Method for preparing perovskite solution and method for manufacturing perovskite cell

Abstract

A method for preparing a perovskite solution and a method for manufacturing a perovskite cell. The method for preparing the perovskite solution comprises the following steps: S1, dissolving perovskite powder in an organic solvent to obtain a mixed solution; and S2, carrying out ultrasonic oscillation on the mixed solution obtained in S1 to accelerate dissolution, the ultrasonic oscillation time being 10-30 min, and filling the mixed solution with inert gas during the ultrasonic oscillation process, the filling flow rate of the inert gas being 0-5 L / min, so as to obtain a perovskite solution.

Description

A method for preparing a perovskite solution and a method for preparing a perovskite battery

[0001] This application claims priority to the Chinese patent application filed with the Patent Office of China on September 15, 2023, with application number 202311187895.X, and invention name “A method for preparing a perovskite solution and a method for preparing a perovskite battery”, the entire contents of which are incorporated by reference into this application. Technical Field

[0002] The present application relates to the technical field of perovskite solar cells, and in particular to a method for preparing a perovskite solution and a method for preparing a perovskite cell. Background Art

[0003] The statements herein merely provide background information related to the present application and do not necessarily constitute prior art.

[0004] Solar energy is a highly anticipated new clean energy source, boasting the advantages of abundant resources and low costs. Currently, photovoltaic cells are one of the most efficient ways to convert solar energy into electricity, and single-crystal silicon and polycrystalline silicon solar cells have achieved relatively mature industrialization. In recent years, perovskite / crystalline silicon tandem technology has become a research hotspot in the photovoltaic field, garnering widespread attention. The development of this technology is crucial for improving the photoelectric conversion efficiency of solar cells and reducing manufacturing costs, thereby promoting the further development and application of solar power generation technology. The theoretical effective photoelectric conversion efficiency of crystalline silicon / perovskite tandem solar cells is as high as over 40%, far exceeding that of crystalline silicon solar cells. The basic principle of perovskite / crystalline silicon tandem technology is to stack perovskite and crystalline silicon materials to form a heterojunction. This technology leverages the wide bandgap, high absorption coefficient, and high carrier mobility of the perovskite material with the stability and excellent electron transport properties of the crystalline silicon material to improve the photoelectric conversion efficiency of solar cells.

[0005] Most existing crystalline silicon / perovskite tandem solar cells use ready-to-use perovskite solutions without considering or optimizing their stability. Industrial production requires large batches of perovskite films. Using small, multiple batches of ready-to-use perovskite solutions to prepare perovskite films significantly increases production costs and time. Consequently, industrial production tends to prepare large quantities of perovskite solution at once for batch production of perovskite films over periods ranging from a few days to several months. However, existing perovskite solution formulations exhibit poor long-term stability and typically decay within a few days, resulting in poor perovskite film quality and low device performance. Therefore, a stable perovskite solution formulation suitable for large-scale industrial production is urgently needed.

[0006] Therefore, it is necessary to study a new technical solution to solve the above problems. Application Contents

[0007] The purpose of the embodiments of the present application is to provide a method for preparing a perovskite solution and a method for preparing a perovskite battery, which reduces the escape of solvents in the precursor solution during long-term use by filling an inert gas into the preparation process of the existing perovskite solution, effectively prevents ion aggregation in the precursor solution, and improves the long-term stability of the perovskite solution; and provides a guarantee for the stable output of high-quality and high-yield perovskite films on the production line.

[0008] The technical solution adopted in the embodiment of this application is:

[0009] In a first aspect, a method for preparing a perovskite solution is provided, comprising the following steps:

[0010] S1, dissolving perovskite powder in an organic solvent to obtain a mixed solution;

[0011] S2, using ultrasonic oscillation to accelerate the dissolution of the mixed solution obtained in S1, the ultrasonic oscillation time is 10-30 minutes, and during the ultrasonic oscillation process, the mixed solution is filled with inert gas, and the filling flow rate of the inert gas is 0-5L / min to obtain a perovskite solution.

[0012] In one embodiment, the inert gas is at least one of helium, neon, and argon.

[0013] In one embodiment, the organic solvent is at least one of dimethylformamide (DMF), g-butyrolactone (GBL), dimethyl sulfoxide (DMSO) and N,N-dimethylacetamide (DMA).

[0014] In one embodiment, the organic solvent comprises dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), and the molar ratio of dimethylformamide (DMF) to dimethyl sulfoxide (DMSO) is 8:2;

[0015] After the perovskite powder is placed in the organic solvent, ultrasonic vibration is applied for 30 minutes. During the ultrasonic vibration, argon or neon gas is added to the mixed solution at a flow rate of 2 L / min.

[0016] In one embodiment, the structure of the perovskite powder is ABX.

[0017] In a second aspect, a method for preparing a perovskite battery is provided, comprising the following steps:

[0018] Step 1: providing a silicon substrate, sequentially preparing a substrate back passivation layer and a P-type substrate doping layer on the back side of the silicon substrate, and sequentially preparing a substrate surface passivation layer and an N-type substrate doping layer on the surface of the silicon substrate;

[0019] Step 2: Prepare a first transparent electrode layer on the back side of the P-type base doped layer by magnetron sputtering, which includes:

[0020] Place the substrate sample after step 1 in a magnetron sputtering device, set an IZO target, operate the device at 60W power, run for 1.5h, and the thickness of the first transparent electrode layer is 100nm;

[0021] Step 3: Prepare a first metal electrode layer on the back side of the first transparent electrode layer by evaporation, which includes: placing the substrate sample completed in step 2 on a mask, placing it in the evaporation chamber of the evaporation machine for evaporation, and the thickness of the first metal electrode layer is 200nm;

[0022] Step 4: A tunneling layer is formed on the surface of the N-type substrate doped layer by magnetron sputtering, which includes: placing the substrate sample after step 3 in a magnetron sputtering device, setting an IZO target, operating the device at 60W power, running for 1 hour, and the thickness of the tunneling layer is 40nm;

[0023] Step 5: A hole transport layer is prepared on the surface of the tunneling layer by spin coating, which includes: placing the substrate sample completed in step 4 in a UV-Ozone clean for 15 minutes; coating the surface of the tunneling layer with a hole transport layer dispersion at a spin coating speed of 2000 rpm and a spin coating time of 40 seconds. After the spin coating is completed, the substrate sample is annealed at an annealing temperature of 450°C and an annealing time of 30 minutes. The thickness of the hole transport layer is 20 nm.

[0024] Step 6: preparing a perovskite absorption layer on the surface of the hole transport layer by spin coating, which includes: placing the substrate sample completed in step 5 on the base of a spin coater, taking a perovskite solution to coat the surface of the hole transport layer, the spin coating speed is 3500 rpm, and the spin coating time is 30 seconds;

[0025] After spin coating, the substrate sample was placed on a flash evaporation table with a flash evaporation time of 30 s and a flash evaporation temperature of 30 °C.

[0026] After the flash evaporation, annealing treatment was performed at a temperature of 100°C, an annealing time of 15 min, and a perovskite absorption layer thickness of 500 nm.

[0027] And, the perovskite precursor solution is a perovskite solution prepared by the preparation method of any one of claims 1 to 5;

[0028] Step 7: preparing a passivation layer on the surface of the perovskite absorption layer by evaporation, which includes: weighing a certain amount of propylenediamine iodide and placing it in a crucible, placing the substrate sample completed in step 6 on the mask and evaporating it, and the thickness of the passivation layer is 4nm;

[0029] After the evaporation, the substrate sample was annealed at a temperature of 100°C and an annealing time of 8 min.

[0030] Step 8: preparing an electron transport layer on the surface of the passivation layer by evaporation, which includes: weighing a certain amount of C60 and placing it in a crucible, placing the substrate sample completed in step 7 on the mask and evaporating it, and the thickness of the electron transport layer is 20nm;

[0031] Step nine: preparing a buffer layer on the surface of the electron transport layer by atomic layer deposition, which includes: depositing a buffer layer material on the surface of the electron transport layer by atomic layer deposition equipment;

[0032] Step 10: Preparing a second transparent electrode layer on the surface of the buffer layer by magnetron sputtering, which includes: placing the substrate sample after completing step 9 in a magnetron sputtering device, setting an IZO target, the device operating power is 50W, the operating time is 1 hour, and the thickness of the second transparent electrode layer is 100nm;

[0033] Step 11: preparing a second metal electrode layer on the surface of the second transparent electrode layer by evaporation; which includes:

[0034] Place the substrate sample after step 10 on the mask and place it in the evaporation chamber for evaporation. The thickness of the first metal electrode layer is 100 nm.

[0035] Step 12: Prepare an anti-reflection layer on the surface of the second metal electrode layer by evaporation; it includes: placing the substrate sample completed in step 11 on the mask, placing it in the evaporation chamber for evaporation, and the thickness of the anti-reflection layer is 100nm.

[0036] In one embodiment, in step 3, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, evaporation rate 2.5Å / S, and the first transparent electrode layer is made of metallic silver.

[0037] In one embodiment, in step five, the hole transport layer dispersion is prepared by dissolving 0.05 mol of NiOx powder in 1 ml of ultrapure water and ultrasonically vibrating for 20 minutes.

[0038] In one embodiment, in step five, the amount of the hole transport layer dispersion is 100 ul.

[0039] In one embodiment, in step six, the preparation of the perovskite solution includes: weighing perovskite powder and dissolving it in 1 ml of dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent with a solvent ratio of 8:2, using ultrasonic oscillation to dissolve, and the ultrasonic oscillation time is 30 minutes to prepare a mixed solution; during the ultrasonic oscillation process, the mixed solution is filled with argon gas, and the argon filling flow rate is 2 L / min.

[0040] In one embodiment, in step seven, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, evaporation rate 0.1Å / S.

[0041] In one embodiment, in step eight, the evaporation vacuum degree of the evaporation machine is 1×10 -4 Pa, evaporation rate 0.1 to 0.15Å / s.

[0042] In one embodiment, in step nine, the vacuum degree of the atomic layer deposition equipment is 0.5×10 4 Pa, the deposition channel temperature is 60° C., the deposition chamber temperature is 70° C., and the buffer layer is made of SnO2.

[0043] In one embodiment, in step 11, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, evaporation rate 2.5Å / S, the thickness of the first metal electrode layer is 100nm, and the second metal electrode layer is Ag.

[0044] In one embodiment, in step 12, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, evaporation rate 2Å / S, and the anti-reflection layer is magnesium fluoride.

[0045] The beneficial effects of the perovskite solution preparation method and perovskite cell preparation method provided in the embodiments of this application are as follows: the introduction of inert gas during the preparation process of the existing perovskite solution reduces the escape of solvent from the precursor solution during long-term use, effectively prevents ion aggregation in the precursor solution, and improves the long-term stability of the perovskite solution. Using the stable perovskite solution formula provided by this application, the perovskite solution prepared once can be used for batch production of perovskite films for up to several months without degradation, providing a guarantee for the stable output of high-quality, high-yield perovskite films on the production line. BRIEF DESCRIPTION OF THE DRAWINGS

[0046] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments or exemplary technical descriptions. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0047] FIG1 is a schematic structural diagram of a perovskite solar cell of the present application;

[0048] FIG2 is a schematic diagram of the perovskite solution of the present application being filled with an inert gas;

[0049] FIG3 is a schematic diagram of the internal ions of a conventional perovskite solution after storage for 30 days;

[0050] FIG4 is a schematic diagram of the internal ions of the perovskite solution of the present application after storage for 30 days;

[0051] FIG5 is a graph showing the performance test results of perovskite solar cells according to different embodiments of the present application.

[0052] Description of the accompanying drawings:

[0053] 110. First metal electrode layer; 111. First transparent electrode layer; 112. P-type substrate doping layer; 113. Substrate back passivation layer; 114. Silicon substrate; 115. Substrate surface passivation layer; 116. N-type substrate doping layer; 117. Tunneling layer; 211. Hole transport layer; 212. Perovskite absorption layer; 213. Passivation layer; 214. Electron transport layer; 215. Buffer layer; 216. Second transparent electrode layer; 217. Second metal electrode layer; 218. Anti-reflection layer. DETAILED DESCRIPTION

[0054] In order to make the purpose, technical solutions and advantages of this application more clear, the following further describes this application in detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain this application and are not intended to limit this application.

[0055] It should be noted that when a component is referred to as being "fixed on" or "disposed on" another component, it may be directly on the other component or indirectly on the other component. When a component is referred to as being "connected to" another component, it may be directly or indirectly connected to the other component. The terms "upper", "lower", "left", "right", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings. They are only for the convenience of description and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, they cannot be understood as limitations on this application. For ordinary technicians in this field, the specific meanings of the above terms can be understood according to the specific circumstances. The terms "first" and "second" are only used for the purpose of convenience of description and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features. "Multiple" means two or more, unless otherwise clearly and specifically defined.

[0056] In order to illustrate the technical solution provided by this application, a detailed description is given below with reference to specific drawings and embodiments.

[0057] 1 to 5 , a method for preparing a perovskite solution in an embodiment of the present application includes the following steps:

[0058] S1, dissolving perovskite powder in an organic solvent to obtain a mixed solution;

[0059] S2, using ultrasonic oscillation to accelerate the dissolution of the mixed solution prepared in S1, the ultrasonic oscillation time is 10-30 minutes, and during the ultrasonic oscillation process, the mixed solution is filled with inert gas, and the filling flow rate of the inert gas is 0-5L / min.

[0060] The inert gas is usually at least one of helium, neon, and argon; of course, it can also be an inert gas such as krypton and xenon.

[0061] Preferably, in the mixed solution prepared in S1, the structure of the perovskite powder is ABX; the organic solvent is at least one of dimethylformamide (DMF), G-butyrolactone (GBL), dimethyl sulfoxide (DMSO) and N,N-dimethylacetamide (DMA), and the solvent ratio can be 0-3:7-10.

[0062] Preferably, the organic solvent includes dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), and the molar ratio of dimethylformamide (DMF) to dimethyl sulfoxide (DMSO) is 8:2; the perovskite powder is placed in the organic solvent to form a mixed solution, and ultrasonic vibration is used for 30 minutes. During the ultrasonic vibration process, argon or neon is filled into the mixed solution, and the filling flow rate of the argon or neon is 0-5 L / min (preferably 2 L / min).

[0063] 1 , the present application also discloses a perovskite cell, which comprises, from bottom to top, a first metal electrode layer 110 , a first transparent electrode layer 111 , a P-type base doping layer 112 , a base back passivation layer 113 , a silicon substrate 114 , a base surface passivation layer 115 , an N-type base doping layer 116 , a tunneling layer 117 , a hole transport layer 211 , a perovskite absorption layer 212 , a passivation layer 213 , an electron transport layer 214 , a buffer layer 215 , a second transparent electrode layer 216 , a second metal electrode layer 217 , and an anti-reflection layer 218 .

[0064] The following provides several specific examples of preparing perovskite cells to clearly and completely describe the technical solutions of this application. Obviously, the described examples are only a portion of the embodiments of this application, not all of them. Based on the examples in this application, all other embodiments obtained by persons of ordinary skill in the art without inventive effort are within the scope of protection of this application. Example

[0065] A method for preparing a perovskite battery comprises the following steps:

[0066] Step 1: Provide a silicon substrate 114 , and sequentially prepare a back-side passivation layer 113 and a P-type base doping layer 112 on the back side of the silicon substrate 114 , and sequentially prepare a surface passivation layer 115 and an N-type base doping layer 116 on the surface of the silicon substrate 114 .

[0067] Step 2: A first transparent electrode layer 111 is prepared on the back side of the P-type base doped layer 112 by magnetron sputtering, which includes: placing the silicon substrate 114 (base sample) completed in step 1 in a magnetron sputtering device, setting an IZO target, the device operating power is 60W, the operating time is 1.5h, and the thickness of the first transparent electrode layer 111 is 100nm.

[0068] Step 3: Prepare the first metal electrode layer 110 on the back of the first transparent electrode layer 111 by evaporation method, which includes: placing the silicon substrate (substrate sample) completed in step 2 on the mask, placing it in the evaporation chamber for evaporation, and the evaporation vacuum degree is 2×10 -4 Ag is evaporated onto the first transparent electrode layer 111 at an evaporation rate of 2.5 Å / s. The thickness of the first metal electrode layer 110 is 200 nm.

[0069] Step 4: A tunneling layer 117 is prepared on the surface of the N-type base doping layer 116 by magnetron sputtering, which includes: placing the silicon substrate (base sample) completed in step 3 in a magnetron sputtering device, setting an IZO target, the device operating power is 60W, the operating time is 1h, and the thickness of the tunneling layer is 40nm.

[0070] Step 5: Prepare the hole transport layer 211 on the surface of the tunneling layer 117 by spin coating, which includes: placing the silicon substrate (substrate sample) completed in step 4 in a UV-Ozone for cleaning for 15 minutes; coating the surface of the tunneling layer 117 with the hole transport layer 211 dispersion, the spin coating speed is 2000r / pm, the spin coating time is 40s, and the amount of the hole transport layer 211 dispersion is 100ul, wherein: the hole transport layer 211 dispersion can be a certain amount of NiOx powder dissolved in a certain amount of ultrapure water, such as weighing 0.05mol of NiOx powder and dissolving it in 1ml of ultrapure water, and ultrasonically shaking for 20min.

[0071] After the spin coating is completed, the substrate sample is annealed at a temperature of 450° C. for 30 minutes. The thickness of the hole transport layer 211 is 20 nm.

[0072] Step 6: A perovskite absorption layer 212 is prepared on the surface of the hole transport layer 211 by spin coating, which includes: preparing a perovskite solution, weighing perovskite powder and dissolving it in 1 ml of dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent, with a solvent ratio of 8:2, using ultrasonic oscillation to dissolve, and the ultrasonic oscillation time is 30 minutes; during the ultrasonic oscillation process, the perovskite solution is filled with argon gas, and the argon filling flow rate is 2L / min.

[0073] The silicon substrate 114 (substrate sample) after step five is placed on the base of a spin coater, and the perovskite solution is coated on the surface of the hole transport layer 211 at a spin coating speed of 3500 r / pm and a spin coating time of 30 s.

[0074] After the spin coating is completed, the silicon substrate (substrate sample) is placed on a flash evaporation table with a flash evaporation time of 30 s and a flash evaporation temperature of 30 °C.

[0075] After the flash evaporation, an annealing treatment is performed. The annealing temperature is 100° C., the annealing time is 15 min, and the thickness of the perovskite absorption layer 212 is 500 nm.

[0076] Step 7: Prepare the passivation layer 213 on the surface of the perovskite absorption layer 212 by evaporation, which includes: weighing a certain amount of propylene diamine iodide and placing it in a crucible, placing the substrate sample completed in step 6 on the mask, and evaporating the vacuum degree to 2×10 -4 Pa, the evaporation rate is 0.1Å / S, and the thickness of the passivation layer 213 is 4nm.

[0077] After the evaporation, the substrate sample was annealed at a temperature of 100° C. for 8 min.

[0078] Step 8: Prepare the electron transport layer 214 on the surface of the passivation layer 213 by evaporation, which includes: weighing a certain amount of C60 and placing it in a crucible, placing the silicon substrate completed in step 7 on the mask, and evaporating the vacuum degree to 1×10 -4 Pa, with an evaporation rate of 0.1 to 0.15 Å / S, C60 is evaporated onto the passivation layer 213, and the thickness of the electron transport layer 214 is 20 nm.

[0079] Step 9: Prepare the buffer layer 215 on the surface of the electron transport layer 214 by atomic layer deposition, which includes: using an atomic layer deposition device, setting the vacuum degree of the atomic layer deposition device to 0.5×10 4 Pa, the deposition channel temperature is 60° C., the deposition chamber temperature is 70° C., SnO 2 is evaporated onto the surface of the electron transport layer 214 , and the thickness of the buffer layer 215 is 15 nm.

[0080] Step 10: A second transparent electrode layer 216 is prepared on the surface of the buffer layer 215 by magnetron sputtering, which includes: placing the silicon substrate completed in step 9 in a magnetron sputtering device, setting an IZO target, the device operating power is 50W, the operating time is 1h, and the thickness of the second transparent electrode layer 216 is 100nm.

[0081] Step 11: Prepare the second metal electrode layer 217 on the surface of the second transparent electrode layer 216 by evaporation; the process includes: placing the silicon substrate obtained in step 10 on a mask, placing it in an evaporation chamber for evaporation, and performing evaporation at a vacuum degree of 2×10 -4 Pa, with an evaporation rate of 2.5 Å / S, Ag is evaporated onto the layer film, and the thickness of the first metal electrode layer 110 is 100 nm.

[0082] Step 12: Prepare an anti-reflection layer 218 on the surface of the second metal electrode layer 217 by evaporation; the process includes: placing the silicon substrate obtained in step 11 on a mask, placing it in an evaporation chamber for evaporation, and performing evaporation at a vacuum degree of 2×10 -4 Pa, with an evaporation rate of 2 Å / s, magnesium fluoride is evaporated onto the second metal electrode layer 217. The thickness of the anti-reflection layer 218 is 100 nm. In other words, this embodiment 1 is a method for preparing a perovskite solar cell based on a ready-made perovskite solution containing argon. Example

[0083] This embodiment is basically the same as Example 1, except that after the perovskite solution is prepared in step 6, the prepared perovskite solution is allowed to stand for 30 days before performing subsequent preparation steps; that is, this embodiment is a method for preparing a perovskite solar cell based on the use of an argon-containing perovskite solution stored for 30 days. Example

[0084] This embodiment is substantially the same as Example 1, except that, in step 6, neon gas is added to the perovskite solution at a flow rate of 2 L / min. This embodiment is a method for preparing a perovskite solar cell using a freshly prepared neon-containing perovskite solution. Example

[0085] This example is essentially the same as Example 3, except that after preparing the perovskite solution in step 6, the perovskite solution is allowed to stand for 30 days before proceeding to the subsequent preparation steps. Specifically, this example is a method for preparing a perovskite solar cell using a neon-containing perovskite solution that has been stored for 30 days. Example

[0086] This embodiment is substantially the same as embodiment 1, except that no gas is added to the perovskite solution during the shaking process of preparing the perovskite solution in step 6. In other words, this embodiment is a method for preparing a perovskite solar cell based on a freshly prepared perovskite solution that is not filled with an inert gas. Example

[0087] This embodiment is substantially the same as Example 5, except that, during the shaking process of preparing the perovskite solution in step 6, no gas is introduced into the perovskite solution, and the prepared perovskite solution is allowed to stand for 30 days before proceeding to the subsequent preparation steps. In other words, this embodiment is a method for preparing a perovskite solar cell device using a perovskite solution that is not filled with inert gas after being stored for 30 days.

[0088] A solar simulator was used to calibrate the intensity of a standard sun and to measure the area of ​​1.0 cm 2 The device of the embodiment is subjected to an IV test for a long period of time, with the starting voltage set to 1.95V, the cut-off voltage set to 0V, the range set to 100mA, and the result rounded to two decimal places. The test results are shown in FIG5 .

[0089] The key design focus of this application lies in the fact that it primarily introduces inert gas during the preparation process of existing perovskite solutions, reducing the escape of solvents from the precursor solution during long-term use, effectively preventing ion aggregation in the precursor solution, and improving the long-term stability of the perovskite solution. Using the stable perovskite solution formula provided by this application, a perovskite solution prepared once can be used for batch production of perovskite films for up to several months without degradation, ensuring the stable output of high-quality, high-yield perovskite films on the production line. Specifically, as shown in Figure 5, the solar cell (device) prepared in Example 6 uses a perovskite solution without inert gas after 30 days of storage. In terms of device performance, the device performance of Example 6 shows significant degradation compared to that of Example 5 using the ready-to-use perovskite solution without inert gas. Its photoelectric conversion efficiency decreases from 31.09% to 26.52%. This indicates that the perovskite solution without inert gas is very unstable and degrades within 30 days of storage, resulting in poor film quality and low device performance.

[0090] As for the inert gas-containing perovskite solutions used in Examples 2 and 4, their 30-day storage did not lead to serious attenuation of the precursor solution; as for the device performance of Examples 1 and 2, the addition of argon inert gas perovskite solution greatly improved the stability of the perovskite precursor solution relative to the perovskite precursor solution without inert gas; in Example 2, in which neon perovskite solution was added after 30 days of storage, the device performance only attenuated by less than 1 percentage point relative to Example 1; as for the device performance of Examples 3 and 4, there was no attenuation after the addition of neon perovskite solution within 30 days of storage; and the device performance of Example 4 was even better than that of Example 3.

[0091] The above are merely optional embodiments of the present application and are not intended to limit the present application. For those skilled in the art, the present application may have various modifications and variations. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application should be included within the scope of the claims of the present application.

Claims

1. A method for preparing a perovskite solution, characterized in that: The following steps are included: S1, dissolving perovskite powder in an organic solvent to obtain a mixed solution; S2, using ultrasonic oscillation to accelerate the dissolution of the mixed solution obtained in S1, the ultrasonic oscillation time is 10-30min, during the ultrasonic oscillation process, inert gas is filled into the mixed solution, the filling flow rate of the inert gas is 0-5L / min, and a perovskite solution is obtained.

2. The method for preparing a perovskite solution according to claim 1, characterized in that: The inert gas is at least one of helium, neon and argon.

3. The method for preparing a perovskite solution according to claim 1, characterized in that: The organic solvent is at least one of dimethylformamide (DMF), G-butyrolactone (GBL), dimethyl sulfoxide (DMSO) and N,N-dimethylacetamide (DMA).

4. The method for preparing a perovskite solution according to claim 3, characterized in that: The organic solvent comprises dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), and the molar ratio of dimethylformamide (DMF) to dimethyl sulfoxide (DMSO) is 8:2; After the perovskite powder is placed in the organic solvent, ultrasonic vibration is used for 30 minutes. During the ultrasonic vibration, argon or neon gas is filled into the mixed solution. The filling flow rate of the argon or neon gas is 2 L / min.

5. The method for preparing a perovskite solution according to any one of claims 1 to 4, characterized in that: The structure of the perovskite powder is ABX.

6. A method for preparing a perovskite battery, characterized in that: The steps include: Step 1: providing a silicon substrate, sequentially preparing a substrate back passivation layer and a P-type substrate doping layer on the back side of the silicon substrate, and sequentially preparing a substrate surface passivation layer and an N-type substrate doping layer on the surface of the silicon substrate; Step 2: preparing a first transparent electrode layer on the back side of the P-type substrate doping layer by magnetron sputtering, which includes: Place the substrate sample after step 1 in a magnetron sputtering device, set an IZO target, the device has an operating power of 60W, a running time of 1.5h, and a first transparent electrode layer thickness of 100nm; Step 3: preparing a first metal electrode layer on the back of the first transparent electrode layer by evaporation, which includes: placing the substrate sample completed in step 2 on a mask plate, placing it in an evaporator chamber for evaporation, and the thickness of the first metal electrode layer is 200nm; Step 4: preparing a tunneling layer on the surface of the N-type substrate doping layer by magnetron sputtering, which includes: placing the substrate sample completed in step 3 in a magnetron sputtering device, setting an IZO target, the device working power is 60W, the running time is 1h, and the thickness of the tunneling layer is 40nm; Step 5: Prepare a hole transport layer on the surface of the tunneling layer by spin coating, which includes: placing the substrate sample completed in step 4 in a UV-Ozone for cleaning for 15 minutes; coating the surface of the tunneling layer with a hole transport layer dispersion, the spin coating speed is 2000r / pm, the spin coating time is 40s, after the spin coating is completed, annealing the substrate sample, the annealing temperature is 450°C, the annealing time is 30min, and the thickness of the hole transport layer is 20nm; Step 6: preparing a perovskite absorption layer on the surface of the hole transport layer by spin coating, which includes: placing the substrate sample completed in step 5 on the base of a spin coater, taking a perovskite solution to coat the surface of the hole transport layer, the spin coating speed is 3500r / pm, and the spin coating time is 30s; After the spin coating, the substrate sample was placed on a flash evaporation table with a flash evaporation time of 30 s and a flash evaporation temperature of 30 °C; After the flash evaporation, annealing treatment was performed at a temperature of 100°C, an annealing time of 15 min, and a thickness of the perovskite absorption layer of 500 nm. And, the perovskite precursor solution is a perovskite solution prepared by the preparation method of a perovskite solution according to any one of claims 1 to 5; Step 7: preparing a passivation layer on the surface of the perovskite absorption layer by evaporation, which includes: weighing a certain amount of propylenediamine iodine and placing it in a crucible, placing the substrate sample completed in step 6 on the mask for evaporation, and the thickness of the passivation layer is 4nm; After the evaporation, the substrate sample was annealed at a temperature of 100°C and an annealing time of 8 min. Step 8: preparing an electron transport layer on the surface of the passivation layer by evaporation, which includes: weighing a certain amount of C60 and placing it in a crucible, placing the substrate sample completed in step 7 on the mask for evaporation, and the thickness of the electron transport layer is 20nm; Step nine: preparing a buffer layer on the surface of the electron transport layer by atomic layer deposition, which includes: depositing a buffer layer material on the surface of the electron transport layer by atomic layer deposition equipment; Step 10: preparing a second transparent electrode layer on the surface of the buffer layer by magnetron sputtering, which includes: placing the substrate sample completed in step 9 in a magnetron sputtering device, setting an IZO target, the device has an operating power of 50W, the operating time is 1h, and the thickness of the second transparent electrode layer is 100nm; Step 11: preparing a second metal electrode layer on the surface of the second transparent electrode layer by evaporation; which includes: Place the substrate sample after step 10 on the mask and put it into the chamber of the evaporator for evaporation. The thickness of the first metal electrode layer is 100 nm. Step 12: Prepare an anti-reflection layer on the surface of the second metal electrode layer by evaporation; it includes: placing the substrate sample completed in step 11 on the mask plate, putting it into the chamber of the evaporator for evaporation, and the thickness of the anti-reflection layer is 100nm.

7. The method for preparing a perovskite battery according to claim 6, characterized in that: In step 3, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, evaporation rate 2.5Å / S, and the first transparent electrode layer is made of metallic silver.

8. The method for preparing a perovskite battery according to claim 6, characterized in that: In step 5, the hole transport layer dispersion is prepared by dissolving 0.05 mol of NiOx powder in 1 ml of ultrapure water and ultrasonically vibrating for 20 minutes.

9. The method for preparing a perovskite battery according to claim 6, characterized in that: In step 5, the amount of the hole transport layer dispersion is 100 ul.

10. The method for preparing a perovskite battery according to claim 6, characterized in that: In step six, the preparation of the perovskite solution includes: weighing perovskite powder and dissolving it in 1 ml of dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent, the solvent ratio is 8:2, using ultrasonic oscillation to dissolve, the ultrasonic oscillation time is 30 minutes, to prepare a mixed solution; during the ultrasonic oscillation process, argon is filled into the mixed solution, and the argon filling flow rate is 2L / min.

11. The method for preparing a perovskite battery according to claim 6, characterized in that: In step 7, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, evaporation rate 0.1Å / S.

12. The method for preparing a perovskite battery according to claim 6, characterized in that: In step eight, the evaporation vacuum degree of the evaporation machine is 1×10 -4 Pa, evaporation rate 0.1 to 0.15Å / S.

13. The method for preparing a perovskite battery according to claim 6, characterized in that: In step nine, the vacuum degree of the atomic layer deposition equipment is 0.5×10 4 Pa, the deposition pipeline temperature is 60° C., the deposition chamber temperature is 70° C., and the buffer layer is made of SnO2.

14. The method for preparing a perovskite battery according to claim 6, characterized in that: In step 11, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, the evaporation rate is 2.5Å / S, the thickness of the first metal electrode layer is 100nm, and the second metal electrode layer is Ag.

15. The method for preparing a perovskite battery according to claim 6, characterized in that: In step 12, the evaporation vacuum degree of the evaporation machine is 2×10 -4 Pa, evaporation rate 2Å / S, and the anti-reflection layer is magnesium fluoride.

Images