Methods for synthesizing perovskite materials
The synthesis of perovskite materials through one-pot method has solved the problem of mass production of industrial in the existing technology, and achieved efficient and low-cost perovskite materials production, which is suitable for industrial production.
Patent Information
- Application Number
- CN202311046069.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-18
- Publication Date
- 2025-08-19
- Estimated Expiration
- 2043-08-18
AI Technical Summary
The existing perovskite material synthesis methods are not suitable for large-scale industrial production. There are trace impurities in liquid phase synthesis, and there are problems of different proportions and high defect states in gas phase synthesis.
Perovskite materials are synthesized by one-pot method, industrial-grade raw materials are used, and hydrogen, halogen element and organic cationic compounds are reacted under specific conditions to avoid pre-synthesis of intermediate products, and a reaction device is used to achieve large-scale production.
It simplifies production steps, reduces synthesis costs, improves material purity and output, and is suitable for industrial production.
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Figure CN117088778B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of perovskite materials, and in particular to a method for synthesizing perovskite materials. Background Art
[0002] With the commercialization of perovskite solar cells, the ability to synthesize industrial-grade perovskite materials inexpensively and in large quantities is crucial. Currently, laboratory-scale, small-batch synthesis methods primarily include two approaches: 1. Liquid-phase synthesis, where a lead salt is iodinated and reacted in a methylamine solution. After cooling, the perovskite powder crystallizes and is purified and dried to obtain iodine-lead methylamine perovskite powder (CH3NH3PbI3). 2. Vapor-phase synthesis, typically performed through simultaneous chemical vapor deposition (CVD), involves the simultaneous evaporation of lead iodide and methylamine iodide. These react in the gaseous state to produce the perovskite powder, CH3NH3PbI3.
[0003] However, the existing methods are suitable for small-batch synthesis at the laboratory level, and further improvement is needed to adapt to the needs of industrial large-scale synthesis. Summary of the Invention
[0004] The present invention aims to solve at least one of the technical problems in the related art to a certain extent. The existing synthesis methods of perovskite materials are not suitable for industrial amplification to meet the needs of industrial mass synthesis. It is mainly manifested in that: the liquid phase synthesis method usually uses hydroiodic acid to iodinate lead salts and methylamine, and commercial hydroiodic acid usually contains 5% hypophosphorous acid as a stabilizer for HI, which makes it possible for trace amounts of phosphate impurities to exist in the final synthesized product, bringing difficulties in the extraction and storage of the final synthetic product, and increasing the synthesis cost of the material. The gas phase synthesis process usually requires dual-source co-evaporation of PbI2 and MAI. The perovskite powder obtained by the reaction has different proportions and the material has a high defect state. Both synthesis routes generally require the pre-synthesis of MAI and PbI2 as raw materials, which is difficult to adapt to industrial mass production.
[0005] The present invention provides a method for synthesizing perovskite materials and a corresponding device, which directly uses industrial-grade raw materials and directly synthesizes perovskite powder in a one-pot method, avoiding the pre-synthesis of intermediate products and simplifying the production steps.
[0006] Specifically, the present invention provides the following technical solutions:
[0007] A first aspect of the present invention provides a method for synthesizing a perovskite material, comprising:
[0008] Mixing hydrogen, a halogen element, a metal element, and an organic cationic compound, and reacting them under predetermined conditions to obtain a product containing a perovskite material;
[0009] Wherein, the metal element is selected from at least one of lead and tin;
[0010] The organic cationic compound is selected from at least one of methylamine and formamidine.
[0011] The method for synthesizing perovskite materials is applicable not only to MAPbI3, but also to FAPbI3, MAPbBr3, MAPbCl3, FAPbBr3, and FAPbCl3. The corresponding raw materials can be replaced with formamidine gas (FA), bromine vapor (Br2), chlorine gas (Cl2), etc. The method for synthesizing perovskite materials can directly synthesize perovskite powder in a one-pot process, avoiding the need for pre-synthesis of intermediates, simplifying the production process, and making it suitable for industrial production.
[0012] According to an embodiment of the present invention, the above method for synthesizing perovskite materials may further include the following technical features:
[0013] According to an embodiment of the present invention, the step of mixing hydrogen, a halogen element, a metal element, and an organic cationic compound and reacting them under preset conditions to obtain a product containing a perovskite material includes:
[0014] (1) reacting hydrogen and a halogen element in the presence of a catalyst under first reaction conditions to obtain a mixed gas;
[0015] (2) reacting the mixed gas with the organic cationic compound and the metal element under a second reaction condition to obtain a product containing a perovskite material.
[0016] According to an embodiment of the present invention, the temperature of the first reaction condition is 50-600 degrees Celsius and the pressure is normal pressure; the temperature of the second reaction condition is 50-400 degrees Celsius and the pressure is greater than 200 kPa.
[0017] According to an embodiment of the present invention, the molar ratio of the halogen element to the hydrogen is greater than 3:1.
[0018] According to an embodiment of the present invention, the metal element is added in the form of a high-temperature powder, the temperature of the high-temperature powder being greater than 200 degrees Celsius, and the particle size of the high-temperature powder being less than 10 microns. Adding the metal element in the form of a high-temperature powder with a very small particle size, for example, less than 10 microns, results in a faster reaction rate and a more thorough reaction.
[0019] According to an embodiment of the present invention, the method further comprises:
[0020] The obtained product containing the perovskite material is sequentially washed, purified, and dried to obtain the perovskite material. During the washing process, a solvent such as isopropyl alcohol or ethyl acetate can be used for washing, followed by purification and drying to effectively remove impurities and obtain the perovskite material.
[0021] A second aspect of the present invention provides a device for synthesizing a perovskite material, comprising:
[0022] reaction chamber;
[0023] an air intake pipe, connected to the reaction chamber, the air intake pipe comprising a first air intake pipe, a second air intake pipe, a third air intake pipe, and a fourth air intake pipe, each of which is independently connected to the reaction chamber;
[0024] Among them, the first air inlet pipe is used to introduce hydrogen into the reaction chamber, the second air inlet pipe is used to introduce halogen elements into the reaction chamber, the third air inlet pipe is used to introduce organic cationic compounds into the reaction chamber, and the fourth air inlet pipe is used to introduce metal elements into the reaction chamber.
[0025] According to an embodiment of the present invention, the above-mentioned device for synthesizing perovskite materials may further include the following technical features:
[0026] According to an embodiment of the present invention, the reaction chamber includes a first reaction chamber and a second reaction chamber connected by a connecting pipe, the first air inlet pipe and the second air inlet pipe are independently connected to the first reaction chamber, and the third air inlet pipe and the fourth air inlet pipe are independently connected to the second reaction chamber.
[0027] The first reaction chamber contains a uniformly distributed catalyst, and the connecting pipe is used to pass the mixed gas obtained by the reaction in the first reaction chamber into the second reaction chamber.
[0028] According to an embodiment of the present invention, the reaction temperature of the first reaction chamber is 50-600 degrees Celsius, and the pressure is normal pressure; for example, 500 degrees Celsius; the reaction temperature of the second reaction chamber is 50-400 degrees Celsius, for example, 300 degrees Celsius, and the pressure is greater than 200 kPa.
[0029] According to an embodiment of the present invention, the molar ratio of the amount of the halogen element introduced into the second air inlet pipe to the amount of the hydrogen introduced into the first air inlet pipe is greater than 3:1.
[0030] According to an embodiment of the present invention, the method further comprises:
[0031] A purification chamber is connected to the second reaction chamber, and the purification chamber is used to sequentially clean, purify and dry the product obtained by the second reaction chamber to obtain perovskite powder crystals.
[0032] The third aspect of the present invention provides a perovskite material, which is synthesized according to the method of the first aspect of the present invention.
[0033] A fourth aspect of the present invention provides a perovskite solar cell, which includes a perovskite layer, wherein the material of the perovskite layer includes the perovskite material described in the third aspect.
[0034] The beneficial effects achieved by the present invention are:
[0035] In the method for synthesizing perovskite materials provided by the present invention, the reaction raw materials are all raw materials used in industry, and the reaction raw materials are not limited by production capacity. The perovskite powder crystals can be produced in large quantities by a one-pot method, which is particularly suitable for large-scale industrial production.
[0036] The apparatus for synthesizing perovskite materials provided by the present invention can produce perovskite materials in a single-pot reaction, using a reaction chamber and several air inlet pipes connected to the reaction chamber. This eliminates production capacity constraints for the reaction raw materials and makes it more suitable for industrial production. For example, the first and second reaction chambers can be connected to different air inlet pipes, allowing the reaction to proceed more efficiently toward the perovskite product, further improving reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0037] Figure 1 3 is a schematic diagram of a reaction device provided according to an embodiment of the present invention, wherein label 1 is a first reaction chamber; 2 is a second reaction chamber; 3 is a first air inlet pipe for introducing hydrogen; 4 is a second air inlet pipe for introducing a halogen element in gaseous form; 5 is a third air inlet pipe for introducing an organic cationic compound in gaseous form; 6 is a fourth air inlet pipe for introducing a metal element in the form of a high-temperature powder; and 7 is a discharge port.
[0038] Figure 2 1 is an XRD pattern of the perovskite powder provided according to an embodiment of the present invention. DETAILED DESCRIPTION
[0039] The embodiments of the present invention are described in detail below. Examples of the embodiments are shown in the accompanying drawings. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present invention, but should not be understood as limiting the present invention.
[0040] The first aspect of the present invention provides a method for synthesizing a perovskite material, comprising: mixing hydrogen, a halogen element, a metal element, and an organic cationic compound, and reacting them under preset conditions to obtain a product containing the perovskite material; wherein the metal element is selected from at least one of lead and tin; and the organic cationic compound is selected from at least one of methylamine and formamidine.
[0041] The method for synthesizing perovskite materials provided by the present invention can be achieved through a one-pot process. Taking iodine, methylamine and lead as an example, the reaction principle can be summarized as: 2CH3NH2+H2+3I2+2Pb——2CH3NH3PbI3. In order to facilitate the reaction, the reaction raw materials used can be methylamine gas, hydrogen, iodine vapor and ultrafine lead powder (particle size less than 10μm). The raw materials are simple and can be used to synthesize perovskite materials.
[0042] In order to ensure a more complete and rapid reaction, the above-mentioned one-step reaction can be disassembled and divided into two steps. First, hydrogen and halogen elements react under catalyst conditions to obtain hydrogen chloride; then hydrogen halide, metal elements and organic cationic compounds react to obtain a product containing perovskite material. According to a specific embodiment of the present invention, the step of mixing hydrogen, halogen elements, metal elements and organic cationic compounds and reacting them under preset conditions to obtain a product containing perovskite material includes:
[0043] (1) reacting hydrogen gas and a halogen element in the presence of a catalyst under first reaction conditions to obtain hydrogen halide gas;
[0044] (2) reacting the hydrogen halide gas with the organic cationic compound and the metal element under a second reaction condition to obtain a product containing a perovskite material.
[0045] According to a specific embodiment of the present invention, the first reaction condition is a temperature of 30-600 degrees Celsius and a pressure of atmospheric pressure; the second reaction condition is a temperature of 50-400 degrees Celsius and a pressure greater than 200 kPa. The catalysts used include, but are not limited to, platinum, palladium, nickel, cobalt, iron, nickel oxide, cobalt oxide, and iron oxide.
[0046] According to a specific embodiment of the present invention, the halogen element is introduced in the form of a gas, and the molar ratio of the halogen element vapor to the hydrogen gas is at least 3:1. When the molar ratio of the halogen element vapor to the hydrogen gas is at least 3:1, when it is higher than 3:1, the reaction is favored to move toward the formation of hydrogen halide, and the excess unreacted halogen element vapor can continue to participate in subsequent reactions, thereby facilitating the reaction to move toward the formation of perovskite powder.
[0047] According to a specific embodiment of the present invention, the metal element is added in the form of a high-temperature powder, the temperature of the high-temperature powder is greater than 200 degrees Celsius, and the particle size of the high-temperature powder is less than 10 microns. Adding the metal element in the form of a high-temperature powder and at a temperature greater than 200 degrees Celsius ensures the activation energy of the metal element's reaction. If the temperature is insufficient, the activation energy of the metal element's reaction is insufficient, the reaction may be incomplete, and unreacted metal element may be present in the generated product, thereby affecting the quality of the ultimately prepared perovskite material.
[0048] According to a specific embodiment of the present invention, the obtained product containing the perovskite material is sequentially cleaned, purified, and dried to obtain the perovskite material.
[0049] In the process of synthesizing perovskite materials, in order to ensure that the reaction is more sufficient and rapid, the above reaction can be disassembled. Taking iodine, methylamine and lead as an example, the reaction can be disassembled into two steps: H2+I2——2HI; HI+CH3NH2+I2+Pb——CH3NH3PbI3. To this end, according to a specific embodiment of the present invention, a method for synthesizing perovskite materials is provided, which includes: (1) hydrogen and iodine vapor are reacted under first reaction conditions in the presence of a catalyst to obtain a mixed gas, the temperature of the first reaction condition is 50~600 degrees Celsius, and the pressure is atmospheric pressure; (2) the mixed gas is reacted with methylamine gas and high-temperature lead powder under second reaction conditions to obtain a product containing perovskite powder, the temperature of the high-temperature lead powder is greater than 200 degrees Celsius, the temperature of the second reaction condition is 50~400 degrees Celsius, and the pressure is greater than 200kPa. According to a specific embodiment of the present invention, the temperature of the first reaction condition in step (1) is 500 degrees Celsius, and the volume ratio of the iodine vapor to the hydrogen is greater than 3:1.
[0050] The present invention also provides a device for synthesizing perovskite materials, comprising: a reaction chamber;
[0051] an air intake pipe, connected to the reaction chamber, the air intake pipe comprising a first air intake pipe, a second air intake pipe, a third air intake pipe, and a fourth air intake pipe, each of which is independently connected to the reaction chamber;
[0052] Among them, the first air inlet pipe is used to introduce hydrogen into the reaction chamber, the second air inlet pipe is used to introduce halogen elements into the reaction chamber, the third air inlet pipe is used to introduce organic cationic compounds into the reaction chamber, and the fourth air inlet pipe is used to introduce metal elements into the reaction chamber.
[0053] According to a specific embodiment, the present invention also provides an apparatus for synthesizing perovskite materials, comprising: a first reaction chamber, wherein the first reaction chamber is independently connected to the first air inlet pipe and the second air inlet pipe, hydrogen is introduced through the first air inlet pipe, and a halogen element is introduced through the second air inlet pipe (provided in the form of halogen element vapor by controlling the temperature), and the first reaction chamber contains a uniformly distributed catalyst; a second reaction chamber, wherein the first reaction chamber and the second reaction chamber are connected by a connecting pipe, and the connecting pipe is used to pass the mixed gas obtained by the reaction in the first reaction chamber into the second reaction chamber, and the second reaction chamber is independently connected to the third air inlet pipe and the fourth air inlet pipe, wherein an organic cationic compound is introduced through the third air inlet pipe (provided in gaseous form by controlling the temperature), and a metal element in the form of a high-temperature powder is introduced through the fourth air inlet pipe;
[0054] The first reaction chamber and the second reaction chamber are used to generate the following reaction:
[0055] 2CH3NH2+H2+3I2+2Pb——2CH3NH3PbI3.
[0056] The first reaction chamber is a normal pressure reaction chamber, and the second reaction chamber is a high pressure reaction chamber. The provided device can realize the synthesis of perovskite materials through two connected reaction chambers and simple raw materials, meeting the needs of industrial production.
[0057] According to a specific embodiment of the present invention, the reaction temperature of the first reaction chamber is 50-600 degrees Celsius, and the pressure is atmospheric pressure, preferably 500 degrees Celsius. Taking iodine vapor as an example, the first reaction chamber is for the reaction between hydrogen and iodine vapor. This reaction is reversible, and the reaction to produce HI is an exothermic reaction. Increasing the temperature favors the reaction to produce HI. In an isometric reaction, pressure changes will not cause a shift in the reaction equilibrium.
[0058] According to a specific embodiment of the present invention, the temperature of the high-temperature lead powder introduced through the fourth air inlet pipe is greater than 200 degrees Celsius; the reaction temperature of the second reaction chamber is 100-400 degrees Celsius, preferably 300 degrees Celsius, and the pressure is greater than 200 kPa.
[0059] According to a specific embodiment of the present invention, the molar ratio of the amount of the halogen element introduced into the second air inlet pipe to the amount of the hydrogen introduced into the third air inlet pipe is greater than 3:1.
[0060] According to a specific embodiment of the present invention, it further includes:
[0061] A purification chamber is connected to the second reaction chamber, and the purification chamber is used to sequentially clean, purify and dry the product obtained by the second reaction chamber to obtain perovskite crystals.
[0062] The present invention is described below with reference to specific examples. It should be noted that these examples are only used to help those skilled in the art understand and should not be regarded as limiting the scope of protection of the present invention.
[0063] Example 1
[0064] Example 1 The perovskite material was synthesized by the following method, and the reaction principle equation is:
[0065] 2CH3NH2+H2+3I2+2Pb——2CH3NH3PbI3
[0066] (1) hydrogen (through the first air inlet pipe 3) and iodine vapor (through the second air inlet pipe 4) are slowly introduced into the first reaction chamber, wherein the volume ratio of iodine vapor to hydrogen is greater than three to one, the first reaction chamber is a normal pressure reaction chamber, the first reaction chamber contains a uniformly distributed iron oxide catalyst, the reaction temperature is 500°C, and the reaction chamber pressure is 101 kPa at normal pressure;
[0067] (2) The mixed gas after sufficient reaction enters the second reaction chamber, which is a high-pressure reaction chamber with a pressure of 10 MPa and a temperature of 300°C. Methylamine gas is first introduced (through the third air inlet pipe 5) and mixed evenly with the gas from the first reaction chamber. Heated ultrafine lead powder is then sprayed in (through the fourth air inlet pipe 6). The lead powder is heated to 200°C and has a particle size of less than 10 μm. High-temperature lead powder is continuously sprayed in small amounts and multiple times. The high-temperature lead powder reacts with the mixed gas and is converted into perovskite powder, which is collected from the discharge port 7.
[0068] (3) The collected perovskite powder is washed, purified, and dried using isopropyl alcohol and ethyl acetate in sequence to obtain perovskite crystal MAPbI3.
[0069] The XRD patterns of the prepared perovskite crystals are shown in Figure 2. Figure 2 Compared with the standard card of MAPbI3, it can be seen that MAPbI3 powder was synthesized.
[0070] Example 2
[0071] Example 1 The perovskite material was synthesized by the following method, and the reaction principle equation is:
[0072] 2FA+H2+3I2+2Pb——2FAPbI3
[0073] (1) hydrogen (through the first air inlet pipe 3) and iodine vapor (through the second air inlet pipe 4) are slowly introduced into the first reaction chamber, wherein the volume ratio of iodine vapor to hydrogen is greater than three to one, the first reaction chamber is a normal pressure reaction chamber, the first reaction chamber contains a uniformly distributed iron oxide catalyst, the reaction temperature is 500°C, and the reaction chamber pressure is 101 kPa at normal pressure;
[0074] (2) The mixed gas after sufficient reaction enters the second reaction chamber, which is a high-pressure reaction chamber with a pressure of 20 MPa and a temperature of 300°C. First, formamidine gas is introduced (through the third air inlet pipe 5) and mixed evenly with the gas from the first reaction chamber. Then, heated ultrafine lead powder is sprayed in (through the fourth air inlet pipe 6). The lead powder is heated to 200°C and has a particle size of less than 10 μm. High-temperature lead powder is continuously sprayed in small amounts and multiple times. The high-temperature lead powder reacts with the mixed gas and is converted into perovskite powder, which is collected from the discharge port 7.
[0075] (3) The collected perovskite powder is washed, purified, and dried using isopropyl alcohol and ethyl acetate in sequence to obtain perovskite crystal FAPbI3.
[0076] Example 3
[0077] Example 1 The perovskite material was synthesized by the following method, and the reaction principle equation is:
[0078] 2MA+H2+3Br2+2Pb——2MAPbBr3
[0079] (1) hydrogen (through the first air inlet pipe 3) and bromine vapor (through the second air inlet pipe 4) are slowly introduced into the first reaction chamber, wherein the volume ratio of bromine vapor to hydrogen is greater than three to one, the first reaction chamber is a normal pressure reaction chamber, the first reaction chamber contains a uniformly distributed iron oxide catalyst, the reaction temperature is 500°C, and the reaction chamber pressure is 101 kPa at normal pressure;
[0080] (2) The mixed gas after sufficient reaction enters the second reaction chamber, which is a high-pressure reaction chamber with a pressure greater than 200 kPa and a temperature of 300°C. Methylamine gas is first introduced (through the third air inlet pipe 5) and mixed evenly with the gas from the first reaction chamber. Heated ultrafine lead powder is then sprayed in (through the fourth air inlet pipe 6). The lead powder is heated to 200°C and has a particle size of less than 10 μm. High-temperature lead powder is continuously sprayed in small amounts and multiple times. The high-temperature lead powder reacts with the mixed gas and is converted into perovskite powder, which is collected from the discharge port 7.
[0081] (3) The collected perovskite powder is washed, purified, and dried using isopropyl alcohol and ethyl acetate in sequence to obtain perovskite crystal MAPbBr3.
[0082] Example 4
[0083] Example 1 The perovskite material was synthesized by the following method, and the reaction principle equation is:
[0084] 2FA+H2+3Br2+2Pb——2FAPbBr3
[0085] (1) hydrogen (through the first air inlet pipe 3) and bromine vapor (through the second air inlet pipe 4) are slowly introduced into the first reaction chamber, wherein the volume ratio of bromine vapor to hydrogen is greater than three to one, the first reaction chamber is a normal pressure reaction chamber, the first reaction chamber contains a uniformly distributed iron oxide catalyst, the reaction temperature is 500°C, and the reaction chamber pressure is 101 kPa at normal pressure;
[0086] (2) The mixed gas after sufficient reaction enters the second reaction chamber, which is a high-pressure reaction chamber with a pressure greater than 200 kPa and a temperature of 300°C. First, formamidine gas is introduced (through the third air inlet pipe 5) and mixed evenly with the gas from the first reaction chamber. Then, heated ultrafine lead powder is sprayed in (through the fourth air inlet pipe 6). The lead powder is heated to 200°C and has a particle size of less than 10 μm. High-temperature lead powder is continuously sprayed in small amounts and multiple times. The high-temperature lead powder reacts with the mixed gas and is converted into perovskite powder, which is collected from the discharge port 7.
[0087] (3) The collected perovskite powder is washed, purified, and dried using isopropyl alcohol and ethyl acetate in sequence to obtain perovskite crystal FAPbBr3.
[0088] Comparative Example 1
[0089] Comparative Example 1: Perovskite powder was synthesized in a small batch in the laboratory, comprising the following steps:
[0090] (1) stirring the methylamine aqueous solution and the hydroiodic acid solution in an ice-water bath for 24 hours to form a first solution;
[0091] (2) heating lead iodide at 100° C. and dissolving it in a hydroiodic acid solution to form a second solution;
[0092] (3) Slowly adding the first solution into the second solution, black perovskite powder can be seen to be generated, and a large amount of perovskite powder crystals are precipitated during the cooling process;
[0093] (4) Filter, wash, and dry the generated perovskite powder to obtain perovskite powder crystals.
[0094] The comparative example uses a solution method for synthesis. This method presents challenges such as wastewater disposal, difficult reaction chamber cleaning, and high acid corrosion resistance requirements for the entire system. Large-scale industrial synthesis also presents numerous issues, including subsequent equipment cleanup. Furthermore, aqueous solutions of HI acid often contain stabilizers such as hypophosphorous acid, which results in trace amounts of impurities such as phosphate in the final product, contributing to the presence of impurities in the perovskite product.
[0095] The above examples verify that the method for preparing the perovskite material provided by the present invention uses raw materials that are used industrially, is not limited by production capacity, and can produce perovskite powder crystals in large quantities using a one-pot method, making it particularly suitable for large-scale industrial production.
[0096] In the description of this specification, reference to the terms "one embodiment," "some embodiments," "example," "specific example," or "some examples" means that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any appropriate manner in any one or more embodiments or examples. In addition, those skilled in the art may combine and combine different embodiments or examples described in this specification, as well as features of different embodiments or examples, unless they are mutually inconsistent.
[0097] Although the embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and are not to be construed as limitations on the present invention. A person skilled in the art may change, modify, replace and modify the above embodiments within the scope of the present invention.
Claims
1. A method for synthesizing perovskite material, characterized in that: include: mixing hydrogen, a halogen element, a metal element, and at least one of methylamine and formamidine, and reacting them under predetermined conditions to obtain a product containing a perovskite material; The metal element is selected from at least one of lead and tin; the metal element is added in the form of a high-temperature powder, the temperature of the high-temperature powder is greater than 200 degrees Celsius, and the particle size of the high-temperature powder is less than 10 microns; The halogen element is in gaseous form; The step of obtaining a product containing a perovskite material by reacting under preset conditions includes: (1) reacting hydrogen and a halogen element in the presence of a catalyst under first reaction conditions to obtain a mixed gas; (2) reacting the mixed gas with at least one of methylamine and formamidine and a metal element under a second reaction condition to obtain a product containing a perovskite material; Wherein, the temperature of the first reaction condition is 50-600 degrees Celsius and the pressure is normal pressure; the temperature of the second reaction condition is 50-400 degrees Celsius and the pressure is greater than 200 kPa; Wherein, the molar ratio of the halogen element to the hydrogen is greater than 3:
1.
2. The method according to claim 1, characterized in that Further including: The obtained product containing the perovskite material is washed, purified, and dried in sequence to obtain the perovskite material.
Citation Information
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