CN111592232A - One-dimensional lead-free cesium copper iodine perovskite yellow light film and preparation method thereof - Google Patents
One-dimensional lead-free cesium copper iodine perovskite yellow light film and preparation method thereof Download PDFInfo
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- CN111592232A CN111592232A CN202010469588.0A CN202010469588A CN111592232A CN 111592232 A CN111592232 A CN 111592232A CN 202010469588 A CN202010469588 A CN 202010469588A CN 111592232 A CN111592232 A CN 111592232A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/284—Halides
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
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Abstract
The invention relates to a one-dimensional lead-free cesium copper iodine perovskite yellow light film and a preparation method thereof, belonging to the technical field of preparation of optoelectronic materials. The preparation method comprises the following steps: dissolving cesium iodide and cuprous iodide in a mixed solution of N, N-dimethylformamide and dimethyl sulfoxide to obtain CsCu2I3Precursor solution, adopting a differential spin coating method to coat the CsCu2I3Coating the precursor solution on a glass sheet, dripping an anti-solvent in the last 10-20s of the spin coating, and then annealing. The film consists of a large number of pine-leaf-shaped micron rods, the length of the micron rods is about several to ten-odd microns, the micron rods not only have good crystal structures, but also have stable structures, do not contain heavy metal lead, reduce the harm to human bodies and the environment, and have wide application prospects in the aspect of photoelectric devices. The preparation method is simple and easy to realize, has low cost and can be popularized in industrial production.
Description
Technical Field
The invention belongs to the technical field of photoelectron material preparation, and particularly relates to a one-dimensional lead-free cesium copper iodine perovskite yellow-light film and a preparation method thereof.
Background
In recent years, lead-halogen perovskite, as a direct band gap semiconductor material, has the advantages of high carrier mobility, long diffusion length, high absorption coefficient, high quantum efficiency and the like, so that the lead-halogen perovskite has excellent performance in the photovoltaic field and also has wide application in the fields of photodetectors, light emitting diodes and the like. The preparation of all-inorganic lead-halogen perovskite nano material has been greatly developed, but the following problems still exist: 1. the problem that the lead-halogen perovskite nano material is easily decomposed in water and heat causes short service life of the device, and the commercial application of the perovskite-based device is seriously limited; 2. the lead-halogen perovskite contains heavy metal lead, has harmfulness to human bodies and the environment, and limits the application of the lead-halogen perovskite in the field of luminous display in the future. Therefore, the existing technology for preparing the lead-halogen perovskite nano material is still to be improved and developed, and the low-toxicity and stable nano material needs to be excavated.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a one-dimensional lead-free cesium copper iodoperovskite yellow light film; the second purpose is to provide a one-dimensional lead-free cesium copper iodine perovskite yellow light film.
In order to achieve the purpose, the invention provides the following technical scheme:
1. one-dimensional CsCu2I3The preparation method of the perovskite yellow light film comprises the following steps:
dissolving cesium iodide and cuprous iodide in a mixed solution of N, N-dimethylformamide and dimethyl sulfoxide to obtain CsCu2I3Precursor solution, adopting a differential spin coating method to coat the CsCu2I3Coating the precursor solution on a glass sheet, dripping an anti-solvent in the last 10-20s of spin coating, and then annealing at 100 ℃ for 1 h; the mass-to-volume ratio of cesium iodide, cuprous iodide, dimethyl sulfoxide and N, N-dimethylformamide is 259-261:380-382:0.8:0.2 and mg: mg: mL: mL, and the differential speed is slow speed first and fast speed later.
Preferably, the dissolving of cesium iodide and cuprous iodide in the mixed solution of N, N-dimethylformamide and dimethyl sulfoxide specifically comprises: adding cesium iodide and cuprous iodide into a mixed solution of N, N-dimethylformamide and dimethyl sulfoxide, and stirring at 40-60 ℃ until the cesium iodide and cuprous iodide are dissolved in the mixed solution.
Preferably, the differential spin coating method specifically comprises: spin coating at 1500-2000rpm for 10-20s, and then spin coating at 3000-4000rpm for 30-50 s.
Preferably, the anti-solvent is methyl acetate.
Preferably, the CsCu2I3The volume ratio of the precursor liquid to the methyl acetate is 7-10: 10-20.
Preferably, the glass sheet is subjected to ultrasonic treatment by using liquid detergent, deionized water, acetone, alcohol and isopropanol in sequence, then is dried by using nitrogen, and then is subjected to ozone treatment.
2. The one-dimensional CsCu prepared by the method2I3Perovskite yellow light film.
The invention has the beneficial effects that: the one-dimensional lead-free cesium copper iodoperovskite yellow-light film prepared by the method consists of a large number of micron rods in pine-leaf shapes, the length of the micron rods is about several to dozens of microns, and the film not only has a good crystal structure, but also is stable in structure, does not contain heavy metal lead, reduces harm to human bodies and the environment, and has a wide application prospect in the aspect of photoelectric devices. The preparation method of the film is simple and easy to realize, has low cost and can be popularized in industrial production.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 shows one-dimensional CsCu prepared in example 12I3Absorption spectrum and fluorescence spectrum of the perovskite yellow light film;
FIG. 2 shows one-dimensional CsCu prepared in example 12I3Photograph of perovskite yellow thin film under fluorescent lamp and UV light respectively (a in FIG. 2 is the thin filmA photograph of the film under a fluorescent lamp, and b in fig. 2 is a photograph of the film under UV light);
FIG. 3 shows one-dimensional CsCu prepared in example 12I3X-ray diffraction patterns of perovskite yellow thin films;
FIG. 4 shows one-dimensional CsCu prepared in example 12I3Scanning electron micrographs of the perovskite yellow thin film;
FIG. 5 shows one-dimensional CsCu prepared in example 12I3Scanning electron microscopy and X-ray energy dispersion spectrograms of the perovskite yellow thin film;
FIG. 6 shows one-dimensional CsCu prepared in example 12I3A stability test result chart of the perovskite yellow light film;
FIG. 7 shows one-dimensional CsCu prepared in example 22I3A fluorescence spectrum of the perovskite yellow thin film;
FIG. 8 shows one-dimensional CsCu prepared in example 22I3Scanning electron micrographs of the perovskite yellow thin film;
FIG. 9 shows one-dimensional CsCu prepared in example 32I3X-ray diffraction patterns of perovskite yellow thin films;
FIG. 10 shows one-dimensional CsCu prepared in example 32I3Scanning electron microscopy of perovskite yellow light thin film.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
Preparation of one-dimensional CsCu2I3Perovskite yellow light film
(1) Carrying out ultrasonic treatment on a glass sheet by using detergent, deionized water, acetone, alcohol and isopropanol in sequence, then drying the glass sheet by using nitrogen, and then carrying out ozone treatment on the glass sheet for later use;
(2) 259.81mg of cesium iodide and 380.9mg of cuprous iodide were added to a mixture of 800. mu. L N, N-dimethylformamide and 200. mu.L of dimethyl sulfoxide, and the mixture was stirred at 60 ℃ until cesium iodide and cuprous iodide were dissolved in the mixture to obtain CsCu2I3Taking 75 μ L of the CsCu as the precursor solution2I3Dripping the precursor on the glass sheet treated in the step (1), spin-coating at 1500rpm for 10s, then spin-coating at 3000rpm for 30s, dripping 100 mu L of methyl acetate at the center of the glass sheet in the last 10s of spin-coating to promote the crystallization of perovskite, and then immediately annealing at 100 ℃ for 1h to prepare the one-dimensional CsCu2I3Perovskite yellow light film.
Example 2
Preparation of one-dimensional CsCu2I3Perovskite yellow light film
(1) Carrying out ultrasonic treatment on a glass sheet by using detergent, deionized water, acetone, alcohol and isopropanol in sequence, then drying the glass sheet by using nitrogen, and then carrying out ozone treatment on the glass sheet for later use;
(2) adding 259mg of cesium iodide and 380mg of cuprous iodide to a mixture of 800. mu. L N, N-dimethylformamide and 200. mu.L of dimethyl sulfoxide, and stirring at 40 ℃ until cesium iodide and cuprous iodide are dissolved in the mixture to obtain CsCu2I3Taking 90 μ L of the CsCu as the precursor solution2I3Dropping the precursor onto the glass sheet treated in the step (1), spin-coating at 1800rpm for 20s, then spin-coating at 3500rpm for 50s, dropping 150 mu L of methyl acetate at the center of the glass sheet for the last 15s of spin-coating to promote the crystallization of perovskite, and then immediately annealing at 100 ℃ for 1h to obtain the one-dimensional CsCu2I3Perovskite yellow light film.
Example 3
Preparation of one-dimensional CsCu2I3Perovskite yellow light film
(1) Carrying out ultrasonic treatment on a glass sheet by using detergent, deionized water, acetone, alcohol and isopropanol in sequence, then drying the glass sheet by using nitrogen, and then carrying out ozone treatment on the glass sheet for later use;
(2) adding 261mg cesium iodide and 382mg cuprous iodide to 800. mu.LStirring the mixture of N, N-dimethylformamide and 200. mu.L of dimethyl sulfoxide at 50 ℃ until cesium iodide and cuprous iodide are dissolved in the mixture to obtain CsCu2I3Taking 100 μ L of the CsCu as the precursor solution2I3Dripping the precursor on the glass sheet treated in the step (1), spin-coating at 2000rpm for 15s, then spin-coating at 4000rpm for 40s, dripping 200 mu L of methyl acetate at the center of the glass sheet in the last 20s of spin-coating to promote the crystallization of perovskite, and then immediately annealing at 100 ℃ for 1h to prepare the one-dimensional CsCu2I3Perovskite yellow light film.
FIG. 1 shows one-dimensional CsCu prepared in example 12I3As can be seen from FIG. 1, the absorption spectrum and fluorescence spectrum of the perovskite yellow thin film have an absorption peak of about 320nm, and the optimal luminescence peak is about 576 nm.
FIG. 2 shows one-dimensional CsCu prepared in example 12I3The photographs of the perovskite yellow film under the fluorescent light and the UV light respectively are shown in the figure 2, wherein a is the photograph of the film under the fluorescent light, and the figure 2, b is the photograph of the film under the UV light, and as can be seen from the figure 2, under the excitation of the UV light, the film emits yellow light, which corresponds to the fluorescence spectrum in the figure 1.
FIG. 3 shows one-dimensional CsCu prepared in example 12I3The X-ray diffraction pattern of the perovskite yellow thin film is shown in FIG. 3, and the diffraction peak of the thin film and CsCu2I3Standard card (JCPDS No.77-0069) corresponds to the prepared CsCu2I3Has good crystal structure.
FIG. 4 shows one-dimensional CsCu prepared in example 12I3Scanning electron microscopy of the perovskite yellow thin film, as can be seen from fig. 4, the thin film is composed of a large number of micron rods exhibiting a pine-leaf type, the length of the micron rods being about several to ten and several microns.
FIG. 5 shows one-dimensional CsCu prepared in example 12I3FIG. 5 shows a scanning electron micrograph and an X-ray energy dispersion spectrogram of the perovskite yellow thin film, and the CsCu is2I3The three elements of Cs, Cu and I in the perovskite yellow light film are uniformly distributed.
FIG. 6 shows one-dimensional CsCu prepared in example 12I3The stability test result chart of the perovskite yellow light film comprises the following test conditions: humidity 75%, temperature 60 ℃ and the CsCu shown in FIG. 62I3The perovskite yellow light film has higher stability.
FIG. 7 shows one-dimensional CsCu prepared in example 22I3As is clear from FIG. 7, the fluorescence spectrum of the perovskite yellow thin film showed an emission peak of about 577 nm.
FIG. 8 shows one-dimensional CsCu prepared in example 22I3Scanning electron microscopy of the perovskite yellow thin film, as can be seen from fig. 8, the thin film is composed of a large number of micron rods exhibiting a pine-leaf type, the length of the micron rods being about several to ten and several microns.
FIG. 9 shows one-dimensional CsCu prepared in example 32I3The X-ray diffraction pattern of the perovskite yellow thin film is shown in FIG. 9, and the diffraction peak of the thin film and CsCu2I3Standard card (JCPDS No. 77-0069).
FIG. 10 shows one-dimensional CsCu prepared in example 32I3Scanning electron microscopy of the perovskite yellow thin film, as can be seen from fig. 10, the thin film is composed of a large number of micron rods exhibiting a pine-leaf type, the length of the micron rods being about several to ten and several microns.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (7)
1. One-dimensional CsCu2I3The preparation method of the perovskite yellow light film is characterized by comprising the following steps:
dissolving cesium iodide and cuprous iodide in a mixed solution of N, N-dimethylformamide and dimethyl sulfoxide to obtain CsCu2I3Precursor solution, miningThe CsCu is coated by a differential speed spin coating method2I3Coating the precursor solution on a glass sheet, dripping an anti-solvent in the last 10-20s of spin coating, and then annealing at 100 ℃ for 1 h; the mass-to-volume ratio of cesium iodide, cuprous iodide, dimethyl sulfoxide and N, N-dimethylformamide is 259-261:380-382:0.8:0.2 and mg: mg: mL: mL, and the differential speed is slow speed first and fast speed later.
2. The method according to claim 1, wherein the cesium iodide and cuprous iodide are dissolved in a mixed solution of N, N-dimethylformamide and dimethylsulfoxide, specifically: adding cesium iodide and cuprous iodide into a mixed solution of N, N-dimethylformamide and dimethyl sulfoxide, and stirring at 40-60 ℃ until the cesium iodide and cuprous iodide are dissolved in the mixed solution.
3. The method according to claim 1, characterized in that the differential spin coating is in particular: spin coating at 1500-2000rpm for 10-20s, and then spin coating at 3000-4000rpm for 30-50 s.
4. The process of claim 1, wherein the anti-solvent is methyl acetate.
5. The method of claim 4, in which the CsCu2I3The volume ratio of the precursor liquid to the methyl acetate is 7-10: 10-20.
6. The method of any one of claims 1-5, wherein the glass sheet is treated with a detergent, deionized water, acetone, alcohol, and isopropanol in sequence, followed by nitrogen blow-drying, and then ozone treatment.
7. One-dimensional CsCu prepared by the method of any of claims 1-62I3Perovskite yellow light film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114464692A (en) * | 2022-01-21 | 2022-05-10 | 湖北文理学院 | Perovskite ink and application thereof |
| CN114592239A (en) * | 2022-03-04 | 2022-06-07 | 广州大学 | Method for improving performance of deep ultraviolet photoelectric detector |
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| CN109943322A (en) * | 2019-03-26 | 2019-06-28 | 华中科技大学 | A kind of application and preparation method thereof of compound as scintillator material |
| CN110611014A (en) * | 2019-09-19 | 2019-12-24 | 深圳第三代半导体研究院 | Cs (volatile organic Compounds)3Cu2I5Ultraviolet detector and film preparation method thereof |
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2020
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| CN109943322A (en) * | 2019-03-26 | 2019-06-28 | 华中科技大学 | A kind of application and preparation method thereof of compound as scintillator material |
| CN110611014A (en) * | 2019-09-19 | 2019-12-24 | 深圳第三代半导体研究院 | Cs (volatile organic Compounds)3Cu2I5Ultraviolet detector and film preparation method thereof |
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| RICHENG LIN等: "All-Inorganic CsCu2I3 Single Crystal with High-PLQY(≈15.7%) Intrinsic White-Light Emission via Strongly Localized 1D Excitonic Recombination", 《ADVANCED MATERIALS》 * |
| TAEHWAN JUN等: "One-step solution synthesis of white-light-emitting films via dimensionality control of the Cs–Cu–I system", 《APL MATERIALS》 * |
| ZHUANGZHUANG MA等: "Stable Yellow Light-Emitting Devices Based on Ternary Copper Halides with Broadband Emissive Self-Trapped Excitons", 《ACS NANO》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114464692A (en) * | 2022-01-21 | 2022-05-10 | 湖北文理学院 | Perovskite ink and application thereof |
| CN114592239A (en) * | 2022-03-04 | 2022-06-07 | 广州大学 | Method for improving performance of deep ultraviolet photoelectric detector |
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