of simple synthesis process, stable quantum dot product and commercial feasibility;
(3) the short-chain inorganic acid ester passivated perovskite quantum dot provided by the invention has higher performance and stability in specific application, and shows the application potential of the short-chain inorganic acid ester in improving the performance of photoelectric devices through perovskite defect passivation.
In conclusion, the short-chain inorganic acid ester provided by the invention interacts with defects and has a good passivation effect on the surface of the perovskite quantum dot.
Drawings
The invention is further described below with reference to the figures and examples.
FIG. 1 shows FA0.8Cs0.2PbBr3Quantum dots and 2-aminoethanol hydrogen sulfate (2-AEHS) passivated FA0.8Cs0.2PbBr3Fluorescence emission spectra of quantum dots.
FIG. 2 shows FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3Transient fluorescence spectra of quantum dots.
FIG. 3 is FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3XRD pattern of quantum dots.
FIG. 4 shows FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3TEM and HRTEM images of quantum dots.
FIG. 5 shows FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3Quantum dot light emitting diode device architecture diagram.
FIG. 6 shows FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3Efficiency-voltage curve of quantum dots.
FIG. 7 shows FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3And the brightness change curve chart of the light emitting diode of the quantum dot under the condition of continuous lighting.
Detailed Description
The technical scheme of the invention is further explained in detail by combining the attached drawings: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection authority of the present invention is not limited to the following embodiments. In the examples, 2-AEHS is used to passivate perovskite quantum dots, and the specific structure is as follows:
example 1
When the amount of 2-aminoethanol hydrogen sulfate (2-AEHS) added was 0mg/mL, FA was added0.8Cs0.2PbBr3The preparation method of the quantum dot comprises the following steps:
(1) weighing 73.4mg of lead bromide and 39.9mg of formamidine bromide, dissolving the lead bromide and formamidine bromide in 2mL of N, N-Dimethylformamide (DMF), adding 90 mu L of oleic acid and 15 mu L of octylamine, stirring at 50 ℃ for 30min, dissolving to obtain a precursor solution A, and cooling for later use; weighing 17.0mg of cesium bromide and 73.4mg of lead bromide, dissolving in 2mL of N, N-Dimethylformamide (DMF), adding 90. mu.L of oleic acid and 15. mu.L of octylamine, stirring at 70 ℃ for 30min, dissolving to obtain a precursor solution B, and cooling for later use.
(2) And mixing the precursor solution A and the precursor solution B, and stirring for 30min at 50 ℃ to obtain the required perovskite precursor solution. And (3) quickly injecting 250 mu L of perovskite precursor solution into 10mL of toluene which is stirred vigorously, centrifuging the solution at the rotating speed of 5000rpm for 10min after the injection is finished, and storing the supernatant as a quantum dot solution in a sealed manner for spin coating.
FA synthesized by the above preparation method0.8Cs0.2PbBr3The quantum dots showed good fluorescence effect as shown in fig. 1 and 2. As shown in FIG. 3, XRD thereof also showed stabilityA perovskite crystalline phase of (a).
Use of FA0.8Cs0.2PbBr3The quantum dot is used for preparing the light-emitting diode, and the preparation process is as follows in sequence:
firstly, taking 70 mu L of PEDOT, namely PSS, to be spin-coated on an ITO substrate treated by ultraviolet ozone, and spin-coating at the rotating speed of 3000rpm for 60s to prepare a hole transport layer;
secondly, dripping 50 mu L of PVK chlorobenzene solution on a substrate, spin-coating at the rotating speed of 1000rpm for 20s to prepare a film, and annealing at 160 ℃ for 30 min;
third, 100. mu.L of FA is taken0.8Cs0.2PbBr3The quantum dot solution is spin-coated at 6000rpm for 20s, and 100 μ L of FA is taken0.8Cs0.2PbBr3Spin-coating the quantum dot solution at the rotating speed of 3000rpm for 30s, and repeating the operation for 3 times to obtain the perovskite quantum dot film;
the fourth step, will have FA0.8Cs0.2PbBr3Putting the substrate of the quantum dot film into a vacuum evaporation chamber, and sequentially evaporating B3PYMPM TPBi and B3PYMPM Cs2CO3And mixing the electron transport layer and the Al metal electrode in a double-layer manner to obtain the light-emitting diode structure shown in figure 5.
Example 2
When the addition amount of 2-AEHS in the precursor solution is 0.5mg/mL, the 2-AEHS passivated FA0.8Cs0.2PbBr3The preparation method of the quantum dots comprises the following steps:
(1) 5mg of 2-AEHS was dissolved in 10mL of DMF to prepare a 0.5mg/mL solution of 2-AEHS.
(2) Weighing 73.4mg of lead bromide and 39.9mg of formamidine bromide, dissolving the lead bromide and formamidine bromide in 2mL of 0.5mg/mL 2-AEHS solution, adding 90 mu L of oleic acid and 15 mu L of octylamine, stirring for 30min at 50 ℃, dissolving to obtain a precursor solution A, and cooling for later use; weighing 17.0mg of cesium bromide and 73.4mg of lead bromide, dissolving in 2mL of 0.5mg/mL 2-AEHS solution, adding 90 μ L of oleic acid and 15 μ L of octylamine, stirring at 70 ℃ for 30min, dissolving to obtain a precursor solution B, and cooling for later use.
(3) And mixing the precursor solution A and the precursor solution B, and stirring at 50 ℃ for 30min to obtain the required perovskite precursor solution. And (3) quickly injecting 250 mu L of perovskite precursor solution into 10mL of toluene which is stirred violently, centrifuging the solution at 5000rpm for 10min after injection is finished, and storing the supernatant as 2-AEHS-passivated quantum dot solution in a sealed manner for spin coating.
The fluorescence spectrum of the 2-AEHS passivated quantum dot is shown in figure 1, and the 2-AEHS passivated quantum dot is found to be compared with FA0.8Cs0.2PbBr3The fluorescence intensity of the quantum dots is obviously improved, and FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3The fluorescence spectrum peak position and full width at half maximum of the quantum dots are not changed. FIG. 2 shows FA0.8Cs0.2PbBr3Quantum dots and 2-AEHS passivated FA0.8Cs0.2PbBr3Transient fluorescence Spectroscopy of Quantum dots, 2-AEHS passivated FA0.8Cs0.2PbBr3Quantum dot to FA0.8Cs0.2PbBr3The fluorescence attenuation of the quantum dots is obviously slowed down, and the average service life is prolonged. As shown in TEM and HRTEM of FIG. 4, introduction of 2-AEHS into FA0.8Cs0.2PbBr3The size appearance and the interplanar spacing of the quantum dots have no influence.
FA passivated with 2-AEHS0.8Cs0.2PbBr3The preparation process of the perovskite quantum dot light-emitting diode prepared by the quantum dot is the same as that of the embodiment 1. Fig. 6 is a current efficiency-voltage curve of the led obtained from example 1 and example 2 tested under applied voltage, and it was found that the led prepared by using 2-AEHS passivated quantum dots has higher current efficiency. FIG. 7 is a graph of luminance decay for the devices shown in examples 1 and 2, and finding 2-AEHS passivated FA0.8Cs0.2PbBr3The light-emitting diode prepared by the quantum dots has slower brightness decay speed, which shows that the 2-AEHS passivated quantum dots have better stability under continuous electrification.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can understand that the modifications or substitutions within the technical scope of the present invention are included in the scope of the present invention, and therefore, the scope of the present invention should be subject to the protection scope of the claims.
Claims (8)
1. A short-chain inorganic acid ester passivation material is characterized by comprising an extremely short alkyl chain segment, wherein the alkyl chain segment comprises a functional group A and a functional group B, the functional group A is at least one of sulfate, bisulfate, sulfite, nitrate, sulfonate, phosphate and hydrogen phosphate, and the functional group B is an amino group.
2. The short-chain inorganic acid ester passivation material of claim 1, wherein the short-chain inorganic acid ester passivation material has a general structural formula as follows:
wherein R = (CH)2)nN is more than or equal to 1 and less than or equal to 6, n is an integer, and X is at least one of sulfate ester group, bisulfate ester group, sulfite ester group, bisulfite ester group, nitrite ester group, nitrate ester group, sulfonate ester group, phosphate ester group and hydrogen phosphate ester group.
3. Use of a short chain inorganic acid ester passivation material according to any of claims 1 to 2, characterized in that: the short-chain inorganic acid ester passivation material passivates perovskite quantum dots.
4. Use of a short chain inorganic acid ester passivation material according to claim 3, characterized in that: the short-chain inorganic acid ester passivation material is directly added into the perovskite precursor solution to be used as an additive.
5. Use of a short chain inorganic acid ester passivation material according to claim 3, characterized in that: the short-chain inorganic acid ester passivation material is directly added into the perovskite quantum dots to be used as a post-treatment additive.
6. Use of a short chain inorganic acid ester passivation material according to claim 3, characterized in that it comprises the following steps:
s1, dissolving short-chain inorganic acid ester passivation material, metal source halide and organic/inorganic source halide in a polar solvent according to different stoichiometric ratios, and uniformly stirring to prepare perovskite quantum dot precursor solution;
s2, dripping the perovskite quantum dot precursor solution prepared in the step S1 into toluene, and then centrifuging, and taking supernatant, namely the perovskite quantum dot after the material is passivated.
7. Use of a short chain inorganic acid ester passivation material according to claim 6, characterized in that: the metal source halide is at least one of lead halide and stannous halide; the organic/inorganic source halide is at least one of cesium halide, formamidine hydrohalide and methylamine hydrohalide.
8. Use of a short chain inorganic acid ester passivation material according to claim 7, characterized in that: the perovskite quantum dots can be applied to light emitting diodes, solar cells, photodetectors, thin film transistors and lasers.
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| CN101373185A (en) * | 2007-08-23 | 2009-02-25 | 佳能株式会社 | Structure, target substance detection element and target substance detection kit |
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| CN110938432A (en) * | 2019-12-17 | 2020-03-31 | 南京邮电大学 | Preparation method of perovskite quantum dot material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101373185A (en) * | 2007-08-23 | 2009-02-25 | 佳能株式会社 | Structure, target substance detection element and target substance detection kit |
| CN107739349A (en) * | 2017-10-18 | 2018-02-27 | 山东京博石油化工有限公司 | The synthetic method of the thioketones of 3 benzyl, 1,3 thiazole 2 and application |
| CN110938432A (en) * | 2019-12-17 | 2020-03-31 | 南京邮电大学 | Preparation method of perovskite quantum dot material |
Non-Patent Citations (1)
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| A. RADCHANKA和M. ARTEMYEV: "Water-Soluble Cadmium Selenide Quantum Dots withControlled Surface Charge", 《INTERNATIONAL JOURNAL OF NANOSCIENCE》 * |
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