CN111892081A - CsPbI3Mixed phase perovskite film and controllable preparation method thereof - Google Patents
CsPbI3Mixed phase perovskite film and controllable preparation method thereof Download PDFInfo
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- CN111892081A CN111892081A CN202010602904.7A CN202010602904A CN111892081A CN 111892081 A CN111892081 A CN 111892081A CN 202010602904 A CN202010602904 A CN 202010602904A CN 111892081 A CN111892081 A CN 111892081A
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Abstract
The invention relates to CsPbI3The mixed phase perovskite thin film and the controllable preparation method thereof comprise the following operation steps: step 1: adding octadecene, oleylamine, oleic acid and lead iodide into a three-neck flask, heating and stirring at 140-180 ℃ under a vacuum condition to serve as a reaction solvent; step 2: dissolving cesium stearate and oleic acid in octadecene to form a precursor solution; and step 3: quickly injecting the precursor solution into a reaction solvent, quickly cooling by water, and then centrifugally purifying to obtain the perovskite CsPbI3Quantum dots; and 4, step 4: taking CsPbI3Spin coating the dispersion liquid of the quantum dots on the surface of a clean glass sheet, and performing heat treatment in the atmospheric environment to obtain CsPbI3A mixed phase perovskite thin film. CsPbI prepared by the method3A mixed phase perovskite thin film. The invention usesCsPbI3The monomer emission white light is obtained, and the material is novel; based on the all-inorganic perovskite material, the material is more stable than the traditional perovskite material; CsPbI achievement by temperature and time of thermal treatment3The method is simple and easy to implement.
Description
Technical Field
The invention relates to CsPbI3A mixed phase perovskite film and a controllable preparation method thereof, belonging to the technical field of novel nano materials.
Background
White electroluminescent light is a phenomenon simulating natural light, and has become a common and important daily lighting means in people's daily life, such as backlight in liquid crystal displays or indoor/street lighting. Generally, commercial electroluminescent white light is mainly realized by covering a yellow phosphor on a blue chip, but the color rendering index is low and the luminous efficiency is low. There are two main ways to realize white light, one is the mixture of red, green and blue, and the other is the direct monomer emission of white light.
At present, the external quantum efficiency of red and green perovskite light emitting diodes exceeds 20%, the blue light efficiency is low but close to 10%, and the research on the real electro-white light is very little, so that the development of high-efficiency white light emitting diodes becomes the current research hotspot. A single material with efficient and stable white light emission is most desirable for illumination, but it is difficult to achieve photon emission that covers the entire visible spectrum. Recently, the exciton self-trapping mechanism of perovskite provides possibility for realizing white light emission of monomer, and is a hot spot of current research, and the self-trapping behavior requires strong coupling between exciton (or carrier) and lattice distortion, so that white light emission with wide spectrum is shown.
Disclosure of Invention
In order to solve the technical problems, the invention provides CsPbI3The mixed phase perovskite film and the controllable preparation method thereof have the following specific technical scheme:
controllable preparation CsPbI3The method for preparing the mixed phase perovskite thin film comprises the following operation steps:
step 1: adding octadecene, oleylamine, oleic acid and lead iodide into a three-neck flask, heating and stirring at 140-180 ℃ under a vacuum condition to serve as a reaction solvent;
step 2: dissolving cesium stearate and oleic acid in octadecene to form a precursor solution;
and step 3: quickly injecting the precursor solution into a reaction solvent, quickly cooling by water, growing the quantum dot nuclei, and then centrifugally purifying to remove redundant long-chain organic ligands on the surfaces of the quantum dots so as to promote the transport of current carriers, namely the perovskite CsPbI is prepared3Quantum dots;
and 4, step 4: perovskite CsPbI3Quantum dots are dispersed in a solvent to obtain CsPbI3Dispersing liquid of quantum dots, CsPbI3Spin coating the quantum dot dispersion on the surface of a clean glass sheet, and heat treating in atmospheric environment, CsPbI3The black phase can change phase under the action of water and oxygen, part of the black phase can be converted into yellow phase, and CsPbI is obtained by controlling the temperature and the time3The mixed phase perovskite thin film has large contact surface area of the black phase and the yellow phase, so that the mixed phase thin film well combines the excellent photoelectric property and carrier transport property of the black phase and the wide spectrum of the yellow phase, meanwhile, the black phase effectively supplements the red spectrum part, and the two phases are cooperatively matched to realize the spectrum coverage of the whole visible light and obtain the emission of the white light of the monomer.
Furthermore, the volume ratio of oleic acid to octadecene in the reaction solvent prepared in the step 1 is 1: 10-20, the molar ratio of oleic acid to lead iodide is 1: 1-2, and the volume ratio of oleic acid to oleylamine is 1: 1-2.
Furthermore, the volume ratio of oleic acid to octadecene in the precursor solution prepared in the step 2 is 1: 10-20, and the molar ratio of oleic acid to cesium stearate is 1: 1-2.
Further, the stirring speed in the step 1 is 600-800 r/min.
Further, the volume ratio of the precursor solution to the reaction solvent in the step 3 is 1: 10-20.
Further, the centrifugal purification process in step 3 is as follows: dissolving the water-cooled precursor solution and the reaction solvent mixed solution into a flocculating agent, stirring and mixing uniformly, then placing the flocculating agent on a centrifuge for centrifugation, attaching the precipitate to the side wall after centrifugation, and pouring out the solution to obtain the precipitate, namely the perovskite CsPbI3The flocculant is methanol, isopropanol, acetone, n-butanol or tert-butanol.
Further, the solvent in the step 4 is selected from n-octane, n-hexane or toluene, CsPbI3The concentration of the dispersion of quantum dots was 15 mg/mL.
Further, CsPbI in the step 43In the preparation of the quantum dot dispersion, a solvent is added to the precipitate of step 3 and stirred until the precipitate is completely dissolved.
Further, the relative humidity of the environment for heat treatment in the step 4 is 40-60%, the time for heat treatment is 20-60min, and the treatment temperature is 120-140 ℃.
CsPbI prepared by any one of the above methods3A mixed phase perovskite thin film.
The invention has the beneficial effects that:
1) the invention uses CsPbI3The homogeneous heterogeneous structure is obtained, the black phase and the yellow phase emit different colors and complement each other on the spectrum, so that the monomer emits white light jointly, and the material is novel;
2) the nano material prepared by the invention is based on an all-inorganic perovskite material, and is more stable than the traditional perovskite material;
3) the invention can realize CsPbI through heat treatment3The black phase is converted into the yellow phase, the phase regulation and control are realized by regulating the temperature and the time, and the method is simple and easy to implement.
Drawings
FIG. 1 shows CsPbI prepared in example 1 of the present invention3SEM scan of the miscible thin film,
FIG. 2 shows CsPbI prepared in example 1 of the present invention3The XRD pattern of the mixed phase film,
FIG. 3 shows CsPbI prepared in example 1 of the present invention3The photoluminescence spectrum of the mixed-phase film,
FIG. 4 shows CsPbI prepared in example 1 of the present invention3Light absorption spectrum of the miscible thin film.
Detailed Description
The present invention will now be described in further detail with reference to the accompanying drawings.
The invention relates to a method for preparing perovskite CsPbI by using a high-temperature thermal injection method3Quantum dot, spin coating on substrate to form film, and heat treating to control CsPbI under certain humidity and temperature3Conversion of yellow and black phases to obtain CsPbI3A method for preparing a mixed phase perovskite thin film.
Example 1
The controllable preparation CsPbI described in the embodiment3The method for preparing the mixed phase perovskite thin film specifically comprises the following steps:
1) adding 15 mL of octadecene, 2mL of oleylamine, 1mL of oleic acid and 0.5 mmol of lead iodide into a three-neck flask, placing the three-neck flask in a heating jacket at 180 ℃, vacuumizing the device and keeping an argon atmosphere, keeping the temperature stable at 180 ℃, turning on magnetic stirring, and stirring at the speed of 800 r/min.
2) And completely dissolving cesium stearate and oleic acid in octadecene according to the molar ratio of 1:1.1 to form a precursor solution.
3) And (3) quickly injecting the prepared precursor mixed solution into the reaction solvent which is being heated and stirred according to the volume ratio of 1:15, reacting for 5-10 s, and quickly cooling to room temperature by water.
4) Adding a mixed solution of isopropanol and ethyl acetate into the obtained reaction product, cleaning, centrifuging, removing supernatant, and dispersing the precipitate in n-octane to obtain the final CsPbI3Perovskite quantum dots.
5) Using CsPbI3Spin-coating the quantum dot dispersion liquid on the surface of a clean glass sheet by using a spin coater, and carrying out heat treatment for 30 min in an atmospheric environment with the relative humidity of 40-60%, wherein the treatment temperature is 120 ℃, so as to obtain CsPbI3A mixed phase perovskite thin film.
FIG. 1 shows CsPbI prepared in this example3The SEM scanning image of the mixed phase perovskite film can be seen, the film is uniform and flat, and the good operability is shown.
And CsPbI prepared in this example was added3The mixed phase perovskite thin film is respectively tested to obtain an XRD pattern shown in figure 2, a photoluminescence pattern shown in figure 3, a light absorption pattern shown in figure 4 and a junctionAs can be seen from FIGS. 2-4, CsPbI is also present in the film3The black phase and the yellow phase prove the feasibility of phase regulation, and meanwhile, the photoluminescence spectrum covers the whole visible light and shows the characteristics of white light emission
Example 2
Similar to example 1, except that the mixed solution of isopropyl alcohol and ethyl acetate in step 4 of example 1 was changed to a mixed solution of isopropyl alcohol and butyl acetate, and other conditions were maintained to be the same, the CsPbI-based sample was prepared3A mixed phase perovskite thin film of the material.
Example 3
Similar to example 1, except that n-octane was changed to n-hexane in step 4) of example 1, and the other conditions were kept the same, the CsPbI-based material was prepared3A mixed phase perovskite thin film of the material.
Example 4
Similar to example 1, except that n-octane in step 4) of example 1 was changed to toluene and the other conditions were kept the same, the CsPbI-based sample was prepared3A mixed phase perovskite thin film of the material.
Example 5
Similar to example 1, except that the treatment temperature in step 5) of example 1 was changed to 130 ℃, other conditions were kept consistent, and CsPbI-based substrates were prepared3A mixed phase perovskite thin film of the material.
Example 6
Similar to example 1, except that the treatment time in step 5) of example 1 was changed to 40min, and other conditions were kept consistent, CsPbI-based samples were prepared3A mixed phase perovskite thin film of the material.
By adjusting different purification solvents and dispersion solvents to process the perovskite quantum dots, the mixed solution of isopropanol and butyl acetate has better purification effect on the perovskite quantum dots, n-octane is used for dispersing the perovskite quantum dots, and the treatment temperature and time of 40min at 120 ℃ are optimal in terms of heat treatment time.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. Controllable preparation CsPbI3The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: the method comprises the following operation steps:
step 1: adding octadecene, oleylamine, oleic acid and lead iodide into a three-neck flask, heating and stirring at 140-180 ℃ under a vacuum condition to serve as a reaction solvent;
step 2: dissolving cesium stearate and oleic acid in octadecene to form a precursor solution;
and step 3: quickly injecting the precursor solution into a reaction solvent, quickly cooling by water, growing the quantum dot nuclei, and then centrifugally purifying to remove redundant long-chain organic ligands on the surfaces of the quantum dots so as to promote the transport of current carriers, namely the perovskite CsPbI is prepared3Quantum dots;
and 4, step 4: perovskite CsPbI3Quantum dots are dispersed in a solvent to obtain CsPbI3Dispersing liquid of quantum dots, CsPbI3Spin coating the quantum dot dispersion on the surface of a clean glass sheet, and heat treating in atmospheric environment, CsPbI3The black phase can change phase under the action of water and oxygen, part of the black phase can be converted into yellow phase, and CsPbI is obtained by controlling the temperature and the time3The mixed phase perovskite thin film has large contact surface area of the black phase and the yellow phase, so that the mixed phase thin film well combines the excellent photoelectric property and carrier transport property of the black phase and the wide spectrum of the yellow phase, meanwhile, the black phase effectively supplements the red spectrum part, and the two phases are cooperatively matched to realize the spectrum coverage of the whole visible light and obtain the emission of the white light of the monomer.
2. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: in the reaction solvent prepared in the step 1, the volume ratio of oleic acid to octadecene is 1: 10-20, and the oleic acid and lead iodide have molThe molar ratio is 1: 1-2, and the volume ratio of the oleic acid to the oleylamine is 1: 1-2.
3. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: the volume ratio of oleic acid to octadecene in the precursor solution prepared in the step 2 is 1: 10-20, and the molar ratio of oleic acid to cesium stearate is 1: 1-2.
4. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: the stirring speed in the step 1 is 600-800 r/min.
5. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: the volume ratio of the precursor solution to the reaction solvent in the step 3 is 1: 10-20.
6. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: the centrifugal purification process in the step 3 comprises the following steps: dissolving the water-cooled precursor solution and the reaction solvent mixed solution into a flocculating agent, stirring and mixing uniformly, then placing the flocculating agent on a centrifuge for centrifugation, attaching the precipitate to the side wall after centrifugation, and pouring out the solution to obtain the precipitate, namely the perovskite CsPbI3The flocculant is methanol, isopropanol, acetone, n-butanol or tert-butanol.
7. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: the solvent in the step 4 is selected from n-octane, n-hexane or toluene, CsPbI3The concentration of the dispersion of quantum dots was 15 mg/mL.
8. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: CsPbI in the step 43In the preparation of the dispersion of quantum dotsAdding a solvent into the precipitate obtained in the step 3 and stirring until the precipitate is completely dissolved.
9. Controllable preparation CsPbI according to claim 13The method for preparing the mixed phase perovskite thin film is characterized by comprising the following steps: the relative humidity of the environment for heat treatment in the step 4 is 40-60%, the time for heat treatment is 20-60min, and the treatment temperature is 120-140 ℃.
10.CsPbI3The mixed phase perovskite thin film is characterized in that: made by the process of any preceding claim.
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Cited By (3)
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| CN113285030A (en) * | 2021-04-26 | 2021-08-20 | 北方民族大学 | Planar CsPbI3Method for preparing battery |
| CN114316970A (en) * | 2021-12-30 | 2022-04-12 | 宁波东旭成新材料科技有限公司 | Preparation method of quantum dot film |
| CN117417742A (en) * | 2023-06-30 | 2024-01-19 | 浙江大学温州研究院 | Preparation method of alcohol-resistant perovskite quantum dot |
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