An automated high-throughput preparation system for perovskite thin films

Abstract

This invention belongs to the field of perovskite optoelectronic materials technology, specifically an automated high-throughput perovskite thin film preparation system. The system includes: a glass substrate gripping device, a solution addition and removal unit, an automatic spin-coating unit, a vacuum flash evaporation unit, and an annealing device. The modules are connected via a communication bus or local area network to achieve bidirectional data and command interaction. The system collects parameters in real time through a unified data bus and stores them in a database, achieving full process traceability. All components are controlled digitally via the I / O interface of a robotic arm, and the program is written through the robotic arm's teach pendant. This invention supports collaborative optimization and iterative processing of workflows using machine learning and generative AI, achieving closed-loop control without human intervention. It utilizes a robotic arm and redundant units to verify multi-dimensional experimental procedures while ensuring emergency response capabilities and experimental breakpoint preservation. It also enables efficient task execution sequence design.

Description

Technical Field

[0001] This invention belongs to the field of perovskite optoelectronic materials technology, specifically relating to an automated high-throughput perovskite thin film preparation device. Background Technology

[0002] Perovskite optoelectronic materials have become important candidate materials for high-efficiency photovoltaic and optoelectronic devices due to their excellent light absorption properties, tunable band gaps, and low-temperature solution preparation characteristics. However, the performance of perovskite thin films is affected by many factors, including solution ratios, additive types, solvent systems, and film formation processes. Traditional artificial preparation methods are inefficient, have poor repeatability, and make it difficult to obtain systematic and traceable data, which seriously restricts the progress of material research and development. At the same time, improving the quality of perovskite thin films requires a large number of trials with additive molecules in the precursor solutions, but manual trial and error methods are difficult to use efficiently to screen suitable additives.

[0003] While existing high-throughput experimental concepts can improve screening efficiency, most equipment is designed for chemical or catalytic systems and lacks precise control over the film formation process of photoelectric thin films. The formation of solvated mesophase and annealing crystallization processes in perovskite systems are complex, and existing systems struggle to achieve precise parameter control and batch-to-batch consistency. Summary of the Invention

[0004] The purpose of this invention is to provide an automated high-throughput preparation system for perovskite thin films to solve the problems of low material preparation efficiency, poor repeatability and lack of process monitoring in the prior art, and to realize the rapid preparation, verification and performance optimization of optoelectronic materials.

[0005] The automated high-throughput perovskite thin film preparation system provided by this invention integrates functional modules such as glass substrate clamping, solution addition and dispensing, automatic spin coating, vacuum flash evaporation, annealing, and in-situ characterization. It realizes automated, standardized, and highly repeatable control of the entire process of perovskite thin film preparation from substrate treatment to film formation and heat treatment, and is suitable for high-throughput experiments and precision process development.

[0006] The system includes a glass substrate clamping unit, a solution addition and removal unit, an automatic spin coating and vacuum flash evaporation unit, and an annealing unit. Each functional unit operates sequentially under the coordination of a unified control system. Among them: The glass substrate gripping unit includes a programmable robotic arm 1 and a sample stage 13 placed on a detachable tray 14. The sample stage 13 is used to place cleaned conductive glass substrates, and the tray structure facilitates quick replacement and batch management. The robotic arm 1 is a six-axis articulated robotic arm with a flexible gripper 18 installed at its end effector, which can stably grip millimeter-sized glass substrates. A pressure sensor 19 is placed near the flexible gripper 18 to detect and adjust the gripping force in real time to prevent the glass substrate from slipping or breaking during the handling process. At the same time, an infrared monitor 20 is arranged on one side of the flexible gripper 18 to identify whether the glass substrate has been successfully gripped or has fallen during the transfer process, thereby improving the reliability and safety of the system operation.

[0007] The solution dispensing unit includes a solution container, a pipette, a pipette holder, a pipette tip box, and disposable pipette tips. The solution container holds multiple glass solution bottles (4 mL in volume) for storing precursor solutions, additives, or solvents. The pipette is fixed to the end of a robotic arm via a pipette holder, and a micro-motor assembly is located on its side. This micro-motor assembly includes two micro-push rods for precise pressing and dispensing of the pipette. During the process of drawing the solution from the solution bottle and dispensing it onto the glass substrate surface, the stroke and speed of the micro-push rods are controlled to ensure consistent dispensing force for each dispensing, thereby guaranteeing the volume accuracy and positional consistency of solution dispensing. Furthermore, the dispensing rate of the pipette and the height between the pipette tip and the glass substrate are adjustable to effectively avoid splashing or bubble generation, improving the uniformity of the film precursor spreading.

[0008] The automatic spin coating and vacuum flash evaporation unit includes a programmable spin coater, a nitrogen blower, a vacuum chuck, and a vacuum flash evaporation device. The spin coater is driven by a servo motor to rotate the vacuum chuck, achieving vacuum adsorption and fixation of the glass substrate. The rotation speed range is 500–20000 rpm, and segmented acceleration and constant speed spin coating programs can be set. The nitrogen blower 8 is controlled by an air pump and performs directional blowing on the film surface during or after spin coating to accelerate solvent evaporation and film formation. The vacuum flash evaporation device 10 is set on the flash evaporation stage 11 to achieve rapid transformation of the perovskite film from a wet film to a semi-dry film state, supporting only one substrate at a time. The flash evaporation stage 11 has a limiting slot 12 in the center to ensure that the glass substrate remains in the same position before and after flash evaporation, thereby avoiding film defects.

[0009] The annealing unit includes a high-precision annealing stage 15, which can heat the film at a maximum temperature of 100℃ (e.g., 90℃-100℃). The annealing unit adopts a PID temperature control system with a temperature control accuracy of ±0.5℃, and supports staged heating and constant temperature program settings. In addition, the annealing unit can be equipped with an in-situ PL fiber optic probe 26 and a fiber optic probe holder 17, so that the film is located below the fiber optic probe during the annealing process, thereby realizing real-time acquisition of in-situ photoluminescence signals.

[0010] A stainless steel bracket 16, 1 mm thick, is installed at the position where the robotic arm 1 picks up and places the glass substrate. This bracket matches the height of the robotic arm's gripper, ensuring a smooth and reliable gripping process. Its cross-section is shown below. Figure 5 As shown.

[0011] The functional modules are connected via a communication bus or local area network to achieve bidirectional transmission of instructions and data; the system collects process parameters in real time and stores them in the database through a unified data bus to achieve full traceability of the preparation process; all equipment is controlled digitally through the robot's IO interface, and the motion program is written and called through the robot's teach pendant, thereby achieving a high degree of automation and modular operation of the system.

[0012] The following describes the interconnections and coordination among the four parts.

[0013] In this invention, the glass substrate clamping unit, the solution addition and removal unit, the automatic spin coating and vacuum flash evaporation unit, and the annealing unit constitute the four core components of the system. These units are sequentially connected and work together under the coordination of a unified control system to achieve fully automated preparation of perovskite thin films from substrate treatment, solution distribution, film formation to heat treatment and characterization.

[0014] The glass substrate gripping unit and the solution dispensing unit are the basic front-end units of the system, and they need to work together. The glass substrate gripping unit is responsible for picking up, placing, transferring and positioning the conductive glass substrate, while the solution dispensing unit completes the quantitative aspiration and precise dispensing of the precursor solution after the glass substrate is stably gripped. The gripping unit synchronizes its actions with the liquid dispensing unit's pipetting actuator through the robot's motion control interface, ensuring positional accuracy and repeatability during the solution dispensing process.

[0015] After solution dispensing is completed, the glass substrate is transferred from the clamping unit to the automatic spin coating and vacuum flash evaporation unit. This unit is connected to the front-end unit via a communication bus to receive the glass substrate arrival signal and automatically start the spin coating program. During spin coating, a vacuum chuck fixes the glass substrate. After spin coating is completed, the glass substrate is transferred to the vacuum flash evaporation device, where it undergoes a transition from a wet film to a semi-dry film under controlled negative pressure. The limiting structure in the flash evaporation stage ensures that the substrate is in the same position before and after processing, thus maintaining good connection with the preceding and following processes.

[0016] The annealing unit is connected to the automatic spin coating and vacuum flash evaporation unit and is used to heat-treat the glass substrate that has completed film formation. The glass substrate is placed in the designated position on the annealing table by the transfer of the robot arm. The annealing unit performs staged heating and constant temperature control according to the preset program, and can simultaneously call the in-situ optical characterization module to monitor the changes in film performance in real time. After annealing, the glass substrate can be taken out again or enter the subsequent process.

[0017] The four units mentioned above achieve bidirectional interaction of commands and data through a communication bus or local area network. All actions are scheduled and managed by a unified control system. This system adopts a multi-layered communication architecture to achieve efficient collaboration and data interaction between the robot and various functional modules. The underlying communication is mainly based on RS232 or EtherCAT bus to complete real-time data exchange. The RS232 bus supports multi-point communication and can connect multiple devices simultaneously, meeting the stable connection requirements under the complex spatial layout of the experimental platform. The EtherCAT bus has higher real-time performance and synchronization accuracy, and is suitable for key process links with high timing control requirements, such as spin coating and air blowing. The robot uses digital IO interfaces to realize the on / off control of various actuators, including pipette pressing, air blowing head start / stop, vacuum pump control, etc. The IO interface response time is less than 10ms to ensure the timeliness and accuracy of action triggering. For parameters that need to be continuously adjusted, such as temperature, pressure, and speed, the system transmits signals through analog IO interfaces to achieve precise setting and real-time feedback.

[0018] Furthermore, the system enables data communication between the host computer and the robotic arm teach pendant via a local area network (LAN), supporting remote monitoring, process parameter setting, and program download. The host computer software can display equipment status, process parameters, and process progress in real time, and supports historical data query and analysis. Infrared monitors, pressure sensors, temperature sensors, and other components configured in each functional module feed back real-time status to the robotic arm control system via I / O interfaces. The robotic arm corrects its actions or handles anomalies based on the feedback information. The system establishes a complete data recording and traceability mechanism, recording millisecond-level timestamps for each operation node, including base plate retrieval. The system records the start and end times of sheet and solution dispensing, spin coating start and stop, air blowing switch, flash evaporation process, and annealing. It also records key action nodes and process parameters, such as the robot's spatial coordinates and attitude angles, gripper opening and closing status and pressure values, liquid transfer volume and pressing force, spin coating speed curve, air blowing pressure and duration, vacuum flash evaporation pressure change curve, annealing temperature curve, and in-situ PL test data. All data is stored in a structured format in a relational database. Each record includes the experimental batch number, sample number, operation type, timestamp, equipment status parameters, and execution result, enabling full-process traceability and efficient statistical analysis.

[0019] The specific operation process of the automated high-throughput perovskite thin film preparation system of the present invention is as follows: (1) Base loading and initialization: The cleaned conductive glass substrate is neatly placed in a replaceable tray-type sample stage. The sample stage is installed in a fixed position in the system to provide stable and repeatable initial coordinates for subsequent automatic sample picking. (2) Robotic arm for picking up and positioning the piece: A programmable six-axis articulated robot moves to the top of the sample stage according to a preset program, grasps a single millimeter-sized glass substrate with a flexible gripper, and completes attitude correction and spatial positioning. The robot controls the opening and closing of the flexible gripper through an I / O interface. (3) Infrared detection of the grasping state; During the gripping process, the robotic arm uses an infrared monitor to determine in real time whether the glass substrate has been successfully gripped or has fallen. If an abnormality is detected, an alarm is triggered or the gripping process is restarted. (4) Transfer of substrate to solution dispensing station: The robotic arm transfers the gripped glass substrate to the designated position in the solution dispensing unit, keeping the substrate horizontal to ensure spatial consistency and positional accuracy of subsequent solution dispensing; (5) Solution sampling and volume control: The solution container holds 4mL glass vials containing precursor solutions, additives, or solvents; the robotic arm drives a push rod via a micro-motor assembly to control the pressing of the pipette; it is linked to the pipette holder via an IO interface to ensure accurate positioning and fixation of the pipette; with disposable pipette tips, the pipette is pressed by the push rod assembly driven by the micro-motor to achieve precise aspiration of the solution; (6) The solution is automatically distributed to the substrate surface: The robotic arm transfers the glass substrate with the solution dispensed to the vacuum chuck of the programmable spin coater and automatically activates the vacuum adsorption mode. The pipette dispenses the perovskite solution onto the surface of the glass substrate to avoid sputtering or bubble generation and to ensure consistency in volume and position. (7) Spin coating and gas-assisted treatment: The robotic arm sends start / stop commands to the spin coater via the IO interface and fixes the substrate using a vacuum suction cup. The spin coating process is driven by a servo motor with a speed range of 500–20000 rpm. The acceleration and holding stages can be controlled in segments. At the same time, a nitrogen blower helps remove the solvent to promote rapid film formation. (8) Vacuum flash evaporation treatment: When needed, the robotic arm controls the vacuum flash evaporation device via the IO interface. The robotic arm transfers the spin-coated substrate to the vacuum flash evaporation device, and the vacuum pump quickly reduces the ambient pressure to realize the transformation of the perovskite film from a wet film to a semi-dry film. The central limiting slot of the flash stage ensures that the position of the sample does not change. (9) Annealing and temperature control: After film formation, the glass substrate is transferred to a high-precision annealing stage. The robotic arm communicates with the PID temperature control system of the annealing stage through the IO interface to set and monitor the annealing temperature curve. Under the control of the PID temperature control system, the heating process is carried out with a temperature control accuracy of ±0.5℃, and it can execute staged heating and constant temperature programs. After annealing, the robotic arm uses a stainless steel support to safely pick up and put down the substrate. (10) In-situ optical inspection and quality assessment (optional): During the annealing process, the perovskite film was monitored in real time using an in-situ PL testing device and an optical fiber support to conduct a preliminary assessment of the film's crystallization quality and uniformity. (11) The robotic arm completes the entire cycle of substrate processing in sequence. When the processed substrate storage box is full, the signal light will light up and notify the personnel to change the material.

[0020] Technical effects of the invention: This invention includes a high-precision solution preparation module and an automated perovskite thin film preparation module, which can realize the precise proportioning, dropping and mixing of multi-component solutions, and complete spin coating and annealing in a controlled environment; it supports real-time control and recording of key parameters (such as volume, dropping rate, temperature and time), and achieves process traceability, data standardization and high repeatability.

[0021] This invention can significantly improve the efficiency and stability of material preparation, providing a reliable technical basis for high-throughput screening and preparation optimization of optoelectronic materials, especially perovskite thin films, and has advantages such as compact structure, high precision, and strong scalability.

[0022] This invention utilizes a high-throughput automated perovskite thin film preparation system to achieve precise control over the entire process, from solution preparation and distribution to thin film formation. It features high efficiency, high throughput, and high repeatability, enabling rapid screening of multi-component materials and optimization of process parameters. The system's continuous data acquisition and recording ensures traceability and standardized management of material composition, process, and performance, providing a reliable basis for experimental optimization and database construction. Its modular design offers excellent scalability, allowing for flexible upgrades or replacements of functional modules based on different material systems. Automated operation significantly reduces human intervention and operational risks, while environmental control and safety protection modules ensure experimental stability and safety. Furthermore, the system has a wide range of applications, extending beyond perovskite thin films to high-throughput preparation and performance optimization of optoelectronic materials, functional thin films, and nanocomposite materials, providing effective support for standardized experimental procedures, cross-laboratory collaboration, and industrialization.

[0023] The main technical features of this invention are: (1) A modular and integrated high-throughput experimental platform that supports collaborative optimization and solution iteration of work processes by machine learning and generative AI, and realizes closed-loop control without human intervention; (2) Verification of multi-dimensional experimental schemes, such as spin coating, characterization, and data processing, using flexible robotic arms and redundant units, while ensuring certain emergency handling capabilities and experimental breakpoint preservation. (3) Integrate multi-source sensors to intelligently monitor platform parameters and introduce AI to write, read and provide feedback on experimental logs to ensure crisis management capabilities and emergency response. (4) A collaborative control scheme for a multi-machine cluster, which adopts node decomposition of the original task space and sub-task space design to carry out multi-objective collaborative decision planning and achieve efficient task execution sequence design. Attached Figure Description

[0024] Figure 1 This refers to the overall appearance of the experimental platform.

[0025] Figure 2 Design a top view for the workbench.

[0026] Figure 3 A multi-functional design for the front end of a robotic arm.

[0027] Figure 4 This is the annealing unit.

[0028] Figure 5 A side view of the gripper holding the conductive glass.

[0029] Figure 6 The flowchart is for the main sequence.

[0030] Figure 7 Comparison of power conversion efficiency between manually spin-coated thin films and high-throughput automated perovskite devices (23 sub-cells each).

[0031] Figure 8 Bar charts and corresponding normal distribution plots of efficiency data prepared by (a) manual and (b) high-throughput processes.

[0032] The following are the labels in the diagram: 1 is the robotic arm, 2 is the solution bottle box, 3 is the pipette tip box, 4 is the pipette tip, 5 is the pipette holder, 6 is the pipette, 7 is the spin coater, 8 is the nitrogen blower, 9 is the vacuum squeegee, 10 is the vacuum flash evaporator, 11 is the flash stage, 12 is the limiting slot, 13 is the sample stage, 14 is the detachable tray, 15 is the annealing stage, 16 is the metal slot, 17 is the light probe holder, 18 is the flexible gripper, 19 is the pressure sensor, 20 is the infrared monitor, 21 is the pipette, 22 is the pipette holder, 23 is the micro motor, 24 is the push rod, 25 is the glass slide, and 26 is the in-situ PL fiber optic probe. Detailed Implementation

[0033] Phase 1: Substrate Modification (SAMs Solution Treatment): This stage primarily involves surface modification of the substrate to provide a suitable interface for perovskite growth. The specific process is as follows: (1) Base preparation and positioning Operation: The operator places the UV-ozone pretreated glass substrate into a removable tray and transfers it into the sample stage in the glove box; Control: Task queue instructions are issued via the robotic arm's touchpad; (2) Basal metastasis Parameters: Robotic arm repeatability ±0.05mm; Action: The robotic arm removes the substrate from the storage box and precisely places it on the high-precision spin coater platform; (3) SAMs solution dropwise addition and spin coating Action: The robotic arm changes to a pipette, aspirates the SAMs solution, and drops it onto the center of the substrate; (4) Heat annealing treatment Action: After the homogenization is completed, the robotic arm transfers the glass substrate to the heating table; Equipment performance: Temperature control accuracy ±0.1℃; (5) Recycling and Storage Action: After annealing, the robotic arm places the substrate into the processed storage box, repeating the operation until the box is full, at which point a signal light indicates that the substrate needs to be changed.

[0034] Phase Two: Perovskite Thin Film Preparation and In-situ Characterization This is a core process step, involving complex solvent engineering and in-situ data monitoring; (1) Perovskite solution deposition Action: The robotic arm moves the substrate that has undergone SAMs treatment to the spin coater; Solution preparation: Perovskite precursor solutions containing specific additive combinations; (2) Spin coating and air blowing off solvent Key equipment: High-precision spin coater with air blower; Process details: During spin coating, air blowing is used through the air blower on the cap to accelerate solvent evaporation; (3) Annealing process under in-situ monitoring: Preliminary annealing and characterization: The robotic arm moves the substrate to the heating stage and begins annealing at 100°C; For in-situ testing (first 5 minutes): Use the in-situ testing interface provided with the heating platform to monitor the following modules: Continue annealing: After 5 minutes of in-situ monitoring, the robotic arm moves the sample to the area next to the heating stage to complete the remaining 25 minutes of annealing process (total annealing time 30 minutes). Example

[0035] Achieving large-area film uniformity using high-throughput air blowing technology This embodiment focuses on verifying the difference in photoelectric efficiency between manually lifting a nitrogen gas gun and using a spin coater's air blowing system to prepare perovskite thin films.

[0036] (A) Experimental objective: To compare the effects of two fabrication methods on the final efficiency of perovskite devices.

[0037] (B) Experimental materials: Wide-bandgap CsFAPbIBr perovskite solution. Specific device structure: FTO / 4PADCB / Cs 0.22 FA 0.78 PbI 2.55 Br 0.45 / PDADI / C 60 / BCP / Ag.

[0038] (C) Experimental procedures and parameters.

[0039] Steps for preparing perovskite thin films and devices: (1) Cleaning of FTO substrate: Commercial FTO conductive glass was ultrasonically cleaned in sequence with neutral detergent, deionized water and ethanol, dried with nitrogen and then placed in an ultraviolet ozone device for 10 minutes. (2) Hole transport layer (4PADCB) deposition: After filtering, 1 mg / mL 4PADCB solution was spin-coated onto FTO substrate (rotation speed: 4000 rpm, time: 30 s), and then annealed on a hot plate at 100 °C for 10 minutes. (3) Preparation of perovskite light-absorbing layer: Weigh CsI, FAI, PbI2 and PbBr2 (I:Br ≈ 85:15) according to stoichiometric ratio, dissolve them in DMF:DMSO (volume ratio 4:1) mixed solvent to prepare a 1.3 M precursor solution; drop the solution onto a 4PADCB / FTO substrate, spin coat at 1000 rpm for 10 s, then accelerate to 6000 rpm for 40 s; after blowing off the solvent, immediately place it on a hot plate at 100℃ for annealing for 30 minutes; (4) Deposition of interface modification layer (PDADI): Dissolve PDADI material in anhydrous ethanol and spin-coat it onto the perovskite surface (rotation speed: 3000 rpm, time: 30 s), and then anneal at 100℃ for 5 minutes.

[0040] To fabricate devices and verify the quality of perovskite thin films: (1) Electron transport layer (C 60 Deposition: High-purity C 60 The powder was placed in a crucible of a thermal evaporation apparatus and subjected to a high vacuum environment (<5×10⁻⁶). -6 Evaporation was carried out at a rate of 0.5–1 Å / s under Torr conditions, with the film thickness controlled at 20–30 nm; (2) Buffer layer (BCP) deposition: In the same vapor deposition system, BCP material is used instead, and in C 60 Further evaporation was carried out on the layer, with the thickness controlled at 6–8 nm and the evaporation rate at approximately 0.1–0.3 Å / s; (3) Top electrode (Ag) vapor deposition: in high vacuum (<5×10 -6 Under Torr conditions, Ag electrodes were deposited by thermal evaporation with a thickness of 80–100 nm and a deposition rate of 2 Å / s. Control group A: The air blowing was turned on 10 seconds before the start of spin coating, and the nitrogen gun was raised to a height of 1 cm above the glass slide with a pressure of 0.2 MPa. Control group B: Air blowing was started 10 seconds before the start of spin coating. The distance between the nitrogen air blower outlet and the glass slide was 1 cm, and the pressure was 0.2 MPa. (4) Characterization and analysis: The JV curves of PSCs were measured at room temperature under AM 1.5G conditions in a nitrogen-filled glove box using a Keithley 2602B source at an intensity of 100 mW cm⁻¹. -2 Calibration was performed using a standard Si solar cell (PVM937, Newport); (5) Proof: The automated platform can achieve highly repeatable thin film preparation by precisely controlling the linkage between spin coating and air blowing (the signal linkage response accuracy is guaranteed by the communication protocol between the robotic arm and the spin coater); In order to compare the final device efficiency of perovskite thin films prepared by two different processes, we continued to complete the high-vacuum evaporation of electron transport layers and metal electrodes; Box diagram ( Figure 7 It contains efficiency values ​​for 23 sub-cells, while the bar chart and normal distribution plot ( Figure 8 The figure shows the average and standard deviation of the two sets of efficiency values. It can be found that when preparing 23 films, the high-throughput automated preparation has higher overall efficiency and better repeatability.

Claims

1. An automated high-throughput perovskite thin film fabrication system, characterized in that, This system integrates functional modules for glass substrate clamping, solution addition and dispensing, automated spin coating, vacuum flash evaporation, annealing, and in-situ characterization, achieving automated, standardized, and highly repeatable control of the entire perovskite thin film process from substrate preparation to film formation and heat treatment. Specifically, it includes a glass substrate clamping unit, a solution addition unit, an automated spin coating and vacuum flash evaporation unit, and an annealing unit. Each functional unit operates sequentially under the coordination of a unified control system. The glass substrate gripping unit includes a programmable robotic arm (1) and a sample stage (13) placed on a detachable tray (14). The sample stage (13) is used to place the cleaned conductive glass substrate, and the tray structure facilitates quick replacement and batch management. The robotic arm (1) is a six-axis articulated robotic arm, and its end effector is equipped with a flexible gripper (18) for stable gripping of millimeter-sized glass substrates. A pressure sensor (19) is set near the flexible gripper (18) to detect and adjust the gripping force in real time to prevent the glass substrate from slipping or breaking during the picking and placing process. An infrared monitor (20) is arranged on one side of the flexible gripper (18) to identify whether the glass substrate has been successfully gripped or has fallen during the transfer process. The solution dispensing unit includes a solution bottle box (2), a pipette (21), a pipette holder (5), a pipette tip box (3), and disposable pipette tips (4). The solution bottle box (2) is used to hold multiple glass solution bottles, which can store precursor solutions, additives, or solvents respectively. The pipette (21) is fixed to the end of the robot arm by a pipette holder (22), and a micro motor assembly (23) is provided on its side. The micro motor assembly includes two micro push rods (23) for precise pressing and dispensing operations of the pipette. During the process of the solution being drawn from the solution bottle and dispensed onto the glass substrate surface, the stroke and speed of the micro push rods are controlled to ensure that the dispensing force is consistent each time, thereby ensuring the volume accuracy and positional consistency of the solution dispensing. In addition, the dispensing rate of the pipette and the height between the tip and the glass substrate can be adjusted to effectively avoid splashing or bubble generation and improve the uniformity of the film precursor spreading. The automatic spin coating and vacuum flash evaporation unit includes a programmable spin coater (7), a nitrogen blower (8), a vacuum chuck (9), and a vacuum flash evaporation device (10). The spin coater (7) is driven by a servo motor to rotate the vacuum chuck (9) to achieve vacuum adsorption and fixation of the glass substrate. The rotation speed range is 500–20000 rpm, and it is equipped with segmented acceleration and constant speed spin coating programs. The nitrogen blower (8) is controlled by an air pump and is used to directionally blow the film surface during or after spin coating to accelerate solvent evaporation and film formation. The vacuum flash evaporation device (10) is set on the flash evaporation stage (11) to achieve rapid transformation of the perovskite film from a wet film to a semi-dry film state. It supports only single substrate processing at a time. The flash evaporation stage (11) has a limiting slot (12) in the center to ensure that the glass substrate remains in the same position before and after flash evaporation, thereby avoiding film defects. The annealing unit includes a high-precision annealing stage (15) for heating the film at a maximum temperature of 100°C. The annealing unit adopts a PID temperature control system with a temperature control accuracy of ±0.5°C and supports staged heating and constant temperature program settings. In addition, the annealing unit can be equipped with an in-situ PL fiber optic probe (26) and a fiber optic probe holder (17) so that the film is located below the fiber optic probe during the annealing process, thereby realizing real-time acquisition of in-situ photoluminescence signals.

2. The automated high-throughput perovskite thin film fabrication system according to claim 1, characterized in that, The various functional modules are connected via a communication bus or local area network to achieve bidirectional transmission of instructions and data; process parameters are collected in real time and stored in the database through a unified data bus to achieve full traceability of the preparation process; all equipment is controlled digitally through the robot's IO interface, and the motion program is written and called through the robot's teach pendant, thereby achieving a high degree of automation and modular operation of the system.

3. The automated high-throughput perovskite thin film fabrication system according to claim 2, characterized in that, The collaborative relationship among the four modules is as follows: The glass substrate gripping unit and the solution dispensing unit are the basic front-end units of the system, and they work together. The glass substrate gripping unit is responsible for picking up, placing, transferring and positioning the conductive glass substrate, while the solution dispensing unit completes the quantitative aspiration and precise dispensing of the precursor solution after the glass substrate is stably gripped. The gripping unit achieves synchronized action with the liquid dispensing unit's pipetting actuator through the robot's motion control interface, ensuring positional accuracy and repeatability during the solution dispensing process. After solution dispensing, the glass substrate is transferred from the clamping unit to the automatic spin coating and vacuum flash evaporation unit. This unit is connected to the front-end unit via a communication bus to receive the glass substrate arrival signal and automatically start the spin coating program. During spin coating, a vacuum chuck fixes the glass substrate. After spin coating, the glass substrate is transferred to the vacuum flash evaporation device, where it undergoes a transition from a wet film to a semi-dry film under controlled negative pressure. The limiting structure in the flash evaporation stage ensures that the substrate is in the same position before and after processing, thus maintaining good connection with the preceding and following processes. The annealing unit is connected to the automatic spin coating and vacuum flash evaporation unit and is used to heat-treat the glass substrate that has completed film formation. The glass substrate is placed in the designated position on the annealing table by the robot. The annealing unit performs staged heating and isothermal control according to the preset program, and simultaneously calls the in-situ optical characterization module to monitor the changes in film performance in real time. After annealing, the glass substrate is taken out again or enters the subsequent process.

4. The automated high-throughput perovskite thin film fabrication system according to claim 3, characterized in that, A multi-layered communication architecture is adopted to achieve efficient collaboration and data interaction between the robotic arm and various functional modules. The underlying communication is based on RS232 or EtherCAT bus to complete real-time data exchange. The RS232 bus supports multi-point communication and can connect multiple devices simultaneously, meeting the stable connection requirements under the complex spatial layout of the experimental platform. The EtherCAT bus has higher real-time performance and synchronization accuracy, and is suitable for critical process links with high timing control requirements, such as spin coating and air blowing. The robotic arm realizes on / off control of various actuators through digital I / O interfaces, including pipette pressing, air blowing head start / stop, and vacuum pump control. The I / O interface response time is less than 10ms to ensure the timeliness and accuracy of action triggering. For parameters that need to be continuously adjusted, such as temperature, pressure, and speed, the system transmits signals through analog I / O interfaces to achieve precise setting and real-time feedback.

5. The automated high-throughput perovskite thin film fabrication system according to claim 4, characterized in that, Data communication between the host computer and the robotic arm teach pendant is achieved through a local area network (LAN), supporting remote monitoring, process parameter setting, and program download. The host computer software displays the equipment status, process parameters, and process progress in real time, and supports historical data query and analysis. Infrared monitors, pressure sensors, and temperature sensors configured in each functional module feed back real-time status to the robotic arm control system via I / O interfaces. The robotic arm corrects its actions or handles anomalies based on the feedback information. The system has established a complete data recording and traceability mechanism, recording millisecond-level timestamps for each operation node, including substrate picking and solution processing. The system allocates start and end times, spin coating start and stop times, air blowing switch times, flash evaporation process times, and annealing time points. It also records key action nodes and process parameters, including the robot's spatial coordinates and attitude angles, gripper opening and closing status and pressure values, liquid transfer volume and pressing force, spin coating speed curve, air blowing pressure and duration, vacuum flash evaporation pressure change curve, annealing temperature curve, and in-situ PL test data. All data is stored in a structured format in a relational database. Each record includes the experimental batch number, sample number, operation type, timestamp, equipment status parameters, and execution result, enabling full-process traceability and efficient statistical analysis.

6. The automated high-throughput perovskite thin film fabrication system according to any one of claims 1-5, characterized in that, The specific operation procedure is as follows: (1) Base loading and initialization: The cleaned conductive glass substrate is neatly placed in a replaceable tray-type sample stage. The sample stage is installed in a fixed position in the system to provide stable and repeatable initial coordinates for subsequent automatic sample picking. (2) Robotic arm for picking up and positioning the piece: A programmable six-axis articulated robot moves to the top of the sample stage according to a preset program, grasps a single millimeter-sized glass substrate with a flexible gripper, and completes attitude correction and spatial positioning. The robot controls the opening and closing of the flexible gripper through an I / O interface. (3) Infrared detection of the grasping state; During the gripping process, the robotic arm uses an infrared monitor to determine in real time whether the glass substrate has been successfully gripped or has fallen. If an abnormality is detected, an alarm is triggered or the gripping process is restarted. (4) Transfer of substrate to solution dispensing station: The robotic arm transfers the gripped glass substrate to the designated position in the solution dispensing unit, keeping the substrate horizontal to ensure spatial consistency and positional accuracy of subsequent solution dispensing; (5) Solution sampling and volume control: The solution bottle box contains 4 mL glass bottles containing precursor solutions, additives, or solvents; the robotic arm drives the push rod through a micro motor assembly to control the pressing of the pipette; the pipette is linked with the pipette holder (22) through the IO interface to ensure accurate positioning and fixation of the pipette; the pipette, with the help of a disposable pipette tip, is pressed by the push rod assembly driven by the micro motor to achieve precise aspiration of the solution; (6) The solution is automatically distributed to the substrate surface: The robotic arm transfers the glass substrate with the solution dispensed to the vacuum chuck of the programmable spin coater and automatically activates the vacuum adsorption mode. The pipette dispenses the perovskite solution onto the surface of the glass substrate to avoid sputtering or bubble generation and to ensure consistency in volume and position. (7) Spin coating and gas-assisted treatment: The robotic arm sends start / stop commands to the spin coater via the IO interface and fixes the substrate using a vacuum suction cup. The spin coating process is driven by a servo motor with a speed range of 500–20000 rpm. The acceleration and holding stages can be controlled in segments. At the same time, a nitrogen blower helps remove the solvent to promote rapid film formation. (8) Vacuum flash evaporation treatment: The robotic arm controls the vacuum flash evaporation device via the IO interface. The robotic arm transfers the spin-coated substrate to the vacuum flash evaporation device, and the vacuum pump quickly reduces the ambient pressure to realize the transformation of the perovskite film from a wet film to a semi-dry film. The central limiting slot of the flash stage ensures that the position of the sample does not change. (9) Annealing and temperature control: After film formation, the glass substrate is transferred to a high-precision annealing stage. The robotic arm communicates with the PID temperature control system of the annealing stage through the IO interface to set and monitor the annealing temperature curve. Under the control of the PID temperature control system, the heating process is carried out with a temperature control accuracy of ±0.5 ℃, and it can execute staged heating and isothermal programs. After annealing, the robotic arm uses a stainless steel support to safely pick up and place the substrate. (10) In-situ optical inspection and quality assessment: During the annealing process, the perovskite film was monitored in real time using an in-situ PL testing device and an optical fiber support to conduct a preliminary assessment of the film's crystallization quality and uniformity. (11) The robotic arm completes the entire cycle of substrate processing in sequence. When the processed substrate storage box is full, the signal light will light up and notify the personnel to change the material.

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