A fully transparent high-air-tightness vacuum flash box and application thereof

Abstract

This invention belongs to the field of vacuum flash evaporation box technology, specifically a fully transparent, highly airtight vacuum flash evaporation box and its application. It includes a box body with a vacuum chamber inside, a vacuum interface on the box body connected to a vacuum solenoid valve, damping hinges on the side of the box body, and a lid connected to the box body via the damping hinges. A sealing gasket is located on the side of the lid facing the box body. A sealing truncated cone is fixedly mounted on the top of the box body, and a handle is fixedly connected to one side of the lid. An acrylic plate is located inside the lid. By using acrylic glass material combined with a unique truncated cone foamed silicone sealing structure, high airtightness is ensured while achieving omnidirectional transparency of the device. Researchers can directly observe the dynamic changes of the perovskite wet film during the vacuum flash evaporation process. Combined with a two-stage vacuum oil pump, it perfectly meets the core kinetic requirement of rapid pressure drop in the vacuum flash evaporation process, providing a crucial guarantee for the preparation of high-quality thin films.

Description

Technical Field

[0001] This invention belongs to the field of vacuum flash evaporation box technology, specifically a fully transparent, highly airtight vacuum flash evaporation box and its applications. Background Technology

[0002] Vacuum flash evaporation is a highly efficient and promising process for preparing high-performance perovskite thin films. Its core principle involves rapidly placing the spin-coated perovskite wet film in a vacuum environment. By instantly and drastically reducing the vapor pressure of the solvent surface, the dissolved solvent in the system undergoes violent boiling and flash evaporation. This process significantly enhances the nucleation rate of perovskite, inducing the formation of dense, uniform, and highly covert polycrystalline films. Compared to the widely used traditional antisolvent extraction crystallization method, vacuum flash evaporation fundamentally avoids the process fluctuations and human errors introduced by the difficulty in precisely controlling the timing, amount, and uniformity of antisolvent addition. It provides a reliable technical path for achieving large-area, highly reproducible perovskite solar cell fabrication and is of great significance in promoting its industrialization from the laboratory.

[0003] Laboratories typically rely on general-purpose stainless steel or glass vacuum dryers as alternatives. These devices were not originally designed for perovskite flash evaporation processes, and therefore exhibit numerous limitations in application. Their chamber volumes are often too large, making them incompatible with the small-sized substrates used in conventional laboratory research. This not only wastes equipment costs and space but also leads to low efficiency in subsequent vacuuming due to the large dead volume. Furthermore, the metal chambers completely obstruct the line of sight, preventing researchers from monitoring the dynamic changes of the film in real time as it undergoes solvent boiling, dewetting, and final solidification. This significantly hinders the intuitive study of crystallization mechanisms and the precise definition of the process window.

[0004] Slow vacuuming rates make it difficult to achieve the rapid pressure drop required for the flash evaporation process, directly impacting the instantaneous and synchronous formation of crystal nuclei and easily leading to inhomogeneous defects in the thin film. Furthermore, these systems generally lack integrated automatic control units, with vacuuming and venting operations heavily reliant on manual intervention, making precise and repeatable control of key parameters such as flash evaporation duration impossible. In addition, the complex structures of industrial vacuum chambers, such as bolted seals, result in cumbersome opening and closing operations and inconvenient maintenance of seals, failing to meet the high-frequency, rapid-response operational demands of scientific research experiments.

[0005] Therefore, the present invention provides a fully transparent, highly airtight vacuum flash evaporation box and its application. Summary of the Invention

[0006] To overcome the shortcomings of existing technologies and solve the problems of opaqueness, slow vacuuming speed, cumbersome operation and high cost of existing equipment, this invention proposes a fully transparent high airtight vacuum flash evaporation box and its application.

[0007] The technical solution adopted by the present invention to solve its technical problem is as follows: The present invention provides a fully transparent high airtight vacuum flash evaporation box, including a box body, a vacuum chamber provided inside the box body, a vacuum interface provided on the box body and connected to the vacuum chamber, a vacuum solenoid valve connected to the vacuum interface, a damping hinge installed on the side of the box body, a box cover connected to the box body through the damping hinge, a sealing gasket provided on the side of the box cover facing the box body, a sealing truncated cone fixedly provided on the top of the box body and surrounding one side of the vacuum chamber, a handle fixedly connected to one side of the box cover, and an acrylic plate provided inside the box cover; The box contains an installation box located below the vacuum chamber. The installation box contains a feeding mechanism for assisting in substrate feeding, a compression mechanism, and a driving mechanism. The box also contains a cleaning mechanism for cleaning the vacuum chamber.

[0008] Preferably, the feeding mechanism includes a cylinder, a load-bearing plate, a push rod, and a sealing ring. The cylinder is symmetrically arranged inside the box body, and its two ends are respectively connected to the vacuum chamber and the mounting box. The load-bearing plate is arranged inside the mounting box. The push rod passes through the inside of the cylinder, and its bottom end is fixedly connected to the load-bearing plate. The sealing ring is fixedly arranged inside the cylinder and is used to seal the gap between the push rod and the cylinder.

[0009] Preferably, the driving mechanism includes a threaded ring, a drive motor, a reducer, and a threaded rod. The threaded ring is embedded inside the load-bearing plate. The drive motor is fixedly mounted on the inner wall of the mounting box. The reducer is fixed inside the mounting box by a bracket, and the output end of the drive motor is fixedly connected to the input end of the reducer. The threaded rod is rotatably mounted inside the mounting box, and the outer surface of the threaded rod is threadedly connected to the inside of the threaded ring. One end of the threaded rod is fixedly connected to the output end of the reducer. Guide rods are symmetrically inserted inside the load-bearing plate, and the ends of the guide rods are fixedly connected to the inner wall of the mounting box. A connecting assembly is provided on the load-bearing plate.

[0010] Preferably, the connecting assembly includes a strip frame, connecting shafts, and a push plate. The strip frame is fixed to the top of the load-bearing plate, the array of connecting shafts is fixed inside the strip frame, and one end of the push plate is movably connected to the corresponding connecting shaft.

[0011] Preferably, the compression mechanism includes a compression groove, a compression block, a long plate, and a concave frame. The compression groove is symmetrically arranged inside the mounting box, the compression block is arranged inside the compression groove, the long plate array is mounted on the compression block, the concave frame is fixed to one end of the long plate, and the concave frame is movably connected to a corresponding push plate. A limiting frame corresponding to the long plate is fixedly arranged inside the mounting box, and the long plate passes through the limiting frame. One end of the compression groove is connected to a conveying pipe.

[0012] Preferably, the cleaning mechanism includes a diversion channel and jet holes. The diversion channel is embedded inside the housing and located on one side of the vacuum chamber. The diversion channel is connected to the other end of the corresponding delivery pipe. The jet hole array is arranged on the diversion channel, and a filter screen is arranged inside the jet hole.

[0013] Preferably, the box body is provided with a sliding groove, and the sliding groove is located on one side of the vacuum chamber. The sliding groove is connected to the vacuum chamber. Magnetic plates are symmetrically arranged inside the sliding groove. A strip plate is inserted inside the sliding groove. A magnetic suction plate corresponding to the magnetic plate is embedded inside the strip plate.

[0014] Preferably, a waste trough is provided inside the strip plate, and the waste trough is located on one side of the vacuum chamber, and a pull block is fixedly provided on the top of the strip plate.

[0015] Preferably, a controller is fixedly installed on the front of the box and is electrically connected to the drive motor, and a battery assembly is fixedly installed inside the mounting box and is electrically connected to the drive motor.

[0016] An application method for a fully transparent, highly airtight vacuum flash evaporation box includes the following steps: S1. Spin-coat the perovskite precursor solution onto the substrate to form a wet film. After spin-coating, immediately place the substrate with the wet film into the vacuum chamber, then close the lid and evacuate the vacuum chamber through the vacuum interface for 10 to 60 seconds. After the process is completed, release the vacuum, take out the substrate and anneal it to obtain a perovskite thin film. S2. The vacuuming process must meet the following requirements: reduce the vacuum level to below 100 Pa within 10 seconds and to below 50 Pa within 30 seconds. S3, the solvent for the perovskite precursor solution is a mixture of DMF and NMP, wherein the active component of the perovskite is FA. X MA 1-X PbI3, where 0.6 ≤ x ≤ 0.8; S4, the active component of perovskite is FA 0.7 MA 0.3The PbI3 solvent has a DMF to NMP volume ratio of 840:160, the precursor solution has a PbI2 concentration of 2M, and contains MACl at a concentration of 5 mg / ml and PBAI at a concentration of 2 mg / ml; the vacuum treatment lasts for 30 seconds, and the annealing treatment is performed at 100°C for 15 minutes.

[0017] The beneficial effects of this invention are as follows: 1. The fully transparent, high-airtightness vacuum flash evaporation box described in this invention, by employing acrylic glass material and combining it with a unique frustum-shaped foamed silicone sealing structure, achieves omnidirectional transparency of the device while ensuring high airtightness. Researchers can observe the dynamic changes of the perovskite wet film during the vacuum flash evaporation process in real time and intuitively for the first time, including the violent boiling of the solvent, the color change of the film, and the curing behavior. This provides crucial visual evidence for optimizing process parameters and studying crystallization kinetics. Combined with a two-stage vacuum oil pump, it perfectly meets the core kinetic requirement of rapid pressure drop in the vacuum flash evaporation process, thereby effectively inducing uniform and rapid nucleation of perovskite, providing a key guarantee for the preparation of high-quality films with no pinholes and high coverage.

[0018] 2. The fully transparent, high-airtightness vacuum flash evaporation chamber of this invention features an integrated and lightweight design of the lid, damping hinge, and vacuum interface. Combined with an external solenoid valve and timing control system, it greatly enhances the ease of operation and automation of the equipment. The damping hinge enables stable positioning of the lid at any angle, facilitating one-handed operation. The automatic control system achieves precise and repeatable control of the vacuuming and breaking processes, significantly reducing human error and greatly improving experimental efficiency and data repeatability. Based on low-cost materials and a simple mechanical structure, it breaks away from the expensive and complex traditional vacuum equipment model, enabling high-performance vacuum flash evaporation technology to be more widely adopted in various laboratories, lowering the research threshold. This has significant value for the scientific research and future industrialization of perovskite technology.

[0019] 3. The fully transparent, high-airtightness vacuum flash evaporation box of the present invention facilitates the cleaning of the vacuum chamber through the compression groove and the diversion groove. When the load-bearing plate moves upward, it drives the strip frame to move. Through the cooperation of the strip frame and the connecting shaft, it drives the push plate to move. The movement of the push plate can drive the long plate to move. The limiting frame guides the long plate. The movement of the long plate will push the compression block to move smoothly. When the compression block moves, it will compress the air inside the compression groove, thereby allowing the air to flow. The air will flow into the diversion groove through the delivery pipe, and the air will flow into the vacuum chamber through the air jet hole, thereby cleaning the bottom of the vacuum chamber wall and avoiding the accumulation of debris, which would affect the use effect.

[0020] 4. The fully transparent, high-airtightness vacuum flash evaporation box of the present invention achieves clean treatment of the vacuum chamber by setting a compression groove and a diversion groove. When the load-bearing plate moves upward, it drives the strip frame to move synchronously. The strip frame is linked to the push plate via the connecting shaft. The push plate then drives the long plate to move. The limiting frame guides and limits the movement of the long plate. The movement of the long plate pushes the compression block to move smoothly. When the compression block moves, it compresses the air in the compression groove, promotes air flow, and the air flows into the diversion groove through the delivery pipe. Then it is sprayed into the vacuum chamber through the jet hole to blow clean the bottom of its inner wall and prevent the accumulation of debris from affecting the use effect of the equipment.

[0021] 5. The fully transparent, high-airtightness vacuum flash evaporation box of the present invention has a waste trough for easy collection and removal of debris and impurities. Impurities can flow into the waste trough for temporary storage. When it is necessary to clean impurities, pulling the pull block can move the strip plate, and the movement of the strip plate can remove the waste collected in the waste trough, ensuring the cleanliness of the vacuum chamber. Attached Figure Description

[0022] The invention will now be further described with reference to the accompanying drawings.

[0023] Figure 1 This is a perspective view of the fully transparent, highly airtight vacuum flash evaporation box of the present invention; Figure 2 This is a schematic diagram of the box structure in this invention; Figure 3 This is a schematic diagram of the structure of the mounting box and cylinder in this invention; Figure 4 This is a schematic diagram of the connection between the push plate and the long plate in this invention; Figure 5 This is a schematic diagram of the load-bearing plate in this invention; Figure 6 This is a schematic diagram of the structure of the long plate and the compression block in this invention; Figure 7 This is a schematic diagram of the strip plate structure in this invention; Figure 8 This is the present invention. Figure 1 Enlarged structural diagram of A in the middle; Figure 9 This is a schematic diagram of the vacuum degree of the vacuum flash evaporation box changing over time in this invention; Figure 10 This is a schematic diagram of the band gap Tauc image of the FA0.7MA0.3PbI3 perovskite thin film in this invention; Figure 11 This is a schematic diagram of the steady-state fluorescence emission spectrum of the FA0.7MA0.3PbI3 perovskite thin film of the present invention; Figure 12 This is a current density-voltage (J-V) test curve of the perovskite solar cell prepared by this invention; Figure 13 This is a schematic diagram of the steady-state efficiency output curve of the perovskite solar cell of the present invention; Figure 14 This is a schematic diagram of the external quantum efficiency curve and the current density integral curve of the perovskite solar cell of the present invention; Figure 15 This is a histogram of the efficiency statistics of 48 perovskite solar cells in this invention; Figure 16 This is a schematic diagram of the perovskite battery module fabricated according to the present invention; Figure 17 This is a schematic diagram of the J-V test curve of the perovskite battery module in this invention.

[0024] In the diagram: 1. Box body; 2. Vacuum chamber; 3. Vacuum interface; 4. Vacuum solenoid valve; 5. Damping hinge; 6. Box cover; 7. Handle; 8. Sealing gasket; 9. Sealing truncated cone; 10. Acrylic sheet; 11. Mounting box; 12. Cylinder; 13. Load-bearing plate; 14. Threaded ring; 15. Drive motor; 16. Reducer; 17. Threaded rod; 18. Strip frame; 19. Connecting shaft; 20. Push plate; 21. Push rod; 22. Sealing ring; 23. Guide rod; 24. Compression groove; 25. Compression block; 26. Long plate; 27. Concave frame; 28. Conveying pipe; 29. ​​Limiting frame; 30. Diverter groove; 31. Air jet hole; 32. Slide groove; 33. Magnetic plate; 34. Strip plate; 36. Magnetic suction plate; 37. Waste trough; 35. Pull block; 38. Controller; 39. Battery assembly. Detailed Implementation

[0025] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0026] Example 1, please refer to Figures 1 to 17 The present invention discloses a fully transparent, high-airtightness vacuum flash evaporation box, comprising a box body 1, a vacuum chamber 2 inside the box body 1, a vacuum interface 3 on the box body 1 connected to the vacuum chamber 2, a vacuum solenoid valve 4 connected to the vacuum interface 3, a damping hinge 5 installed on the side of the box body 1, a box cover 6 connected to the box body 1 via the damping hinge 5, a sealing gasket 8 on the side of the box cover 6 facing the box body 1, a sealing prism 9 fixedly installed on the top of the box body 1 and surrounding one side of the vacuum chamber 2, a handle 7 fixedly connected to one side of the box cover 6, an acrylic plate 10 inside the box cover 6, an installation box 11 inside the box body 1 and located below the vacuum chamber 2, a feeding mechanism for assisting substrate feeding inside the installation box 11, a compression mechanism inside the installation box 11, a driving mechanism inside the installation box 11, and a cleaning mechanism for cleaning the inside of the vacuum chamber 2 inside the box body 1. When preparing perovskite thin films using a fully transparent, high-airtightness vacuum flash evaporation box, the box body 1 is made of transparent acrylic glass with external dimensions of 150mm×150mm×50mm. The interior is cut to form a vacuum chamber 2 with an effective volume of 100mm×100mm×20mm. The width and height of the sealing prism 9 are both 2mm. The box cover 6 is also made of acrylic glass with dimensions of 150mm×150mm×20mm. The sealing gasket 8 is made of foamed silicone, and its inner surface is tightly adhered to the box cover 6. Its position corresponds precisely to the sealing prism 9 on the box body 1. The box cover 6 can be stably opened and closed at any angle by means of the damping hinge 5. The vacuum interface 3 is a threaded hole and is connected to the vacuum solenoid valve 4 through a metal connector. The pumping port of the vacuum solenoid valve 4 is connected to a two-stage vacuum oil pump with a pumping rate of 2L / min through a pipeline. The venting port is connected to a silencer valve. The vacuum solenoid valve 4 is connected to an external programmable timer control socket through a control signal line to achieve automatic control. The preparation of the perovskite precursor solution first involves preparing the perovskite active component FA. 0.7 MA 0.3 The PbI3 precursor solution, the specific steps are as follows: For precursor solution preparation, PbI₂, MAI, and FAI were accurately weighed at a molar ratio of 1:0.3:0.7 and dissolved in a mixed solvent of DMF and NMP, where the volume ratio of DMF to NMP was 840:160. The concentration of PbI₂ in the solution was controlled at 2M. In addition, 5 mg / mL of MAI and 2 mg / mL of PBAI were added to the precursor solution as crystallization regulators. The mixed solution was sonicated and shaken for 10 minutes to ensure complete dissolution, and then filtered through a 0.22 μm polytetrafluoroethylene syringe filter for later use.

[0027] Preparation and vacuum flash evaporation of perovskite thin films: The vacuum flash evaporation preparation of perovskite thin films includes the following steps: Step 1: The ITO glass is ultrasonically cleaned for 15 minutes each in Nikon 90 cleaning solution, first deionized water and second deionized water. After drying with clean compressed air, it is UV treated for 15 minutes. Step 2: Deposit a PTAA hole transport layer on the ITO glass surface, spin coat the PTAA solution using a spin coater at 4000 rpm for 20 seconds, and then anneal on a 100°C hot plate for 2 minutes. Step 3: Perovskite film deposition. The precursor solution prepared in Step 1 is deposited on the surface of the ITO / PTAA film prepared in Step 2 using a dynamic spin-coating method to form a perovskite pre-wet film. Step 4: Vacuum flash evaporation. The perovskite pre-fabricated wet film that has undergone deposition treatment in Step 3 is immediately placed in the vacuum flash evaporation chamber for vacuum flash evaporation treatment. Step 5: Heat treatment. The vacuum flash-treated glass substrate is placed on a hot stage for heat treatment to complete the preparation of the perovskite thin film.

[0028] The ITO glass in step one is pre-chemically etched ITO glass with dimensions of 20*15*1.1mm.

[0029] In step two, the PTAA solution uses chlorobenzene as a solvent, with a solution concentration of 5 mg / mL. The solution is filtered using a 0.22 μm polytetrafluoroethylene syringe filter before use.

[0030] In step three, the spin coating process of the perovskite solution is carried out in a compressed air glove box. Dry compressed air is introduced into one end of the glove box, and the exhaust gas is discharged through the exhaust pipe at the other end. The ambient temperature of the box is controlled at 20°C and the relative humidity is 12%-15%.

[0031] In step three, during the spin coating process of the perovskite solution, 30 μL of the above perovskite precursor solution is dynamically dropped onto the surface of the ITO / PTAA substrate, and a spin coater is used to spin coat at a speed of 7000 rpm for 10 seconds. The solution is dropped on the second second after the spin coating begins.

[0032] In step four, immediately after spin coating, the substrate with the perovskite wet film is transferred to the vacuum chamber 2 of the vacuum flash evaporation box of this invention. The box cover 6 is quickly closed, the vacuum system is started, and the vacuuming time is set to 30 seconds via the timer controller. The system reduces the vacuum level to below 100 Pa within 10 seconds (actually reaching approximately 80 Pa). The total vacuum flash evaporation time is 30 seconds, and the actual minimum vacuum level is approximately 50 Pa. Under this vacuum environment, the solvent flashes rapidly, and the film changes from an initial transparent wet film state to a yellow transparent state.

[0033] In step four, the vacuum flash evaporation box of the present invention is also in an air glove box environment, and the gas introduced is the air in the glove box when the vacuum is broken.

[0034] In step five, after the vacuum flash evaporation process is completed, the vacuum is automatically released, the sample is taken out and placed on a hot plate at 100°C for annealing for 15 minutes, and finally a black mirror-finish perovskite film with good crystallinity is formed.

[0035] Complete fabrication of solar cell devices On the perovskite thin film obtained by the above steps, a complete solar cell device is further fabricated. Its structure is ITO / PTAA / Perovskite / PCBM / BCP / Ag, including: using ITO glass as the anode, depositing a PTAA hole transport layer, depositing a perovskite active layer on it, and sequentially spin-coating a PC60BM electron transport layer and a Bphen cathode interface layer, and finally evaporating Ag as the cathode.

[0036] Electron transport layer: A PCBM solution is spin-coated onto the perovskite layer to form an electron transport layer. A chlorobenzene solution (20 mg / mL) of PCBM is spin-coated at 6000 rpm for 30 s to form an electron transport layer with a thickness of 70–100 nm. Then, the vacuum flash evaporation chamber of this invention is used for vacuum treatment for 60 s to promote the rapid evaporation of the PCBM film in the solution, thereby improving the final quality of the electron transport layer.

[0037] Cathode interface layer: After the electron transport layer is prepared, BCP solution is spin-coated as the cathode interface layer. Bphen ethanol solution (0.7 mg / mL) is spin-coated at 6000 rpm in the same manner to form a cathode buffer layer of approximately 7 nm.

[0038] Metal cathode: An Ag electrode prepared by vacuum thermal evaporation at a vacuum level of 5 × 10⁻⁶. -4 A 100 nm thick Ag electrode was deposited under Pa conditions to complete the device structure before packaging.

[0039] Thin film morphology: The surface and cross-sectional morphology of the prepared thin film were characterized using a Zeiss Sigma 300+ scanning electron microscope (SEM). 0.7 MA 0.3 The PbI3 perovskite thin film has uniform, dense, and non-porous grains on its surface, and the cross-section shows excellent structural characteristics of uniform crystallization, no voids, and no obvious delamination.

[0040] Optical performance: The absorption spectrum of the thin film was measured using an Agilent HP8453 UV-Vis spectrophotometer. FA 0.7 MA 0.3 The Tauc curve was derived from the absorption spectrum of the PbI3 perovskite thin film. Based on the Tauc curve, the band gap of the film was calculated to be approximately 1.53 eV. The fluorescence performance of the film was tested using a self-made steady-state fluorescence spectrometer. An 80 mW 532 nm green laser was used as the excitation source. The measured steady-state fluorescence spectrum is as follows: Figure 11As shown, the main emission peak is located at 800 nm, consistent with the absorption spectrum, further verifying the excellent photoelectric properties of the thin film. All devices were unpackaged, and tests were conducted in air. A Zolix Solar IV-150A-ZZU photovoltaic testing system was used under standard AM1.5G (100 mW / cm²) illumination conditions, irradiated using a Zolix-HPS-300XA solar simulator, and calibrated using a Zolix QE-B1 silicon-based standard cell. The JV curve of the cell shows the optimal performance parameters: open-circuit voltage 1.160V, short-circuit current density 26.500 mA / cm², fill factor 0.823, and photoelectric conversion efficiency of 25.30%. Steady-state output test curve: Under continuous 500s illumination, the continuous output efficiency is 25.3%, with stable output and no significant performance degradation, indicating the high crystallinity of the perovskite thin film. External quantum efficiency (EQE): The EQE curves of the perovskite solar cells were tested using a self-made EQE testing system. A Zolix-HPS-300XA solar simulator was used as the light source. A Zolix Omni-λ series grating monochromator output monochromatic light, and a Gillison 2400 was used to collect the photocurrent signal. Finally, the EQE curves were obtained using a certified silicon detector. The EQE curves showed excellent response over a wide spectral range of 300-850 nm, and the integrated current density was in high agreement with the JV test results.

[0041] Under the conditions of this embodiment, 48 perovskite solar cell devices were continuously fabricated. The efficiency histogram shows that the average efficiency is as high as 24.45% and the standard deviation is only 0.33%, which proves the great advantage of the vacuum flash evaporation box of the present invention in terms of process repeatability.

[0042] When the thin film is prepared and unloaded, the unloading mechanism is driven to move through the drive mechanism. The movement of the unloading mechanism can lift the substrate, which facilitates the unloading process. When the unloading mechanism is driven to move, the compression mechanism is driven to move and compress air. After the compressed air flows into the cleaning mechanism, it can clean the inside of the vacuum chamber 2, ensuring the cleanliness of the vacuum chamber 2.

[0043] Example 2, please refer to Figures 1 to 17 This invention relates to a fully transparent, highly airtight vacuum flash evaporation box. This embodiment details the entire process of preparing a formamidinium-methylamine mixed cation perovskite solar cell module using the vacuum flash evaporation box described in this invention.

[0044] Specifically, to achieve modular applications, this invention also constructs a large-area perovskite solar cell module, whose device structure is the same as that of a single cell, namely ITO / PTAA / perovskite / PCBM / BCP / Ag. The module divides a 5×5 cm² area into 10 series-connected sub-cells using laser scribing (P1, P2, P3) technology.

[0045] The specific preparation steps are as follows: Step 1: Use a P1 laser (power 0.5W, speed 2000mm / s, wavelength 1064nm) to pattern and scribble the ITO substrate to form independent anode regions of tandem sub-units; Step 2: Clean and treat with ultraviolet ozone in the same manner as the single cell (Example 1), spin coat the PTAA layer at 4000 rpm in a low humidity glove box, and then anneal at 100°C for 2 min. Step 3, perovskite solution spin coating process: 100 μL of perovskite precursor solution is dynamically dropped onto the surface of ITO / PTAA substrate, and spin-coated for 10 seconds at 7000 rpm using a spin coater. The solution is dropped on the second second after the start of spin coating. Step 4, vacuum flash evaporation: The perovskite pre-fabricated wet film that has undergone deposition treatment in step 3 is immediately placed in the vacuum flash evaporation chamber for vacuum flash evaporation treatment. Step 5: Spin-coating the PCBM and BCP layers using the process related to Example 1; Step 6: Use a P2 laser (0.1W power, 5000mm / s speed) to etch, ensuring complete removal of all covering layers on the ITO surface without damaging the ITO layer; Step 7: Deposit Ag electrode (100nm) under vacuum of 5×10-4Pa, and remove Ag layer without damaging ITO by scribing with P3 laser (0.1W power, 2500mm / s) to complete component fabrication; Step 8: After the device fabrication is completed, use conductive copper tape to bring out the positive and negative electrodes, and then use UV resin glue for simple encapsulation to complete the device fabrication.

[0046] In step two, the PTAA spin coating process is the same as in Example 1, but the amount of PTAA solution used needs to be increased to 60 μL to ensure complete coverage of the PTAA on the large-size substrate.

[0047] In step three, the solvent ratio and the molar ratio of PbI2, MAI, and FAI in the perovskite solution are exactly the same as in Example 1. The difference is that the concentration of PbI2 in the solution is reduced to 1.4 M, and the final thickness of the perovskite film will be reduced to about 300 nm.

[0048] In step four, the vacuum flash evaporation procedure is the same as in Example 1.

[0049] Perovskite module performance testing: After simple encapsulation with AB glue, the modules were tested in an air environment. The JV curve measurement instrument was the same as the single-cell testing system. The JV test results showed that the highest photoelectric conversion efficiency reached 22.9%.

[0050] The above description fully illustrates that the fully transparent vacuum flash evaporation box proposed in this invention can be used to construct high-performance perovskite solar cells and large-area perovskite solar cell modules.

[0051] Example 3, please refer to Figures 1 to 17 The fully transparent, high-airtightness vacuum flash evaporation box of the present invention includes a feeding mechanism comprising a cylinder 12, a load-bearing plate 13, a push rod 21, and a sealing ring 22. The cylinder 12 is symmetrically arranged inside the box body 1, and both ends of the cylinder 12 are respectively connected to the vacuum chamber 2 and the mounting box 11. The load-bearing plate 13 is arranged inside the mounting box 11. The push rod 21 passes through the inside of the cylinder 12, and the bottom end of the push rod 21 is fixedly connected to the load-bearing plate 13. The sealing ring 22 is fixedly arranged inside the cylinder 12, and the sealing ring 22 is used to seal the gap between the push rod 21 and the cylinder 12. The cylinder 12 facilitates the movement of the push rod 21. After the perovskite thin film is prepared on the substrate, when the workpiece is unloaded, the load-bearing plate 13 is moved by the drive mechanism, which will drive the push rod 21 to move. After the push rod 21 moves into the vacuum chamber 2, it will push the substrate upward, which facilitates rapid unloading and improves work efficiency.

[0052] Furthermore, the drive mechanism includes a threaded ring 14, a drive motor 15, a reducer 16, and a threaded rod 17. The threaded ring 14 is embedded inside the load-bearing plate 13. The drive motor 15 is fixedly mounted on the inner wall of the mounting box 11. The reducer 16 is fixed inside the mounting box 11 by a bracket, and the output end of the drive motor 15 is fixedly connected to the input end of the reducer 16. The threaded rod 17 is rotatably mounted inside the mounting box 11, and the outer surface of the threaded rod 17 is threadedly connected to the inside of the threaded ring 14. One end of the threaded rod 17 is fixedly connected to the output end of the reducer 16. Guide rods 23 are symmetrically inserted inside the load-bearing plate 13, and the ends of the guide rods 23 are fixedly connected to the inner wall of the mounting box 11. A connecting assembly is provided on the load-bearing plate 13. When the drive mechanism moves, the drive motor 15 controls the movement of the reducer 16, which drives the threaded rod 17 to rotate. When the threaded rod 17 rotates, it causes the load-bearing plate 13 to move through the threaded ring 14. The guide rod 23 guides the load-bearing plate 13, which allows the push rod 21 to move smoothly. When the load-bearing plate 13 moves, it drives the connecting components to move.

[0053] Furthermore, the connecting assembly includes a strip frame 18, a connecting shaft 19, and a push plate 20. The strip frame 18 is fixed to the top of the load-bearing plate 13, the connecting shafts 19 are arrayed and fixed inside the strip frame 18, and one end of the push plate 20 is movably connected to the corresponding connecting shaft 19. When the load-bearing plate 13 moves upward, it will drive the strip frame 18 to move. Through the cooperation of the strip frame 18 and the connecting shaft 19, it will drive the push plate 20 to move. The movement of the push plate 20 can drive the long plate 26 to move.

[0054] Furthermore, the compression mechanism includes a compression groove 24, a compression block 25, a long plate 26, and a concave frame 27. The compression groove 24 is symmetrically arranged inside the mounting box 11, the compression block 25 is arranged inside the compression groove 24, the long plate 26 is arrayed and installed on the compression block 25, the concave frame 27 is fixed to one end of the long plate 26, and the concave frame 27 is movably connected to the corresponding push plate 20. A limiting frame 29 corresponding to the long plate 26 is fixedly arranged inside the mounting box 11, and the long plate 26 passes through the limiting frame 29. One end of the compression groove 24 is connected to a conveying pipe 28. When the push plate 20 moves, it drives the long plate 26 to move through the concave frame 27. The limit frame 29 guides the long plate 26. The movement of the long plate 26 pushes the compression block 25 to move smoothly. When the compression block 25 moves, it compresses the air inside the compression groove 24, which in turn allows the air to flow. The air then flows into the diversion groove 30 through the delivery pipe 28.

[0055] Furthermore, the cleaning mechanism includes a diversion channel 30 and jet holes 31. The diversion channel 30 is embedded inside the housing 1 and is located on one side of the vacuum chamber 2. The diversion channel 30 is connected to the other end of the corresponding delivery pipe 28. An array of jet holes 31 is arranged on the diversion channel 30, and a filter screen is provided inside the jet holes 31. After compressed air flows into the distribution tank 30 through the delivery pipe 28, it flows into the vacuum chamber 2 through the jet hole 31, which can clean the bottom of the inner wall of the vacuum chamber 2, prevent the accumulation of debris and affect the performance. The filter screen can effectively prevent impurities from entering the jet hole 31.

[0056] Furthermore, the box body 1 is provided with a sliding groove 32, and the sliding groove 32 is located on one side of the vacuum chamber 2. The sliding groove 32 is connected to the vacuum chamber 2. Magnetic plates 33 are symmetrically arranged inside the sliding groove 32. A strip plate 34 is inserted inside the sliding groove 32. A magnetic suction plate 36 corresponding to the magnetic plate 33 is embedded inside the strip plate 34. The slide 32 provides installation space for the magnetic plate 33 and the strip plate 34. The magnetic plate 36 and the magnetic plate 33 work together to limit the position of the strip plate 34.

[0057] Furthermore, a waste trough 37 is provided inside the strip plate 34, and the waste trough 37 is located on one side of the vacuum chamber 2. A pull block 35 is fixedly provided on the top of the strip plate 34. The diversion channel 37 is located on one side of the vacuum chamber 2. When removing impurities inside the vacuum chamber 2, the impurities will flow into the waste tank 37 for temporary storage. When it is necessary to remove impurities, pulling the pull block 35 will move the strip plate 34. The strip plate 34 moves through the waste tank 37 to remove the collected waste.

[0058] Furthermore, a controller 38 is fixedly installed on the front of the box 1, and the controller 38 is electrically connected to the drive motor 15. A battery assembly 39 is fixedly installed inside the mounting box 11, and the battery assembly 39 is electrically connected to the drive motor 15. The drive motor 15 can be controlled by the controller 38, and the battery pack 39 provides power for the drive motor 15.

[0059] An application method for a fully transparent, highly airtight vacuum flash evaporation box includes the following steps: S1. Spin-coat the perovskite precursor solution onto the substrate to form a wet film. After spin-coating, immediately place the substrate with the wet film into the vacuum chamber 2, then close the lid 6, and vacuum chamber 2 through the vacuum interface 3 for 10 to 60 seconds. After the process is completed, release the vacuum, take out the substrate and perform annealing to obtain a perovskite thin film. S2. The vacuuming process must meet the following requirements: reduce the vacuum level to below 100 Pa within 10 seconds and to below 50 Pa within 30 seconds. S3, the solvent for the perovskite precursor solution is a mixture of DMF and NMP, wherein the active component of the perovskite is FA. X MA 1-X PbI3, where 0.6 ≤ x ≤ 0.8; S4, the active component of perovskite is FA 0.7 MA 0.3 The PbI3 solvent has a DMF to NMP volume ratio of 840:160, the precursor solution has a PbI2 concentration of 2M, and contains MACl at a concentration of 5 mg / ml and PBAI at a concentration of 2 mg / ml; the vacuum treatment lasts for 30 seconds, and the annealing treatment is performed at 100°C for 15 minutes.

[0060] Working principle: First, the perovskite precursor solution is spin-coated onto the substrate to form a wet film. After spin-coating, the substrate with the wet film is immediately placed into the vacuum chamber 2. Then, the cover 6 is closed, and the vacuum chamber 2 is evacuated through the vacuum interface 3 for 10 to 60 seconds. After evacuation, the vacuum is released, the substrate is removed, and annealing is performed to obtain the perovskite thin film. When the film is prepared and unloaded, the drive motor 15 is controlled to move, which drives the threaded rod 17 to rotate through the reducer 16. When the threaded rod 17 rotates, it moves the load-bearing plate 13 through the threaded ring 14. The guide rod 23 guides the load-bearing plate 13, allowing the push rod 21 to move smoothly. After the push rod 21 moves into the vacuum chamber 2, it pushes the substrate upward, which facilitates rapid unloading and improves work efficiency. When the load-bearing plate 13 moves upward, it drives the strip frame 1. The movement of the push plate 20, driven by the cooperation of the strip frame 18 and the connecting shaft 19, will drive the long plate 26 to move. The limit frame 29 will guide the long plate 26. The movement of the long plate 26 will push the compression block 25 to move smoothly. When the compression block 25 moves, it will compress the air inside the compression tank 24, thereby allowing the air to flow. The air will flow into the diversion tank 30 through the delivery pipe 28, and will flow into the vacuum chamber 2 through the jet hole 31, thereby cleaning the bottom of the inner wall of the vacuum chamber 2 and preventing the accumulation of debris, which will affect the use effect. The impurities will flow into the waste tank 37 for temporary storage. When it is necessary to remove the impurities, pulling the pull block 35 will drive the strip plate 34 to move. The movement of the strip plate 34 through the waste tank 37 can remove the collected waste, ensuring the cleanliness of the vacuum chamber 2.

[0061] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A fully transparent, highly airtight vacuum flash evaporation box, characterized in that: The device includes a box body (1), a vacuum chamber (2) is provided inside the box body (1), a vacuum interface (3) is provided on the box body (1) and the vacuum interface (3) is connected to the vacuum chamber (2), a vacuum solenoid valve (4) is connected to the vacuum interface (3), a damping hinge (5) is installed on the side of the box body (1), a box cover (6) is connected to the box body (1) through the damping hinge (5), a sealing gasket (8) is provided on the side of the box cover (6) facing the box body (1), a sealing truncated cone (9) is fixedly provided on the top of the box body (1) and the sealing truncated cone (9) surrounds one side of the vacuum chamber (2), a handle (7) is fixedly connected to one side of the box cover (6), and an acrylic plate (10) is provided inside the box cover (6). The box (1) is provided with an installation box (11) inside, and the installation box (11) is located below the vacuum chamber (2). The installation box (11) is provided with a feeding mechanism for assisting substrate feeding, a compression mechanism, a driving mechanism, and a cleaning mechanism for cleaning the inside of the vacuum chamber (2).

2. The fully transparent, highly airtight vacuum flash evaporation box according to claim 1, characterized in that: The feeding mechanism includes a cylinder (12), a load-bearing plate (13), a push rod (21), and a sealing ring (22). The cylinder (12) is symmetrically arranged inside the box body (1), and both ends of the cylinder (12) are connected to the vacuum chamber (2) and the mounting box (11) respectively. The load-bearing plate (13) is arranged inside the mounting box (11). The push rod (21) passes through the inside of the cylinder (12), and the bottom end of the push rod (21) is fixedly connected to the load-bearing plate (13). The sealing ring (22) is fixedly arranged inside the cylinder (12), and the sealing ring (22) is used to seal the gap between the push rod (21) and the cylinder (12).

3. The fully transparent, highly airtight vacuum flash evaporation box according to claim 2, characterized in that: The drive mechanism includes a threaded ring (14), a drive motor (15), a reducer (16), and a threaded rod (17). The threaded ring (14) is embedded inside the load-bearing plate (13). The drive motor (15) is fixedly installed on the inner wall of the mounting box (11). The reducer (16) is fixed inside the mounting box (11) by a bracket, and the output end of the drive motor (15) is fixedly connected to the input end of the reducer (16). The threaded rod (17) is rotatably installed inside the mounting box (11), and the outer surface of the threaded rod (17) is threadedly connected to the inside of the threaded ring (14). One end of the threaded rod (17) is fixedly connected to the output end of the reducer (16). Guide rods (23) are symmetrically inserted inside the load-bearing plate (13), and the end of the guide rods (23) is fixedly connected to the inner wall of the mounting box (11). A connecting component is provided on the load-bearing plate (13).

4. The fully transparent, highly airtight vacuum flash evaporation box according to claim 3, characterized in that: The connecting assembly includes a strip frame (18), a connecting shaft (19), and a push plate (20). The strip frame (18) is fixed on the top of the load-bearing plate (13), the connecting shafts (19) are arrayed and fixed inside the strip frame (18), and one end of the push plate (20) is movably connected to the corresponding connecting shaft (19).

5. The fully transparent, highly airtight vacuum flash evaporation box according to claim 1, characterized in that: The compression mechanism includes a compression groove (24), a compression block (25), a long plate (26), and a concave frame (27). The compression groove (24) is symmetrically arranged inside the mounting box (11). The compression block (25) is arranged inside the compression groove (24). The long plate (26) is arranged in an array on the compression block (25). The concave frame (27) is fixed at one end of the long plate (26) and is movably connected to the corresponding push plate (20). The mounting box (11) is fixedly provided with a limiting frame (29) corresponding to the long plate (26), and the long plate (26) passes through the limiting frame (29). One end of the compression groove (24) is connected to a conveying pipe (28).

6. The fully transparent, highly airtight vacuum flash evaporation box according to claim 5, characterized in that: The cleaning mechanism includes a diversion channel (30) and jet holes (31). The diversion channel (30) is embedded inside the housing (1) and is located on one side of the vacuum chamber (2). The diversion channel (30) is connected to the other end of the corresponding delivery pipe (28). The jet holes (31) are arranged in an array on the diversion channel (30). A filter screen is provided inside the jet holes (31).

7. A fully transparent, highly airtight vacuum flash evaporation box according to claim 6, characterized in that: The box body (1) is provided with a sliding groove (32) inside, and the sliding groove (32) is located on one side of the vacuum chamber (2). The sliding groove (32) is connected to the vacuum chamber (2). Magnetic plates (33) are symmetrically arranged inside the sliding groove (32). A strip plate (34) is inserted inside the sliding groove (32). A magnetic suction plate (36) corresponding to the magnetic plate (33) is embedded inside the strip plate (34).

8. A fully transparent, highly airtight vacuum flash evaporation box according to claim 7, characterized in that: The strip plate (34) is provided with a waste trough (37) inside, and the waste trough (37) is located on one side of the vacuum chamber (2). A pull block (35) is fixedly provided on the top of the strip plate (34).

9. A fully transparent, highly airtight vacuum flash evaporation box according to claim 3, characterized in that: The front of the box (1) is fixedly provided with a controller (38), and the controller (38) is electrically connected to the drive motor (15). The inside of the mounting box (11) is fixedly provided with a battery assembly (39), and the battery assembly (39) is electrically connected to the drive motor (15).

10. A method for applying a fully transparent, highly airtight vacuum flash evaporation box, applicable to the fully transparent, highly airtight vacuum flash evaporation box as described in any one of claims 1-9, characterized in that, Includes the following steps: S1. Spin-coat the perovskite precursor solution onto the substrate to form a wet film. After spin coating, immediately place the substrate with the wet film into the vacuum chamber (2), then close the box cover (6), and vacuum the vacuum chamber (2) through the vacuum interface (3) for 10 to 60 seconds. After the process is completed, release the vacuum, take out the substrate and perform annealing to obtain a perovskite thin film. S2. The vacuuming process must meet the following requirements: reduce the vacuum level to below 100 Pa within 10 seconds and to below 50 Pa within 30 seconds. S3, the solvent for the perovskite precursor solution is a mixture of DMF and NMP, wherein the active component of the perovskite is FA. X MA 1- X PbI3, where 0.6 ≤ x ≤ 0.8; S4, the active component of perovskite is FA 0.7 MA 0.3 The PbI3 solvent has a DMF to NMP volume ratio of 840:160, the precursor solution has a PbI2 concentration of 2M, and contains MACl at a concentration of 5 mg / ml and PBAI at a concentration of 2 mg / ml; the vacuum treatment lasts for 30 seconds, and the annealing treatment is performed at 100°C for 15 minutes.

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