Preparation method of perovskite film
By constructing a functional layer of tin dioxide on the surface of ITO glass and building a perovskite layer based on the MAPbI3 system and performing annealing treatment, the challenges of large-area uniformity and high crystallization quality in the prior art are solved, and efficient and economical perovskite film preparation is achieved.
Patent Information
- Application Number
- CN202510217425.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-26
- Publication Date
- 2025-05-16
AI Technical Summary
The existing perovskite film preparation technology has challenges in large-area uniformity and high crystallization quality, and the equipment costs are high and the process is complex, making it difficult to achieve large-scale production.
A tin dioxide functional layer was constructed on the surface of the initial ITO glass by plasma treatment, and a perovskite layer was constructed on the surface of the functional layer based on the MAPbI3 system, and then annealed to optimize the film structure.
The preparation process of perovskite film is significantly simplified, the equipment cost and process difficulty are reduced, the film uniformity and quality are improved, and it is suitable for the large-scale production of high-performance MAPbI3 perovskite X-ray plane array detectors.
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Figure CN120018743A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the field of material science and engineering technology, and in particular to a method for preparing a perovskite film. Background Art
[0002] Currently, perovskite materials such as MAPbI 3 ) has become a research hotspot, mainly including spin coating, vacuum evaporation, printing, solution dip coating and spraying. Among them, the spin coating method uses a spin coating device to evenly coat the precursor liquid on the surface of the substrate, and then forms a thin film by temperature control crystallization. This method is widely used because of its strong controllability, but there are limitations on large-area uniformity. The vacuum evaporation method evaporates the precursor material and deposits it on the substrate in a vacuum environment, which can achieve high film quality and uniformity, but the equipment cost is high and the process is complicated. The printing method includes inkjet printing and scraping, which can be used to prepare perovskite films on a large area, but it has high requirements on the accuracy of the equipment and the density of the film. The solution dip coating method forms a thin film by immersing the substrate in the precursor liquid and then pulling it up. The operation is simple, but the repeatability is poor, and it is difficult to control the film thickness. In recent years, the spray coating method has begun to attract attention because it is suitable for large-area preparation, but the current spray coating technology has strict requirements on parameter control and there are challenges in high uniformity and high crystal quality.
[0003] However, the existing technologies have many disadvantages. The spin coating method is suitable for the preparation of small-area thin films, but it is difficult to meet the needs of large-area array detectors, and it is easy to form uneven film thickness in the edge area, and a large amount of precursor liquid is wasted, which is costly. The vacuum evaporation method has expensive equipment, high energy consumption, complex process, high maintenance cost, and is difficult to achieve large-scale production, and the yield is low. The printing method has high requirements on equipment accuracy and material rheology, and the quality of thin film crystallization is limited, which may lead to poor detection performance, and it is easy to produce pinholes and unevenness. The solution dip coating method is difficult to accurately control the film thickness, resulting in poor repeatability, material waste during the coating process, and low preparation efficiency. The traditional spray coating method has strict requirements on parameter control, and it is difficult to balance uniformity and density. Defects such as voids and cracks may appear during the film preparation process, affecting the detection performance. In addition, the crystal growth process is easily disturbed by environmental factors (such as humidity, temperature, etc.), affecting stability and performance. At present, there is no appropriate method to solve the above problems. Therefore, it is necessary to propose a method for preparing perovskite film to at least solve some of the above problems. Summary of the invention
[0004] A series of simplified concepts are introduced in the Summary of the Invention section, which will be further described in detail in the Detailed Description of the Invention section. The Summary of the Invention section of this application does not mean to attempt to define the key features and essential technical features of the claimed technical solution, nor does it mean to attempt to determine the scope of protection of the claimed technical solution.
[0005] In a first aspect, an embodiment of the present application provides a method for preparing a perovskite film, the method comprising:
[0006] Pre-treating the initial ITO glass to obtain the target ITO glass;
[0007] constructing a tin dioxide functional layer on the surface of the target ITO glass based on a plasma treatment method to obtain a target thin film;
[0008] Based on MAPbI 3 The system constructs a perovskite layer on the surface of the target film to obtain an initial perovskite film;
[0009] The initial perovskite film is annealed to obtain a target perovskite film.
[0010] In one embodiment of the present invention, the step of pre-treating the initial ITO glass to obtain the target ITO glass comprises:
[0011] Ultrasonic cleaning of the initial ITO glass using deionized water and detergent for a first preset time to obtain a first ITO glass;
[0012] Rinse the first ITO glass with deionized water to obtain a second ITO glass;
[0013] Immersing the second ITO glass in acetone and performing ultrasonic treatment for a second preset time to obtain a third ITO glass;
[0014] The third ITO glass is rinsed with deionized water and then placed in anhydrous ethanol to obtain a fourth ITO glass;
[0015] After the fourth ITO glass was dried using a nitrogen gun, the target ITO glass was obtained.
[0016] In one embodiment of the present invention, the step of constructing a tin dioxide functional layer on the surface of the target ITO glass based on a plasma treatment method to obtain a target thin film comprises:
[0017] Processing the target ITO glass within a third preset time based on a plasma treatment method to obtain an ITO glass;
[0018] Spin coating a water-dispersed solution of tin dioxide on the surface of the ITO glass to obtain a tin dioxide film;
[0019] The tin dioxide film is placed on a hot stage at a first preset temperature for annealing to construct a tin dioxide functional layer and obtain a target film.
[0020] In one embodiment of the present invention, the MAPbI-based 3 The system constructs a perovskite layer on the surface of the target film to obtain an initial perovskite film, comprising:
[0021] Based on MAPbI 3 The system obtains MAPbI of preset quality 3 Perovskite raw materials;
[0022] The MAPbI 3 The perovskite raw material was placed in DMF solvent and stirred to dissolve to obtain MAPbI 3 Precursor solution;
[0023] The target film is placed on a hot stage at a second preset temperature, and a preset volume of MAPbI is heated by nitrogen gas while the temperature of the target film is constant. 3 The precursor solution is sprayed onto the surface of the target film to obtain an initial perovskite film.
[0024] In one embodiment of the present invention, the step of annealing the initial perovskite film to obtain the target perovskite film comprises:
[0025] The initial perovskite film is moved into an air glove box with a preset humidity, and annealed at a third preset temperature and a fourth preset time to obtain a target perovskite film.
[0026] In one embodiment of the present invention, the first preset time is 25 minutes to 30 minutes, and the second preset time is 25 minutes to 30 minutes.
[0027] In one embodiment of the present invention, the third preset time is 4 minutes to 5 minutes.
[0028] In one embodiment of the present invention, the first preset temperature is 150°C.
[0029] In one embodiment of the present invention, the MAPbI 3 The perovskite raw material was placed in DMF solvent and stirred to dissolve to obtain MAPbI 3 The steps of the precursor solution include:
[0030] The MAPbI 3 The perovskite raw material is placed in a DMF solvent and dissolved to obtain an initial solution;
[0031] The initial solution was placed in a magnetic stirrer and stirred for 5-6 hours to obtain MAPbI 3 Precursor solution.
[0032] In one embodiment of the present invention, the second preset temperature is 110°C.
[0033] In summary, a method for preparing a perovskite film according to an embodiment of the present application is provided by using MAPbI 3 The system constructs a perovskite layer on the surface of the target film, specifically, nitrogen is used as a carrier gas to carry MAPbI 3 The precursor solution is sprayed onto the surface of the target film, which significantly simplifies the preparation process of the perovskite film. This process breaks away from the reliance of traditional technology on complex environmental control, greatly reduces equipment costs and process difficulty, while ensuring the uniformity and quality of the film.
[0034] In addition, during the spraying process, the target film is placed on a hot stage at 110°C, which allows the target film to be continuously heated to 90°C and maintained at a constant temperature. Through simultaneous spraying and heating operations, the target film can achieve rapid crystallization during the spraying process, effectively improving the density and uniformity of the perovskite film. This process design not only shortens the preparation time, but also significantly improves the optoelectronic performance and stability of the film. The spraying method of this application can continuously and uniformly prepare high-quality MAPbI on a large-area substrate. 3 The thin film effectively solves the limitations of spin coating in large-area preparation and avoids the common thin film defects in traditional technologies, such as pinholes and cracks. By simplifying equipment requirements, reducing material waste, and improving production efficiency, the economy and industrial applicability of the process are significantly improved, which is especially suitable for large-scale production of high-performance MAPbI 3 Perovskite X-ray array detector.
[0035] The method for preparing the perovskite film proposed in the present application, and other advantages, objectives and features of the present application will be partially reflected through the following description, and will also be partially understood by technicians in this field through research and practice of the present application. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] Various other advantages and benefits will become apparent to those of ordinary skill in the art by reading the detailed description of the preferred embodiments below. The accompanying drawings are only for the purpose of illustrating the preferred embodiments and are not to be considered as limiting the present specification. Also, the same reference symbols are used throughout the accompanying drawings to represent the same components. In the accompanying drawings:
[0037] Figure 1 A schematic diagram of a process for preparing a perovskite film provided in an embodiment of the present application;
[0038] Figure 2A schematic diagram of the process of pre-treating initial ITO glass in a method for preparing a perovskite film provided in an embodiment of the present application;
[0039] Figure 3 A schematic diagram of the process of constructing a tin dioxide functional layer in a method for preparing a perovskite film provided in an embodiment of the present application. DETAILED DESCRIPTION
[0040] In order to better understand the technical solutions provided by the embodiments of this specification, the technical solutions of the embodiments of this specification are described in detail below through the accompanying drawings and specific embodiments. It should be understood that the embodiments of this specification and the specific features in the embodiments are detailed descriptions of the technical solutions of the embodiments of this specification, rather than limitations on the technical solutions of this specification. In the absence of conflict, the embodiments of this specification and the technical features in the embodiments can be combined with each other.
[0041] In this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements includes not only those elements, but also includes other elements not explicitly listed, or also includes elements inherent to such process, method, article or equipment. In the absence of more restrictions, the elements limited by the statement "comprise one..." do not exclude the existence of other identical elements in the process, method, article or equipment including the elements. The term "more than two" includes two or more than two situations.
[0042] See also Figure 1 , is a schematic diagram of a process for preparing a perovskite film provided in an embodiment of the present application, which may specifically include:
[0043] S110, pre-treating the initial ITO glass to obtain the target ITO glass.
[0044] For example, ITO glass is indium tin oxide (ITO) coated glass. During the production, storage and transportation of the initial ITO glass, various pollutants such as dust, grease, organic residues, etc. may adhere to its surface. These pollutants will affect the interface performance between the ITO glass and the subsequently deposited or grown materials, and thus affect the performance of the entire device. For example, pollutants may cause the adhesion of materials on the surface of the ITO glass to deteriorate, or hinder charge transfer, etc. Therefore, the initial ITO glass needs to be pretreated to improve its surface properties to meet specific experimental or production requirements.
[0045] S120, constructing a tin dioxide functional layer on the surface of the target ITO glass based on a plasma treatment method to obtain a target thin film.
[0046] For example, the plasma treatment method is a method of treating materials using the characteristics of plasma. Using the plasma treatment method, a tin dioxide functional layer is successfully constructed on the pre-treated target ITO glass surface, and finally a target film that meets specific application requirements is obtained.
[0047] S130, based on MAPbI 3 The system constructs a perovskite layer on the surface of the target film to obtain an initial perovskite film.
[0048] For example, MAPbI 3 The Chinese name is lead iodide methylamine, which is a typical organic-inorganic hybrid perovskite material with a chemical formula of CH 3 NH 3 PbI 3 Among them, CH 3 NH 3 + (methylamine cation), Pb 2+ (lead ion) and I - (iodine ions) together form the perovskite structure. Based on MAPbI 3 The system means that the entire construction process is based on MAPbI 3 This material is the basis for related material preparation and process operations. 3 The system constructs a perovskite layer on the surface of the target film. After successfully constructing the perovskite layer on the surface of the target film, the obtained product is the initial perovskite film.
[0049] S140, annealing the initial perovskite film to obtain a target perovskite film.
[0050] For example, although the initial perovskite film has a basic perovskite structure, there may be some defects or undesirable conditions in terms of crystal structure integrity, internal stress distribution, and bonding between the film layer and the substrate. For example, during the preparation process, due to factors such as rapid evaporation of solvents and incomplete reaction of precursors, the initial perovskite film may have some amorphous regions, uneven crystal particle size, and many grain boundary defects, which will affect the performance of the perovskite film and therefore require further processing and optimization. After annealing, the initial perovskite film is optimized and improved in terms of crystal structure, internal stress, and interface properties, thereby obtaining a perovskite film that meets specific performance requirements, i.e., the target perovskite film.
[0051] In summary, the method for preparing the perovskite film proposed in the embodiment of the present application is to prepare the perovskite film by MAPbI 3 The system constructs a perovskite layer on the surface of the target film, specifically, nitrogen is used as a carrier gas to carry MAPbI 3 The precursor solution is sprayed onto the surface of the target film, which significantly simplifies the preparation process of the perovskite film. This process breaks away from the reliance of traditional technology on complex environmental control, greatly reduces equipment costs and process difficulty, while ensuring the uniformity and quality of the film.
[0052] In addition, during the spraying process, the target film is placed on a hot stage at 110°C, which allows the target film to be continuously heated to 90°C and maintained at a constant temperature. Through simultaneous spraying and heating operations, the target film can achieve rapid crystallization during the spraying process, effectively improving the density and uniformity of the perovskite film. This process design not only shortens the preparation time, but also significantly improves the optoelectronic performance and stability of the film. The spraying method of this application can continuously and uniformly prepare high-quality MAPbI on a large-area substrate. 3 The thin film effectively solves the limitations of spin coating in large-area preparation and avoids the common thin film defects in traditional technologies, such as pinholes and cracks. By simplifying equipment requirements, reducing material waste, and improving production efficiency, the economy and industrial applicability of the process are significantly improved, which is especially suitable for large-scale production of high-performance MAPbI 3 Perovskite X-ray array detector.
[0053] In some examples, the step of pre-treating the initial ITO glass to obtain the target ITO glass includes:
[0054] S111, ultrasonically cleaning the initial ITO glass with deionized water and detergent within a first preset time to obtain a first ITO glass;
[0055] S112, rinsing the first ITO glass with deionized water to obtain a second ITO glass;
[0056] S113, immersing the second ITO glass in acetone and performing ultrasonic treatment for a second preset time to obtain a third ITO glass;
[0057] S114, rinsing the third ITO glass with deionized water and placing it in anhydrous ethanol to obtain a fourth ITO glass;
[0058] S115, drying the fourth ITO glass using a nitrogen gun to obtain a target ITO glass.
[0059] For example, Figure 2As shown, it is a schematic diagram of the process of pre-treating the initial ITO glass in the preparation method of the perovskite film proposed in the present application. The initial ITO glass is placed on a glass cleaning rack, deionized water and an appropriate amount of detergent are added, and the initial ITO glass is ultrasonically cleaned within a first preset time to obtain a first ITO glass; then the first ITO glass is rinsed with deionized water to obtain a second ITO glass; then the second ITO glass is immersed in acetone and ultrasonically treated within a second preset time to obtain a third ITO glass, and then the third ITO glass is rinsed with deionized water and placed in anhydrous ethanol for standby use to obtain a fourth ITO glass. The fourth ITO glass is taken out and blown dry with a nitrogen gun to obtain the target ITO glass.
[0060] In some examples, the step of constructing a tin dioxide functional layer on the surface of the target ITO glass based on a plasma treatment method to obtain a target thin film includes:
[0061] S121, treating the target ITO glass within a third preset time based on a plasma treatment method to obtain an ITO glass;
[0062] S122, spin coating a water-dispersed solution of tin dioxide on the surface of the ITO glass to obtain a tin dioxide film;
[0063] S123, placing the tin dioxide film on a hot plate at a first preset temperature for annealing to construct a tin dioxide functional layer and obtain a target film.
[0064] For example, Figure 3 As shown, this is a schematic diagram of the process of constructing a tin dioxide functional layer in a method for preparing a perovskite film proposed in this application. The target ITO glass is treated with Plasma (plasma treatment method) within a third preset time to obtain ITO glass. Plasma is a highly ionized gas state composed of ions, electrons and neutral particles. The use of plasma to treat ITO glass is based on the interaction between active particles (such as ions, free radicals, etc.) in the plasma and the surface of the ITO glass. This interaction can change the chemical composition and physical properties of the glass surface, thereby achieving the purpose of cleaning the surface and removing pollutants and impurities.
[0065] Then, SnO was spin-coated on the surface of the ITO glass. 2 (tin dioxide) aqueous dispersion to obtain a tin dioxide film, specifically: an appropriate amount of SnO 2The water-dispersed solution is dripped onto the surface of the ITO glass treated with plasma, and then the glass substrate is rotated at high speed. Under the action of centrifugal force, the solution is evenly spread on the glass surface to form a thin film, which is a tin dioxide film. By accurately controlling the rotation speed, time and other parameters of the spin coating, the thickness and uniformity of the formed film can be accurately controlled. The tin dioxide film after spin coating is placed on a hot plate at a first preset temperature and annealed for 1 hour for use to construct a tin dioxide functional layer and obtain the target film. In this process, the heat energy causes the SnO 2 The atoms inside the film gain enough energy to migrate and rearrange, making the crystal structure of the target film more complete and orderly. Annealing can completely evaporate the water, ensure the chemical composition of the target film is pure, and avoid the adverse effects of residual solvents on the performance of the target film.
[0066] In some examples, the MAPbI-based 3 The system constructs a perovskite layer on the surface of the target film to obtain an initial perovskite film, comprising:
[0067] Based on MAPbI 3 The system obtains MAPbI of preset quality 3 Perovskite raw materials;
[0068] The MAPbI 3 The perovskite raw material was placed in DMF solvent and stirred to dissolve to obtain MAPbI 3 Precursor solution;
[0069] The target film is placed on a hot stage at a second preset temperature, and a preset volume of MAPbI is heated by nitrogen gas while the temperature of the target film is constant. 3 The precursor solution is sprayed onto the surface of the target film to obtain an initial perovskite film.
[0070] For example, the perovskite layer is made of MAPbI 3 (methylammonium lead iodide) system, first weigh a preset volume of MAPbI 3 Perovskite raw materials (methylammonium iodide (MAI) and lead iodide (PbI 2 ), wherein the preset volume is 1M (indicating that the molar concentration of the solution is 1 mol per liter), and then DMF (N, N-dimethylformamide) solvent is added and the whole is placed on a magnetic stirrer at 60°C and stirred for 5-6 hours for use. 2 The ITO glass was placed on the second hot stage with preset temperature. After the temperature was constant, 2 ml of MAPbI was taken with a pipette. 3Add the precursor solution to the spray gun, open the nitrogen valve and adjust the flow meter to 0.5L / min. After each spraying (one spraying area covers the entire substrate), stop for 30 seconds until 2mlMAPbI 3 The precursor solution is exhausted and the initial perovskite film is obtained.
[0071] N, N-dimethylformamide (DMF) is a commonly used organic solvent for the synthesis of MAI and PbI 2 It has good solubility. It can fully dissolve the two raw materials to form a uniform solution system. In addition, DMF has a high boiling point and is not easy to evaporate quickly during subsequent operations, which helps to maintain the stability of the solution. Stirring at 60°C improves the activity of the molecules and accelerates the reaction of MAI and PbI 2 The dissolution process in DMF; on the other hand, the appropriate temperature helps the raw materials to fully react chemically to form a stable MAPbI 3 Precursor solution. Magnetic stirring can fully mix the molecules in the solution to ensure that the solution composition is uniform. 5-6 hours of stirring time can ensure that the raw materials are fully dissolved and reacted to form a stable and uniform MAPbI 3 The precursor solution provides a guarantee for the subsequent preparation of high-quality perovskite films. 3 The precursor solution is sprayed onto the surface of the target film, which significantly simplifies the preparation process of the perovskite film. This process breaks away from the reliance of traditional technology on complex environmental control, greatly reduces equipment costs and process difficulty, while ensuring the uniformity and quality of the film.
[0072] In some examples, the step of annealing the initial perovskite film to obtain a target perovskite film includes:
[0073] The initial perovskite film is moved into an air glove box with a preset humidity, and annealed at a third preset temperature and a fourth preset time to obtain a target perovskite film.
[0074] Exemplarily, the target perovskite film can be obtained by moving the initial perovskite film into an air glove box with a preset humidity and annealing it at a third preset temperature and a fourth preset time. Wherein, the preset humidity is RH=0%, the third preset temperature is 110°C and the fourth preset time is 25min-30min. Placing it in an environment with a humidity of 0% can prevent the perovskite film from being damaged by the intrusion of moisture during the annealing process, thereby ensuring the chemical stability and structural integrity of the material. The atoms inside the target perovskite film obtained at the third preset temperature have sufficient energy to migrate and rearrange. On the one hand, it helps to eliminate the internal stress introduced during the preparation process and make the crystal structure more regular and orderly; on the other hand, the appropriate temperature can promote the further growth and improvement of the perovskite crystals and improve the crystallization quality of the crystals. By placing the prepared MAPbI 3 The whole film was annealed at 110°C for 30 minutes in an air glove box with humidity RH = 0%, which can effectively optimize the crystal structure of the perovskite film, improve its crystal quality, and avoid the influence of adverse factors such as moisture.
[0075] In some examples, the first preset time is 25 minutes to 30 minutes, and the second preset time is 25 minutes to 30 minutes.
[0076] Exemplarily, the first preset time is 25 minutes to 30 minutes. Ultrasonic cleaning uses the cavitation effect generated when ultrasonic waves propagate in liquid. Ultrasonic waves generate a large number of tiny bubbles in the cleaning liquid. These bubbles quickly form and burst near the initial ITO glass surface, generating a strong impact force, which can more efficiently peel off the contaminants from the glass surface and achieve the purpose of deep cleaning. A cleaning time of 30 minutes can ensure the full removal of common contaminants.
[0077] The second preset time is 25 minutes to 30 minutes. The cavitation effect of ultrasound is used again to enhance the dissolution and removal effect of acetone on organic matter. Under the action of ultrasound for 30 minutes, the contact between acetone and the surface of the second ITO glass is more complete, and the organic matter can be dissolved and removed more quickly and effectively, further improving the cleanliness of the surface of the third ITO glass.
[0078] In some examples, the third preset time is 4 minutes to 5 minutes.
[0079] Exemplarily, the third preset time is 4 minutes to 5 minutes. Plasma is a high-energy state substance containing a large number of ions, electrons and active free radicals. When the target ITO glass is exposed to a plasma environment, the active particles in the plasma interact with the target ITO glass surface. This effect can change the chemical composition and structure of the target ITO surface at a microscopic level, and introduce some hydrophilic groups (such as hydroxyl groups, etc.) on the target ITO surface, thereby significantly improving the hydrophilicity of the ITO glass. Improving hydrophilicity is very important for subsequent operations such as coating and coating on the ITO glass surface, which can improve the adhesion and spreadability of the material on the ITO glass surface, help to form a uniform, high-quality film or coating, and thus improve the performance of the entire optoelectronic device. A processing time of 5 minutes can ensure that the hydrophilicity is effectively improved while avoiding excessive treatment to damage the ITO glass surface.
[0080] In some examples, the first preset temperature is 150°C.
[0081] For example, annealing is a common process in material processing. 2 The film was placed on a hot plate and heated to 150°C for 1 hour. During this process, the heat energy causes SnO 2 The atoms inside the film gain enough energy to migrate and rearrange.
[0082] In some examples, the MAPbI 3 The perovskite raw material was placed in DMF solvent and stirred to dissolve to obtain MAPbI 3 The steps of the precursor solution include:
[0083] The MAPbI 3 The perovskite raw material is placed in a DMF solvent and dissolved to obtain an initial solution;
[0084] The initial solution was placed in a magnetic stirrer and stirred for 5-6 hours to obtain MAPbI 3 Precursor solution.
[0085] For example, MAPbI 3 The perovskite raw material is dissolved in DMF solvent to obtain an initial solution. Using DMF as a solvent can make MAPbI 3 The perovskite raw materials are fully dissolved to form a uniform solution system. This is an important prerequisite for the subsequent preparation of high-quality thin films or other material forms. Only when the raw materials are completely dissolved can they be evenly distributed in the subsequent processes to ensure the consistency of material properties. The initial solution is placed in a magnetic stirrer and stirred for 5-6 hours to obtain MAPbI 3Precursor solution. Use a magnetic stirrer to stir the initial solution, the main function is to make the various components in the solution fully mixed. 5-6 hours of stirring can ensure that MAPbI 3 The perovskite raw materials are uniformly dispersed at the molecular level in DMF solvent.
[0086] In some examples, the second preset temperature is 110°C.
[0087] For example, SnO 2 The target film is placed on a hot stage and heated to 110°C, which has an important influence on the nucleation and growth process of the perovskite film, can control the growth rate and orientation of the crystal, and helps to form a uniform, dense perovskite film with a good crystalline structure.
[0088] It should be noted that in the above embodiments, the description of each embodiment has its own emphasis, and for parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.
[0089] Those skilled in the art can clearly understand that, for the convenience and brevity of description, the specific working processes of the systems, devices and units described above can refer to the corresponding processes in the aforementioned method embodiments and will not be repeated here.
[0090] In the several embodiments provided in the present application, it should be understood that the disclosed devices, apparatuses and methods can be implemented in other ways. For example, the device embodiments described above are only schematic, for example, the division of units is only a logical function division, and there may be other division methods in actual implementation, such as multiple units or components can be combined or integrated into another system, or some features can be ignored or not executed. Another point is that the mutual coupling or direct coupling or communication connection shown or discussed can be an indirect coupling or communication connection through some interfaces, devices or units, which can be electrical, mechanical or other forms.
[0091] The units described as separate components may or may not be physically separated, and the components shown as units may or may not be physical units, that is, they may be located in one place or distributed on multiple network units. Some or all of the units may be selected according to actual needs to achieve the purpose of the solution of this embodiment.
[0092] In addition, each functional unit in each embodiment of the present application may be integrated into one processing unit, or each unit may exist physically separately, or two or more units may be integrated into one unit. The above-mentioned integrated unit may be implemented in the form of hardware or in the form of software functional units.
[0093] If the integrated unit is implemented in the form of a software functional unit and sold or used as an independent product, it can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of the present application is essentially or the part that contributes to the prior art or all or part of the technical solution can be embodied in the form of a software product, and the computer software product is stored in a storage medium, including a number of instructions to enable a computer device (which can be a personal computer, a server, or a network device, etc.) to perform all or part of the steps of the various embodiments of the present application. The aforementioned storage medium includes: U disk, mobile hard disk, read-only memory (Read-Only Memory, ROM), random access memory (Random Access Memory, RAM), disk or optical disk and other media that can store program codes.
[0094] The above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present application.
[0095] Although the preferred embodiments of this specification have been described, those skilled in the art may make additional changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of this specification.
[0096] Obviously, those skilled in the art can make various changes and modifications to this specification without departing from the spirit and scope of this specification. Thus, if these modifications and variations of this specification fall within the scope of the claims of this specification and their equivalents, this specification is also intended to include these modifications and variations.
Claims
1. A method for preparing a perovskite film, characterized in that: The method comprises: Pre-treating the initial ITO glass to obtain the target ITO glass; constructing a tin dioxide functional layer on the surface of the target ITO glass based on a plasma treatment method to obtain a target thin film; constructing a perovskite layer on the surface of the target film based on the MAPbI3 system to obtain an initial perovskite film; The initial perovskite film is annealed to obtain a target perovskite film.
2. The method for preparing a perovskite film according to claim 1, characterized in that: The step of pre-treating the initial ITO glass to obtain the target ITO glass comprises: Ultrasonic cleaning of the initial ITO glass using deionized water and detergent for a first preset time to obtain a first ITO glass; Rinse the first ITO glass with deionized water to obtain a second ITO glass; Immersing the second ITO glass in acetone and performing ultrasonic treatment for a second preset time to obtain a third ITO glass; The third ITO glass is rinsed with deionized water and then placed in anhydrous ethanol to obtain a fourth ITO glass; After the fourth ITO glass was dried using a nitrogen gun, the target ITO glass was obtained.
3. The method for preparing a perovskite film according to claim 1, characterized in that: The step of constructing a tin dioxide functional layer on the surface of the target ITO glass based on a plasma treatment method to obtain a target film comprises: Processing the target ITO glass within a third preset time based on a plasma treatment method to obtain an ITO glass; Spin coating a water-dispersed solution of tin dioxide on the surface of the ITO glass to obtain a tin dioxide film; The tin dioxide film is placed on a hot stage at a first preset temperature for annealing to construct a tin dioxide functional layer and obtain a target film.
4. The method for preparing a perovskite film according to claim 1, characterized in that: The step of constructing a perovskite layer on the surface of the target film based on the MAPbI3 system to obtain an initial perovskite film comprises: Obtaining MAPbI3 perovskite raw materials of preset quality based on MAPbI3 system; The MAPbI3 perovskite raw material is placed in a DMF solvent and stirred to dissolve to obtain a MAPbI3 precursor solution; The target film is placed on a hot stage at a second preset temperature. When the temperature of the target film is constant, a preset volume of the MAPbI3 precursor solution is sprayed onto the surface of the target film by nitrogen to obtain an initial perovskite film.
5. The method for preparing a perovskite film according to claim 1, characterized in that: The step of annealing the initial perovskite film to obtain a target perovskite film comprises: The initial perovskite film is moved into an air glove box with a preset humidity, and annealed at a third preset temperature and a fourth preset time to obtain a target perovskite film.
6. The method for preparing a perovskite film according to claim 2, characterized in that: The first preset time is 25 minutes to 30 minutes, and the second preset time is 25 minutes to 30 minutes.
7. The method for preparing a perovskite film according to claim 3, characterized in that: The third preset time is 4 minutes to 5 minutes.
8. The method for preparing a perovskite film according to claim 3, characterized in that: The first preset temperature is 150°C.
9. The method for preparing a perovskite film according to claim 4, characterized in that: The step of placing the MAPbI3 perovskite raw material in a DMF solvent and stirring and dissolving it to obtain a MAPbI3 precursor solution comprises: The MAPbI3 perovskite raw material is placed in a DMF solvent for dissolution to obtain an initial solution; The initial solution is placed in a magnetic stirrer and stirred for 5-6 hours to obtain a MAPbI3 precursor solution.
10. The method for preparing a perovskite film according to claim 4, characterized in that: The second preset temperature is 110°C.
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Method for cleaning perovskite surface
CN120920412A