CN114373864A - Preparation method of organic-inorganic hybrid perovskite film - Google Patents
Preparation method of organic-inorganic hybrid perovskite film Download PDFInfo
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- H—ELECTRICITY
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Abstract
The invention relates to a preparation method of an organic-inorganic hybrid perovskite film, which comprises the following steps: firstly, a certain amount of PbI is added2Sequentially adding the powder and PEAI powder into solvent at a certain ratio, stirring in a beaker at room temperature to dissolve completely to obtain (PEA)2PbI4A perovskite precursor solution; then Prepared (PEA)2PbI4Dripping the precursor solution on a cleaned film substrate, uniformly coating the perovskite precursor solution on the substrate by using a spin coating method, and naturally drying to obtain (PEA)2PbI4A perovskite thin film. Prepared by the invention (PEA)2PbI4The perovskite thin film has the characteristics of high crystallization quality, large grain size and low defect density, and can be used in the fields of photoelectric display, solar cells, photoelectric detectors and the like.
Description
Technical Field
The invention relates to the field of perovskite materials, in particular to a preparation method of an organic-inorganic hybrid perovskite thin film.
Background
As a novel composite functional material, the organic-inorganic hybrid perovskite combines the diversity of organic material structures with the advantage of high carrier mobility of inorganic semiconductor materials, has the characteristics of strong light absorption capacity, high extinction coefficient, long carrier diffusion distance, excellent photoluminescence property and the like, and draws people's attention in the fields of illumination display, photoelectric detectors, solar cells and the like.
Larger organic cations in the organic-inorganic hybrid perovskite material serve as spacers on one hand to isolate an inorganic metal halide octahedral layer, a quantum well superlattice structure is formed on an energy band, and the organic cations serve as an insulation barrier to limit charge carriers in a two-dimensional space, so that the mobility of the charge carriers is improved; on the other hand, the hydrophobic organic cation can also effectively isolate the ion lattice of the inorganic octahedron from the environmental water molecules, and the unique organic-inorganic laminated structure ensures that the inorganic octahedron has good crystallization effect and chemical stability, particularly the stability to water, which cannot be reached by the traditional halogen perovskite material.
At present, the preparation methods of the perovskite thin film commonly used mainly comprise a spraying method and a spin coating method, but the spraying method and the spin coating method have certain requirements on the thin film substrate material to different degrees. Compared with a spraying method for preparing the film, the utilization rate of the perovskite precursor solution can be improved by using a spin-coating method; because the spin coating is carried out in a relatively closed environment, the pollution to the experimental environment is also avoided. An anti-solvent is generally used in the spin coating process, so that the perovskite can be rapidly nucleated and crystallized out to achieve better film forming effect, but the control of the perovskite nucleation density and crystallization rate is also provided with considerable test.
In addition, the traditional spin-coating method for preparing the film is subjected to an annealing process, which puts high requirements on the heat resistance of the substrate to a certain degree, and needs to avoid irreversible influence on the physical and chemical properties of the film in the annealing process. This undoubtedly puts higher demands on the experimenter and the experimental environment, and also increases the risk of experimental failure to some extent.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method which is simple to operate, low in cost, non-selective to a substrate material and easy to grow large-size grains; the method can be carried out only in room temperature and atmospheric environment; the prepared perovskite film has good uniformity, high crystallization quality and good stability.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of an organic-inorganic hybrid perovskite thin film comprises the following steps:
firstly, mixing PbI2Sequentially adding the powder and PEAI powder into solvent, stirring to dissolve completely to obtain (PEA)2PbI4A perovskite precursor solution;
then, the Prepared (PEA)2PbI4The perovskite precursor solution was dropped on the base material, and (PEA) was applied using a spin coating method2PbI4Coating perovskite precursor solution uniformly, and evaporating solvent by natural drying to obtain (PEA)2PbI4Organic-inorganic hybrid perovskite thin films.
Further, the solvent is a polar solvent, and comprises N, N-Dimethylformamide (DMF), gamma-butyrolactone or dimethyl sulfoxide (DMSO).
The PEAI has good solubility in the three polar solvents, the formed perovskite precursor solution is in a yellow transparent liquid state, the required perovskite materials are uniformly mixed in the solvents in an ion form, and the solution does not generate any precipitate after being stored for 150 days and still has good Tyndall effect. Therefore, the perovskite precursor solution can be used for a long time, the utilization rate is high, the waste of medicines is avoided, and the material preparation cost is controlled from the source.
Further, (PEA)2PbI4PbI in perovskite precursor solution2And PEAI concentrations of 0.8-1.2mol/L and 1.6-2.4mol/L, respectively.
Further, the PbI2And the amount of PEAI material is 1: 2.
Further, the stirring time is 10-20 min.
Further, the substrate material comprises common glass, ITO glass, FTO glass or sapphire.
Further, the substrate material is cleaned.
Further, the cleaning process specifically comprises: firstly, cleaning a substrate material by using ethanol, and then, cleaning for the second time by using a polar solvent used for preparing a precursor solution.
Further, the spin coating method comprises the following specific steps: firstly, spin-coating for 1-2min at a low rotation speed, then adjusting the rotation speed to a medium rotation speed, wherein the spin-coating time is 2-3min, and finally, spin-coating for 1min at a high rotation speed.
Further, the low rotation speed is not higher than 500rpm, the medium rotation speed is 800-1000rpm, and the high rotation speed is 2000 rpm.
The perovskite thin film obtained by the method has the characteristic of large-area uniform distribution, and the growth orientation of crystal grains presents a single (002) crystal face direction and is a typical two-dimensional layered structure. The perovskite thin film has the characteristics of high crystallization quality, large grain size and low defect density, and can be used in the fields of photoelectric display, solar cells, photoelectric detectors and the like.
The two chemicals used in the present invention are respectively PbI2Compared with PEAI, the solution of the invention has higher concentration and PbI2And the concentration of PEAI in the solvent is respectively 0.8-1.2mol/L, namely 369-553mg/mL and 1.6-2.4mol/L, namely 340-598mg/mL, to reach a near-saturation state, while the solution concentration of the prior art is usually only 0.4-1mol/L or 0.1-100mg/mL, so that the high solution concentration can be taken as the driving force for crystallization, even in the normal conditionUnder the environment of normal temperature and pressure, the crystal can be supersaturated and separated out along with the volatilization of the solvent, and the heating treatment is not needed.
Compared with the prior art, the invention has the following advantages:
(1) when the perovskite precursor solution is prepared, any one polar solvent of N, N-Dimethylformamide (DMF), gamma-butyrolactone or dimethyl sulfoxide (DMSO) can be used as PbI2And PEAI to provide the solvent environment required for the reaction; a complex system is formed without adding a ligand to control the nucleation and growth of the perovskite crystal, so that the operation is simplified;
(2) the method is a one-step film forming method, namely, a perovskite precursor solution is dripped on a film substrate, and the film can be generated by spin coating and solvent evaporation along with crystal growth and precipitation without using an anti-solvent to induce rapid nucleation of perovskite; in the process of preparing the perovskite thin film by spin coating, an intermediate layer does not need to be deposited and the subsequent annealing process does not need to be carried out to respectively improve the adhesion effect of the thin film and eliminate the surface defects of the thin film, the influence of the annealing mode, temperature and time on the perovskite crystallization process is avoided, and the technological process is simple;
(3) in the process of preparing the perovskite thin film by spin coating, the selection of the thin film substrate is independent, the used thin film substrate can be any one of common glass, ITO glass, FTO glass and sapphire, and the applicability is wide;
(4) in the invention, the preparation processes of the perovskite precursor solution and the film are carried out at room temperature and in the atmospheric environment without controlling the temperature and pressure conditions, so that the invention can quickly realize one-step film formation, is simple and easy to implement, has low cost and is very suitable for industrial production.
Drawings
FIG. 1 is (PEA) prepared in example 12PbI4XRD patterns of perovskite thin films;
FIG. 2 is (PEA) prepared in example 12PbI4PL spectra of the perovskite thin film;
FIG. 3 is (PEA) prepared in example 12PbI4Perovskite thin filmUV-vis absorption spectrum of (1);
FIG. 4 is (PEA) prepared in example 12PbI4Optical microscopy of perovskite thin films;
FIG. 5 is (PEA) prepared in example 12PbI4SEM image of perovskite thin film.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. 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 scope of the present invention is not limited to the following embodiments.
A preparation method of an organic-inorganic hybrid perovskite thin film comprises the following steps:
firstly, mixing PbI2Sequentially adding the powder and PEAI powder into solvent, stirring for 10-20min to dissolve completely to obtain (PEA)2PbI4A perovskite precursor solution; the solvent is a polar solvent, including N, N-Dimethylformamide (DMF), gamma-butyrolactone or dimethyl sulfoxide (DMSO). (PEA)2PbI4PbI in perovskite precursor solution2And PEAI concentrations of 0.8-1.2mol/L and 1.6-2.4mol/L, respectively. PbI2And the amount of PEAI material is preferably 1: 2.
Then, the Prepared (PEA)2PbI4The perovskite precursor solution is dripped on a cleaned substrate material, and the substrate material comprises common glass, ITO glass, FTO glass or sapphire. Using spin coating method (PEA)2PbI4Coating perovskite precursor solution uniformly, and evaporating solvent by natural drying to obtain (PEA)2PbI4Organic-inorganic hybrid perovskite thin films. The spin coating method comprises the following specific steps: firstly, spin-coating for 1-2min at a low rotation speed, then adjusting the rotation speed to a medium rotation speed, wherein the spin-coating time is 2-3min, and finally, spin-coating for 1min at a high rotation speed. The low rotation speed is not higher than 500rpm, the medium rotation speed is 800-1000rpm, and the high rotation speed is 2000 rpm.
Example 1
A preparation method of an organic-inorganic hybrid perovskite thin film specifically comprises the following steps:
(1) firstly according to PbI20.6915g and 0.747g were weighed out at a molar ratio of 1:2, respectively, and added to 1mL of gamma-butyrolactone to form a solution, which was stirred for 10-20min, and PbI was added by a solution method2Completely reacting with PEAI to obtain yellow transparent slightly viscous precursor solution;
(2) and (2) extracting 1 mu L of the perovskite precursor solution prepared in the step (1) by using a liquid-transferring gun, and then dropwise adding the perovskite precursor solution on a common glass substrate which is sequentially cleaned by ethanol and gamma-butyrolactone. Setting the initial spin-coating rotation speed at 500rpm, after 90 seconds of spin-coating, increasing the spin-coating rotation speed to 800-1000rpm, continuing spin-coating for 120 seconds, gradually seeing that yellow crystals on the film substrate begin to precipitate in the process, then increasing the spin-coating speed to 2000rpm again, after 60 seconds of spin-coating, gradually reducing the spin-coating speed until the speed is zero, and after the spin-coating is finished, obtaining (PEA)2PbI4A perovskite thin film.
For the above obtained (PEA)2PbI4The perovskite thin film was tested, and the measured XRD pattern, PL spectrum, UV-vis absorption spectrum, optical microscopy pattern and SEM are shown in FIGS. 1-5.
The result of the invention (PEA) can be seen in FIG. 12PbI4The XRD diffraction peaks of the perovskite thin film crystal are all sharp diffraction peaks of a plane series (00l, l is 2, 4, 6, 8,.., 20) along the c axis at equal intervals, and no diffraction peaks exist in other directions, so that the thin film is proved to have a relatively stable layered structure. In addition, the sharp diffraction peak shows that the crystal structure has high crystallinity and high phase purity, and has good orientation and crystallinity. And the layered structure is formed by alternately arranging inorganic layers and organic layers in parallel with the surface of the substrate in the c-axis direction. By analyzing the positions of the diffraction peaks, it was confirmed that the interlayer distance between the inorganic layers was about
As can be seen from FIG. 2, prepared according to the invention (PEA)2PbI4Thin perovskiteThe luminous center wavelength of the film is positioned near 523nm, the peak shape is symmetrical and sharp, and the full-height half-peak width is narrow and is about 19 nm.
As can be seen in FIG. 3, the UV-VIS absorption spectrum of the film shows that the 2D perovskite film has a continuous absorption edge at 521nm, which is located at approximately the same emission center wavelength as the fluorescence spectrum.
As can be seen from FIG. 4, the light under 365nm ultraviolet lamp (PEA) was observed by an optical microscope2PbI4The perovskite thin film can be clearly seen to be formed by a plurality of flaky crystals, and the thin film is green under the excitation of an ultraviolet lamp.
As can be seen from fig. 5, under the observation by a Scanning Electron Microscope (SEM), it was more accurately verified that the entire film was composed of many plate-like crystals. The size of the single flaky crystal is about 0.15mm, the flatness of the surface of the crystal is high, and the coverage rate of the flaky crystal under a visual field reaches 85%.
Example 2
A preparation method of an organic-inorganic hybrid perovskite thin film specifically comprises the following steps:
(1) firstly according to PbI20.461g and 0.498g of PEAI are weighed out in a ratio of 1:2, and added to 1mL of gamma-butyrolactone solvent in sequence, and stirred for 10-20min to make PbI2And PEAI are completely dissolved in gamma-butyrolactone, and after full reaction, a yellow transparent precursor solution with the concentration of 1mol/L is generated;
(2) and (2) dropwise adding a small amount of the perovskite precursor solution prepared in the step (1) on a common glass substrate which is sequentially cleaned by ethanol and gamma-butyrolactone. The initial spin-coating speed is 500rpm, after 90 seconds of spin-coating, the spin-coating speed is increased to 800-1000rpm, the spin-coating is continued for 120 seconds, then the spin-coating speed is gradually increased to 2000rpm, and the spin-coating is continued for 60 seconds. After that, the spin coating speed is reduced until the speed is zero, and the spin coating is finished to obtain (PEA)2PbI4A perovskite thin film.
Example 3
A preparation method of organic-inorganic hybrid perovskite and a thin film thereof comprises the following steps:
(1) firstly according to PbI2:P0.2305g and 0.249g of EAI are weighed respectively in a proportion of 1:2 and are sequentially added into 1mL of gamma-butyrolactone solution, the mixture is fully stirred for 10-20min, and PbI is added2And PEAI is completely dissolved in the gamma-butyrolactone solution and exists uniformly in an ionic form, and when the concentration of the precursor solution is reduced, the solution gradually shows faint yellow and is slightly viscous;
(2) dropwise adding the perovskite precursor solution prepared in the step (1) on a common glass substrate which is cleaned by ethanol and gamma-butyrolactone in sequence, wherein the initial spin-coating rotation speed is 500rpm, after 90 seconds of spin-coating, increasing the spin-coating rotation speed to 800-1000rpm, continuing to spin-coat for 120 seconds, then increasing the spin-coating speed to 2000rpm again, after 60 seconds of spin-coating, gradually reducing the spin-coating speed until the speed is zero, and after the spin-coating is finished, obtaining (PEA)2PbI4A perovskite thin film.
Example 4
Firstly according to PbI20.461g and 0.498g of PEAI are weighed out in a ratio of 1:2, and added to 1mL of DMF in sequence, and stirred for 10-20min to lead PbI2Completely reacting with PEAI to form a yellow transparent slightly viscous precursor solution with the concentration of 1 mol/L; and dripping the precursor solution on a cleaned common glass substrate. Setting the initial spin-coating rotation speed at 500rpm, after 90 seconds of spin-coating, increasing the spin-coating rotation speed to 800-1000rpm, continuing spin-coating for 120 seconds, gradually seeing that yellow crystals on the film substrate begin to precipitate in the process, then increasing the spin-coating speed to 2000rpm again, after 60 seconds of spin-coating, gradually reducing the spin-coating speed until the speed is zero, and after the spin-coating is finished, obtaining (PEA)2PbI4A perovskite thin film.
Example 5
Firstly according to PbI20.461g and 0.498g of PEAI in a ratio of 1:2 were weighed out, and added to 1mL of DMSO in this order, stirred, and PbI was dissolved in a solution method2And PEAI are completely reacted and dissolved, and the concentration of the solution is 1 mol/L; and dropwise adding the prepared perovskite precursor solution on a cleaned common glass substrate. Spin coating the precursor solution on a substrate using spin coating, the spin coating process being the same as in example 4, and evaporation of the solvent to obtain (PEA)2PbI4A perovskite thin film.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of an organic-inorganic hybrid perovskite thin film is characterized by comprising the following steps:
firstly, mixing PbI2Sequentially adding the powder and PEAI powder into solvent, stirring to dissolve completely to obtain (PEA)2PbI4A perovskite precursor solution;
then, the Prepared (PEA)2PbI4The perovskite precursor solution was dropped on the base material, and (PEA) was applied using a spin coating method2PbI4Coating perovskite precursor solution uniformly, and evaporating solvent by natural drying to obtain (PEA)2PbI4Organic-inorganic hybrid perovskite thin films.
2. The method according to claim 1, wherein the solvent is a polar solvent, and comprises N, N-dimethylformamide, γ -butyrolactone or dimethyl sulfoxide.
3. The method for preparing an organic-inorganic hybrid perovskite thin film as claimed in claim 1, wherein (PEA)2PbI4PbI in perovskite precursor solution2And PEAI concentrations of 0.8-1.2mol/L and 1.6-2.4mol/L, respectively.
4. The method for preparing an organic-inorganic hybrid perovskite thin film as claimed in claim 1 or 3, wherein PbI is used2And amount of PEAI materialThe ratio is 1: 2.
5. The method for preparing an organic-inorganic hybrid perovskite thin film as claimed in claim 1, wherein the stirring time is 10-20 min.
6. The method for preparing an organic-inorganic hybrid perovskite thin film according to claim 1, wherein the substrate material comprises common glass, ITO glass, FTO glass or sapphire.
7. The method for preparing an organic-inorganic hybrid perovskite thin film as claimed in claim 1, wherein the substrate material is a cleaned substrate material.
8. The method for preparing an organic-inorganic hybrid perovskite thin film according to claim 7, wherein the cleaning process specifically comprises: firstly, cleaning a substrate material by using ethanol, and then, cleaning for the second time by using a polar solvent used for preparing a precursor solution.
9. The method for preparing an organic-inorganic hybrid perovskite thin film according to claim 1, wherein the spin coating method comprises the following specific steps: firstly, spin-coating for 1-2min at a low rotation speed, then adjusting the rotation speed to a medium rotation speed, wherein the spin-coating time is 2-3min, and finally, spin-coating for 1min at a high rotation speed.
10. The method for preparing an organic-inorganic hybrid perovskite thin film as claimed in claim 9, wherein the low rotation speed is not higher than 500rpm, the medium rotation speed is 800-1000rpm, and the high rotation speed is 2000 rpm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114784050A (en) * | 2022-06-17 | 2022-07-22 | 湖南大学 | Neuromorphic vision sensor and application and preparation method thereof |
| CN117500343A (en) * | 2023-10-31 | 2024-02-02 | 山东省科学院自动化研究所 | Preparation method of organic-inorganic hybrid perovskite film for controlling luminescence wavelength |
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2021
- 2021-12-29 CN CN202111633103.8A patent/CN114373864A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114784050A (en) * | 2022-06-17 | 2022-07-22 | 湖南大学 | Neuromorphic vision sensor and application and preparation method thereof |
| CN114784050B (en) * | 2022-06-17 | 2022-09-27 | 湖南大学 | Neuromorphic vision sensor and application and preparation method thereof |
| CN117500343A (en) * | 2023-10-31 | 2024-02-02 | 山东省科学院自动化研究所 | Preparation method of organic-inorganic hybrid perovskite film for controlling luminescence wavelength |
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