Perovskite thin film preparation control method and platform
By optimizing the spin coating method using time-sensitive grading and dynamic scheduling algorithms, the problem of low production efficiency in spin coating was solved, enabling efficient mass production of perovskite thin films and improving film quality.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- SHENZHEN UNIVERSITY OF ADVANCED TECHNOLOGY
- Filing Date
- 2025-12-19
- Publication Date
- 2026-04-21
AI Technical Summary
The existing spin-coating method for preparing perovskite thin films has low production efficiency and is difficult to meet the needs of mass production.
By employing time-sensitive hierarchical and dynamic scheduling algorithms, the controller coordinates equipment such as robotic arms, pipettes, spin coaters, and hot stages to prioritize the execution of time-sensitive spin coating steps and rationally arrange annealing and cooling steps, thereby achieving efficient production.
It improves the production efficiency of perovskite thin films, shortens the waiting time of production equipment, and improves the quality and consistency of film formation.
Smart Images

Figure CN121908787A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of thin film material preparation technology, and in particular to a method and platform for controlling the preparation of perovskite thin films. Background Technology
[0002] The fabrication of perovskite thin films requires extremely high precision, primarily due to the stringent requirements for photoelectric conversion efficiency, stability, and large-area uniformity. Perovskite thin film fabrication methods are mainly classified into two categories: wet and dry methods. Spin coating is a wet fabrication method widely used due to its low cost and simple process. It involves dropping a precursor solution onto a substrate and then rotating it at high speed to ensure uniform distribution of the solution.
[0003] The problem with existing technologies is that spin coating for perovskite thin film production has low production efficiency, making it difficult to meet the demands of mass production. Summary of the Invention
[0004] The main objective of this invention is to propose a method and platform for controlling the preparation of perovskite thin films, aiming to improve the production efficiency of perovskite thin film products.
[0005] To achieve the above objectives, this invention proposes a method for controlling the preparation of perovskite thin films, comprising the following steps: Load the sample task queue, wherein each sample task includes a preparation execution step, the preparation execution step includes a first preparation step and a second preparation step executed sequentially, and the time sensitivity of the first preparation step is greater than the time sensitivity of the second preparation step; The pre-completion second step task and the pre-start first step task are determined according to the sample task queue; the remaining step duration of the second preparation step in the pre-completion second step task is calculated; When the duration of the remaining steps exceeds the execution duration of the first preparation step in the pre-start first step task, the pre-start first step task is controlled to start execution.
[0006] In one embodiment, the preparation execution step further includes a third preparation step, and the time sensitivity of the second preparation step is greater than that of the third preparation step; After calculating the remaining time of the second preparation step in the pre-completion second step task, the method further includes: When the remaining step duration is less than or equal to the execution duration of the first preparation step in the pre-start first step task, the pre-start third step task is determined according to the sample task queue. When the remaining steps take longer than the duration of the third preparation step in the pre-start third step task, the pre-start third step task is controlled to start execution.
[0007] In one embodiment, the first preparation step includes a spin coating step for forming a thin film on the sample, and the first preparation step is performed continuously until the preset execution time of the first preparation step is reached; The second preparation step includes an annealing step to solidify the film, and the execution time of the second preparation step meets a preset adjustment range; The third preparation step includes cooling and / or spectral measurement. When the robotic arm is detected to be in an idle period, and the idle period is longer than the duration of the third preparation step, the third preparation step is controlled to start execution.
[0008] In one embodiment, the method for controlling the preparation of the perovskite thin film further includes: The film-forming state parameters of the sample are obtained during the annealing step; The control parameters of the current annealing step are adjusted according to the film-forming state parameters and the first preset threshold so that the sample obtains an annealing treatment that is suitable for its film-forming state.
[0009] In one embodiment, the method for controlling the preparation of the perovskite thin film further includes: After the annealing step is completed, obtain the film-forming state parameters of the sample; The film-forming state parameters are compared with a second preset threshold. When the film-forming state parameter is lower than the second preset threshold, the sample is determined to have defects, and subsequent testing steps for the sample are reduced or skipped; and / or, the control parameters of the annealing step for the same batch of samples are adjusted.
[0010] In one embodiment, the film-forming state parameters include color space parameters and / or spectral response characteristics.
[0011] In one embodiment, the method for controlling the preparation of the perovskite thin film further includes: The first step pre-completion task is determined based on the sample task queue; Check whether the equipment resources required for the process after the first preparation step in the first step pre-completion task are idle. If so, continue to execute the process after the first preparation step after completing the first preparation step.
[0012] In one embodiment, each of the sample tasks includes at least one of a first process task, a second process task, and a third process task: the first process task, the second process task, and the third process task each include the preparation execution steps; The first round of process tasks includes a first spin coating step and a first annealing step, which are executed sequentially to form a SAMs layer on the sample; The second round of process tasks includes a second spin coating step and a second annealing step, which are executed sequentially to form a perovskite master layer on the sample; The third round of process tasks includes a third spin coating step and a third annealing step executed sequentially, used to form a passivation layer on the sample; The first preparation step includes a first spin coating step, a second spin coating step, or a third spin coating step; the second preparation step includes a first annealing step, a second annealing step, or the third annealing step.
[0013] In one embodiment, during the first preparation step, the robotic arm is controlled to perform only operations related to the first preparation step; The first preparation step includes dropping liquid, the triggering time of which is calculated in advance, and the triggering time error of the liquid is controlled to be ≤ ±0.2s.
[0014] This invention also proposes a perovskite thin film preparation control platform, comprising: A robotic arm, including grippers for picking up and placing samples; A pipette is used for drawing and dispensing solutions. Pipe tip holder, used to hold pipette tips; Orifice plates are used to hold solutions. Trash cans are used to store discarded gun barrels; A tray for holding samples; Spin coater, used to achieve spin coating; A heated stage for sample annealing; and, The controller is used to control the robotic arm, pipette, spin coater, and hot plate; The controller includes a memory, a processor, and a program for a perovskite thin film preparation control method stored in the memory and executable on the processor. When the program for the perovskite thin film preparation control method is executed by the processor, it implements the steps of the perovskite thin film preparation control method described above. The perovskite thin film preparation control method includes the following steps: Load the sample task queue, wherein each sample task includes a preparation execution step, the preparation execution step includes a first preparation step and a second preparation step executed sequentially, and the time sensitivity of the first preparation step is greater than the time sensitivity of the second preparation step; The pre-completion second step task and the pre-start first step task are determined according to the sample task queue; the remaining step duration of the second preparation step in the pre-completion second step task is calculated; When the duration of the remaining steps exceeds the execution duration of the first preparation step in the pre-start first step task, the pre-start first step task is controlled to start execution.
[0015] The technical solution of this invention includes the preparation execution steps of each sample task in the sample task queue, which includes information on the first preparation step and the second preparation step, to guide production. By determining the pre-completion of the second step task and the pre-start of the first step task, the calculation of the remaining step time of the second preparation step in the pre-completion of the second step task is facilitated. The remaining step time is compared with the execution time of the first preparation step in the pre-start of the first step task. If the remaining step time is larger, it indicates that there is sufficient spare time to execute the first preparation step of the pre-start of the first step task. The controller controls the first preparation step of the pre-start of the first step task to start execution, thereby reducing the waiting time of the production equipment and improving the production efficiency of perovskite thin film samples. Attached Figure Description
[0016] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.
[0017] Figure 1 A schematic flowchart of an embodiment of the perovskite thin film preparation control method provided by the present invention; Figure 2 A schematic diagram of the overall platform flow of an embodiment of the perovskite thin film preparation control method provided by the present invention; Figure 3 A schematic diagram of the dynamic scheduling logic of an embodiment of the perovskite thin film preparation control method provided by the present invention; Figure 4 A schematic diagram of the three-stage process of a single sample in an embodiment of the perovskite thin film preparation control method provided by the present invention; Figure 5 A schematic diagram of the system execution chain of an embodiment of the perovskite thin film preparation control method provided by the present invention; Figure 6 A time sensitivity grading diagram of an embodiment of the perovskite thin film preparation control method provided by the present invention; Figure 7 A schematic diagram of multi-station dynamic scheduling of an embodiment of the perovskite thin film preparation control method provided by the present invention; Figure 8 A schematic diagram of the controller structure in one embodiment of the perovskite thin film preparation control platform provided by the present invention; Figure 9 This is a schematic diagram of an embodiment of the perovskite thin film preparation control platform provided by the present invention.
[0018] Explanation of icon numbers: 1. Spectrometer; 2. Software scheduling server; 3. Robotic arm; 4. Gun head holder; 5. Orifice plate; 6. Tray; 7. Material tray; 8. Spreader; 9. Heating table; 1001. Processor; 1002. Communication bus; 1003. User interface; 1004. Network interface; 1005. Memory.
[0019] The realization of the objective, functional features and advantages of the present invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation
[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0021] It should be noted that if the embodiments of the present invention involve directional indicators (such as up, down, left, right, front, back, etc.), the directional indicators are only used to explain the relative positional relationship and movement of the components in a specific posture. If the specific posture changes, the directional indicators will also change accordingly.
[0022] Furthermore, if the embodiments of this invention involve descriptions such as "first" or "second," these descriptions are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the use of "and / or" or "and / or" throughout the text includes three parallel solutions. For example, "A and / or B" includes solution A, solution B, or a solution where both A and B are satisfied simultaneously. Furthermore, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.
[0023] The fabrication of perovskite thin films requires extremely high precision, primarily due to the stringent requirements for photoelectric conversion efficiency, stability, and large-area uniformity. Perovskite thin film fabrication methods are mainly classified into two categories: wet and dry methods. Spin coating is a wet fabrication method widely used due to its low cost and simple process. It involves dropping a precursor solution onto a substrate and then rotating it at high speed to ensure uniform distribution of the solution.
[0024] The problem with existing technologies is that spin coating is inefficient for producing perovskite thin films, making it difficult to meet the needs of mass production.
[0025] Based on the above reasons, this invention proposes a method for controlling the preparation of perovskite thin films.
[0026] Please see Figures 1-5 In one embodiment of the present invention, the method for controlling the preparation of a perovskite thin film includes the following steps: S10: Load the sample task queue, wherein each sample task includes a preparation execution step, the preparation execution step includes a first preparation step and a second preparation step executed sequentially, and the time sensitivity of the first preparation step is greater than the time sensitivity of the second preparation step; S20: Determine the tasks to be completed in the second step and the tasks to be started in the first step according to the sample task queue; calculate the remaining time of the second preparation step in the tasks to be completed in the second step. S30: When the remaining step duration is longer than the execution duration of the first preparation step in the pre-start first step task, control the pre-start first step task to start execution.
[0027] The technical solution of this invention includes the preparation execution steps of each sample task in the sample task queue, which includes information on the first preparation step and the second preparation step, to guide production. By determining the pre-completion of the second step task and the pre-start of the first step task, the calculation of the remaining step time of the second preparation step in the pre-completion of the second step task is facilitated. The remaining step time is compared with the execution time of the first preparation step in the pre-start of the first step task. If the remaining step time is larger, it indicates that there is sufficient spare time to execute the first preparation step of the pre-start of the first step task. The controller controls the first preparation step of the pre-start of the first step task to start execution, thereby reducing the waiting time of the production equipment and improving the production efficiency of perovskite thin film samples.
[0028] The sample task queue includes multiple sample tasks, each consisting of multiple preparation steps. The first and second preparation steps can be performed consecutively or interspersed with other preparation steps. The first preparation step has a higher time sensitivity than the second preparation step; that is, the first preparation step requires higher time precision than the second preparation step. This can mean that all actions in the first preparation step require high time precision, or that only a few actions require high time precision. The first and second preparation steps can be predetermined. A "pre-complete second step task" refers to a sample task that is currently performing or waiting for the second preparation step, and has the shortest remaining time before completion. A "pre-start first step task" refers to the task in the sample task queue that has the highest priority for execution among those waiting for the first preparation step. When the remaining step time is less than or equal to the execution time of the first preparation step in the "pre-start first step task," the production equipment is controlled to either not perform the operation or execute other executable commands. It is understandable that if the remaining steps take longer than the execution time of the first preparation step in the pre-start first step task, then executing the pre-complete second step task after the first preparation step is completed will not affect the execution time of the second step task or will be within an acceptable preset adjustment range.
[0029] In one embodiment, the preparation execution step further includes a third preparation step, and the time sensitivity of the second preparation step is greater than that of the third preparation step; After calculating the remaining time of the second preparation step in the pre-completion second step task, the method further includes: S31: When the remaining step duration is less than or equal to the execution duration of the first preparation step in the pre-start first step task, the pre-start third step task is determined according to the sample task queue. S32: When the remaining step duration is longer than the duration of the third preparation step in the pre-start third step task, control the pre-start third step task to start execution.
[0030] If the remaining time is less than or equal to the execution time of the first preparation step in the pre-start first step task, the first preparation step cannot be executed. Step S32 determines whether the third step task can be executed. If the remaining time is greater than the time occupied by the third preparation step (i.e., the initial usage time of robotic arm 3 in the third preparation step), then the third preparation step in the pre-start third step task can be executed, thereby reducing the waiting time of the production equipment and improving the production efficiency of perovskite thin film samples. It should be noted that the initial usage time of robotic arm 3 in the entire execution time of the third preparation step is only a short period; robotic arm 3 is not needed in the subsequent execution time and can be processed after the execution time is completed. Furthermore, this processing has low time requirements.
[0031] Similarly, the pre-start third step task refers to the task with the highest priority among the tasks waiting for the third preparation step in the sample task queue. It is understood that if the remaining step duration exceeds the duration of the third preparation step in the pre-start third step task, the pre-completion second step task can be executed after the initial usage time of the robotic arm 3 in the third preparation step is completed. This will not affect the execution time of the second step task or will remain within an acceptable preset adjustment range, while the subsequent execution of the third preparation step can continue.
[0032] In one embodiment, the first preparation step includes a spin coating step for forming a thin film on the sample, and the first preparation step is performed continuously until a preset execution time for the first preparation step is reached; the second preparation step includes an annealing step for curing the thin film, and the execution time of the second preparation step meets a preset adjustment range; the third preparation step includes cooling and / or spectral measurement, and when it is detected that the robotic arm 3 is in an idle period, and the idle period is longer than the occupancy time of the third preparation step, the third preparation step is controlled to start execution.
[0033] The first preparation step, spin coating, includes droplet and sample rotation operations to form a thin film on the sample. The first preparation step is performed continuously until completion and cannot be interrupted by other steps, thus ensuring the accuracy of the timing of each action in the first preparation step and ensuring the film formation effect. The second preparation step solidifies the thin film formed in the spin coating step on the sample through an annealing step. The execution time of the second preparation step can be adjusted to end earlier or later within a preset range. In the third preparation step, cooling is used to cool the sample after annealing. Spectroscopic measurement refers to the detection of the sample by spectrometer 1. When the controller detects that the idle time of the robotic arm 3 is greater than the occupied time of the third preparation step, the third preparation step is executed. After the occupied time of the third preparation step, the robotic arm 3 enters the next idle time.
[0034] The spin coating step includes controlling the robotic arm 3 to pick up the sample, load the nozzle, draw liquid, drip liquid, and rotate the sample. The annealing step refers to the process of placing the sample on the hot stage 9 and cooling it down together with the hot stage 9. Multiple independent annealing stations are set on the hot stage 9 to anneal the sample. Cooling can be done at a specific station or on the material tray 7.
[0035] In practice, the first preparation step may include the complete spin coating process or only the key steps, such as dropping liquid or rotating the sample.
[0036] In one embodiment, the method for controlling the preparation of the perovskite thin film further includes: S40: Obtain film-forming state parameters of the sample during the annealing step; S41: Adjust the control parameters of the current annealing step according to the film formation state parameters and the first preset threshold, so that the sample can obtain an annealing treatment that is suitable for its film formation state.
[0037] By obtaining the film-forming state parameters of the sample during the annealing step and comparing them with the first preset threshold, it can be determined whether the control parameters of the current sample annealing step need to be adjusted so that the annealing treatment matches the film-forming state of the sample and improves the sample film-forming qualification rate.
[0038] The control parameters for the annealing step include, but are not limited to, the execution time of the annealing step and the initial temperature of the annealing step.
[0039] In another embodiment, the method for controlling the preparation of the perovskite thin film further includes: S42: Obtain the film-forming state parameters of the sample after the annealing step is completed; S43: Compare the film-forming state parameters with a second preset threshold; S44: When the film formation state parameter is lower than the second preset threshold, it is determined that the sample has defects, and the subsequent detection steps of the sample are reduced or skipped; and / or, the control parameters of the annealing step of the same batch of samples are adjusted.
[0040] By obtaining the film-forming state parameters of the sample after the annealing step and comparing the film-forming state parameters with a second preset threshold, if the film-forming state parameters are lower than the second preset threshold, the sample has defects, and subsequent tests can be reduced or no tests can be performed, and the sample can be scrapped; or, the annealing step control parameters of the same batch of samples can be adjusted to avoid defects in subsequent samples of the same batch.
[0041] The above two embodiments can coexist, or one of them can be implemented. The first preset threshold and the second preset threshold can be the same or different.
[0042] In one embodiment, the film-forming state parameters include color space parameters and / or spectral response characteristics.
[0043] Color space parameters include RGB, Lab, or other chromaticity parameters, and spectral response characteristics include the characteristic peak positions of absorption spectra, absorption edge variations, or peak positions and intensity characteristics of photoluminescence spectra.
[0044] In one embodiment, the method for controlling the preparation of the perovskite thin film further includes: S50: Determine the first step pre-completion task based on the sample task queue; S51: Check whether the equipment resources required for the process after the first preparation step in the first step pre-completion task are idle. If so, continue to execute the process after the first preparation step after completing the first preparation step.
[0045] After determining the task to be completed in the first step, check whether the equipment resources required for the subsequent processes are available. If they are available, then execute the subsequent processes to avoid interference between tasks.
[0046] Similarly, before executing the second and third preparation steps, the pre-completion tasks for the second and third steps are determined, and the equipment resources required for subsequent processes are checked. When the equipment resources are available, the corresponding process is executed.
[0047] In one embodiment, each of the sample tasks includes at least one of a first process task, a second process task, and a third process task: the first process task, the second process task, and the third process task each include the preparation execution steps; The first round of process tasks includes a first spin coating step and a first annealing step, which are executed sequentially to form a SAMs layer on the sample; The second round of process tasks includes a second spin coating step and a second annealing step, which are executed sequentially to form a perovskite master layer on the sample; The third round of process tasks includes a third spin coating step and a third annealing step executed sequentially, used to form a passivation layer on the sample; The first preparation step includes a first spin coating step, a second spin coating step, or a third spin coating step; the second preparation step includes a first annealing step, a second annealing step, or the third annealing step.
[0048] Each of the sample tasks may include a first-round process task for forming a SAMs layer on the sample, a second-round process task for forming a perovskite master layer on the sample, or a third-round process task for forming a passivation layer on the sample. It may also include two or three of these tasks simultaneously to achieve sample preparation in multiple ways as needed.
[0049] In the specific implementation process, the first preparation step, within the same process cycle, includes one of the following: a first spin coating step, a second spin coating step, and a third spin coating step. Each of these steps may include one or more droplet and sample rotation actions. Similarly, the second preparation step, within the same process cycle, includes one of the following: a first annealing step, a second annealing step, and a third annealing step. Each of these steps may include one or more annealing processes and may include one or more initial annealing temperatures. The specific number of layers spin-coated on the sample surface is not limited; it can be one, two, or four layers.
[0050] In one embodiment, during the first preparation step, the robotic arm 3 is controlled to perform only operations related to the first preparation step; The first preparation step includes dropping liquid, the triggering time of which is calculated in advance, and the triggering time error of the liquid is controlled to be ≤ ±0.2s.
[0051] The first preparation step is highly time-sensitive. The robotic arm 3 only performs relevant operations to ensure the timing accuracy of each action. The control prioritizes the first preparation step with available system resources to reduce action delays caused by insufficient resources. The dropping time can be calculated in advance from the start of the spin coating step in the first preparation step to the dropping trigger, thereby ensuring the accuracy of the dropping trigger. The dropping trigger time error is ≤ ±0.2s to ensure the quality and consistency of the film formation.
[0052] In practice, the trigger time for the droplet can be calculated at the start of the spin-coating step in the first preparation step, or 5 seconds before the droplet trigger time; the specific time is not limited. A trigger time error of ≤±0.2s is a preferred example. In actual operation, the trigger time error can be ≤±0.3s or ≤±0.5s, etc.
[0053] The present invention also proposes a perovskite thin film preparation control platform, which applies a perovskite thin film preparation control method. The perovskite thin film preparation control method refers to the above embodiments. Since the perovskite thin film preparation control platform adopts all the technical solutions of all the above embodiments, it has at least all the beneficial effects brought about by the technical solutions of the above embodiments, which will not be repeated here.
[0054] Reference Figure 9 In one embodiment of the present invention, the perovskite thin film preparation control platform includes: a robotic arm 3, a pipette, a pipette tip holder 4, a perforated plate 5, a trash can 6, a material tray 7, a spin coater 8, a hot plate 9, and a controller.
[0055] The robotic arm 3 includes grippers for picking up and placing samples; a pipette for aspirating and dispensing solutions; a pipette tip holder 4 for holding pipette tips; a well plate 5 for holding solutions; a waste bin 6 for holding discarded pipette tips; a tray 7 for holding samples; a spin coater 8 for spin coating; a hot plate 9 for annealing samples; and a controller for controlling the robotic arm 3, the pipette, the spin coater 8, and the hot plate 9. The controller includes a memory, a processor 1001, and a program for a perovskite thin film preparation control method stored in the memory and executable on the processor 1001. When the program for the perovskite thin film preparation control method is executed by the processor 1001, it implements the steps of the perovskite thin film preparation control method described above.
[0056] The technical solution of this invention uses grippers on a robotic arm 3 to pick up and place samples, placing the samples at a homogenizer for spin coating. A pipette is used to drop the solution onto the sample during the spin coating step. Each time the pipette draws solution from the orifice plate 5 and drops the solution onto the sample, the pipette tip is discarded into the trash can 6 and replaced with a new tip to improve the accuracy of the solution volume during the dropping process. After the spin coating step, the robotic arm 3 transfers the sample to the hot plate 9 for annealing. The tray 7 can hold the initial sample and the processed sample and is used for cooling the sample after annealing. The controller realizes the coordinated operation between the components, thereby automating the sample processing and improving processing efficiency.
[0057] The pipette can be mounted on the robotic arm 3 with grippers, or the robotic arm 3 can be set up separately for pipetting operations.
[0058] This invention aims to provide a robotic platform for fabricating perovskite thin films, which achieves the following through a time-sensitive hierarchical mechanism, a dynamic scheduling algorithm, precise droplet delivery, and uninterrupted control: 1. Millisecond to sub-second precise droplet triggering: Perform antisolvent or additive droplet addition at a specific moment during spin coating with an error of no more than ±0.2s.
[0059] 2. Time-sensitive dynamic scheduling: Prioritize high-sensitivity steps (spin coating steps); The intermediate-sensitivity step (annealing step) determines whether the next wafer can be started based on the remaining time prediction; Low-sensitivity steps (cooling, spectral measurement) are automatically scheduled during idle time.
[0060] 3. Supports high-throughput preparation of multiple samples and variable processes: Different samples have different formulations, annealing times, and testing logics. The system automatically decides the appropriate path instead of a fixed pipeline.
[0061] 4. Automated teaching and spatial adaptability: The coordinates of all workstations are automatically calculated by teaching reference points, which can adapt to the layout of different batches of material trays 7, gun head frame 4, and perforated plate 5.
[0062] 5. Continuous unmanned preparation capability: Automatically completes the entire process of taking samples, loading pipette tips, aspirating liquid, dispensing liquid, spin coating, heating, and testing.
[0063] Through the above-mentioned mechanism, this invention solves the technical problem that traditional automated platforms cannot simultaneously meet the requirements of high-precision timing control and high-throughput preparation of multiple samples.
[0064] The preparation control platform includes: a six-axis robotic arm 3 and grippers, a pipette, a pipette lifting platform, a spin coater 8, a heating stage 9, a spectrometer 1 (for optional online characterization after the process), a glass slide tray 7, a pipette head holder 4, an orifice plate 5, a trash can 6, and a software scheduling server 2, i.e., the controller.
[0065] Robotic arm 3, grippers, pipette, and spin coater 8 are controlled by software modules via API or communication interfaces. Robotic arm 3 includes position movement interfaces such as / move and / moveTo; the pipette provides operations such as / pipette / aspirate and / pipette / dispense; and spin coater 8 provides interfaces such as / spinCoater / start and / spinCoater / suck.
[0066] The preparation control platform includes reference points and a teaching mechanism. The system records the coordinate reference points of each module through the teaching mode, including: the origin reference point ORef, the XRef / YRef direction reference points, the BaseRef operation reference point, the Nest position of the gun holder 4, the orifice plate 5, the material tray 7, the center suction position and the dripping position of the spin coater 8, and the positioning reference point of the hot stage 9.
[0067] The software calculates the positions of all actual workstations and gripping points based on the teaching points, enabling the platform to adapt to different batches of trays 7 and experimental vessels.
[0068] The preparation control platform includes a multi-station dynamic scheduling mechanism. The software scheduling module is responsible for making dynamic decisions across multiple samples, multiple stations, and steps with different time sensitivities. Its main mechanism is as follows: 1. Time sensitivity grading: Based on the degree of time sensitivity, actions are divided into high-sensitivity actions, medium-sensitivity actions, and low-sensitivity actions. High-sensitivity actions correspond to the first preparation step, medium-sensitivity actions correspond to the second preparation step, and low-sensitivity actions correspond to the third preparation step. See appendix. Figure 6 .
[0069] 2. Remaining Time Prediction and Startup Judgment: The scheduling module calculates the remaining annealing time of hot plate 9 in real time to determine whether it is sufficient to execute the complete uninterrupted process of "spin coating to dropping to deceleration". If "remaining annealing time > complete spin coating cycle time": immediately start the next spin coating to increase throughput; if insufficient: prioritize the completion of annealed sample take-off to avoid over-annealing; do not start the high-sensitivity process for new samples.
[0070] 3. High-sensitivity steps cannot be interrupted. During spin coating, the system enters an uninterrupted zone: the robotic arm 3 does not perform operations unrelated to the task, and is not allowed to delay the dripping due to other tasks occupying resources. The dripping action is precisely triggered by advance calculation (error ≤ ±0.2s).
[0071] 4. Multi-sample, variable process control: Considering that different samples may have different formulations, film-forming states, and testing strategies, resulting in variations in the duration of each step in the preparation process and subsequent processing paths, the scheduling module of this invention dynamically controls the sample process based on the detection results, specifically including: The preparation control method includes a dynamic adjustment mechanism for the number of tests based on the detection results. After a sample completes a certain process step, the system can call the detection module to obtain the corresponding film formation state parameters, including but not limited to spectral signal intensity, characteristic absorption peak positions, or other characterization data reflecting film quality. The scheduling module compares the detection results with a preset threshold. When the detection result is lower than the preset quality threshold, the system automatically determines that the sample has low value for subsequent testing and reduces or skips subsequent detection steps, thereby avoiding occupying detection station resources.
[0072] The preparation control method includes a dynamic adjustment mechanism for annealing parameters based on process detection: During or after sample annealing, the system can adjust the annealing timing parameters based on online or offline detection results, such as color space parameters (e.g., RGB, Lab, or other chromaticity parameters) corresponding to film color changes, spectral response characteristics (e.g., characteristic peak positions of absorption spectra, absorption edge changes, or peak positions and intensity characteristics of photoluminescence spectra), and process status signals (e.g., spin coater speed status, hot stage temperature stability status, or actuator feedback signals). The scheduling module automatically adjusts the annealing timing parameters of the corresponding sample according to the judgment results, including extending the current annealing time or ending the annealing process early when conditions are met, so that different samples receive annealing treatment suitable for their film formation state.
[0073] The preparation control method includes a process simplification and queue reconfiguration mechanism based on sample status: the scheduling module maintains a corresponding status identifier for each sample. When the test results indicate that the sample no longer meets the expected quality requirements or does not need to continue with subsequent processes, the system automatically terminates the subsequent sub-tasks for that sample and removes it from the current task queue. Simultaneously, the scheduling module can insert, skip, or reorder the preparation tasks for other samples based on the released workstation resources, thereby achieving dynamic optimization of workstation resources and improving overall preparation throughput under multi-sample conditions.
[0074] The following example uses a 15mm×15mm cleaning glass substrate to demonstrate a three-stage thin film preparation process using this platform. The material system, dosage, and spin-coating parameters can be adjusted according to requirements.
[0075] The first stage of the process involves pre-coating with SAMs (Self-Assembled Monolayers) using DMF as the solvent, with a total concentration of approximately 0.05M to 0.1M. "Approximately" means within a reasonable tolerance range, such as ±0.02M. Ethanol can also be used as the solvent.
[0076] Robotic arm 3 picks up a 15mm × 15mm substrate from glass sheet tray 7 and precisely places it in the center of spin coater 8. Spin coater 8 then activates vacuum adsorption to fix the substrate on the rotating table.
[0077] The robotic arm 3 moves to the pipette tip holder 4, and the pipette descends to pick up a 200μL pipette tip. Then, the robotic arm 3 moves to the well plate 5, and the pipette aspirates 80μL of the bottom solution at a rate of approximately 30μL / s to 50μL / s, where approximately means within a reasonable error range, such as ±5μL / s.
[0078] Spin coater 8 starts single-step spin coating at 3000 rpm for 30 seconds. After spin coating begins, pipettes drop liquid at a distance of about 10 mm from the substrate. "About" means within a reasonable error range, such as ±1 mm. The drop rate is maintained at about 50 μL / s to 80 μL / s to ensure uniform spread of the solution.
[0079] After spin coating, the robotic arm 3 picks up the sample under vacuum, avoiding any tilting, and places it on the heating stage 9 for annealing at 100℃ for 10 minutes (with an allowable fluctuation of ±30 seconds). After annealing, the robotic arm 3 returns the sample to the material tray 7.
[0080] The second process task: to prepare the perovskite master layer film in the second round. The precursor solution adopted a molar ratio of PbI2:MAI:FAI of 1:1:1, the solvent system was DMF:DMSO of 4:1, the total concentration was 1.2M, and the antisolvent was chlorobenzene (CB).
[0081] The robotic arm 3 removes the substrate from the tray 7 again, places it in the center of the spin coater 8, and starts the vacuum.
[0082] After moving to pipette tip holder 4 and taking the pipette tip, pipette draws 80 μL of perovskite precursor solution. Spin coater 8 starts a multi-step spin coating program: the first step is 1000 rpm for 10 s for initial solution spreading; the second step is 5000 rpm for 30 s for rapid film setting.
[0083] After spin coating begins, the pipette is moved to approximately 10 mm above the dispensing orifice and held. When the system timer reaches 27 seconds (i.e., the 17th second of the second spin coating step), the software triggers the dispensing action according to the pre-calibrated movement time, adding 150 μL of chlorobenzene (CB) at a dispensing rate of approximately 150 μL / s. The dispensing timing error is less than ±0.2 s, ensuring the stability of the solvent engineering process.
[0084] After the liquid is dispensed, continue spin coating until 40 seconds have elapsed. The robotic arm 3 picks up the sample and places it on the heating stage 9, where it is annealed at 100°C for 10 minutes, and then returned to the tray 7.
[0085] The third process step involves using a passivating agent solution, typically PEAI (phenylethylamine iodide) or other organic / inorganic passivating agents, with IPA (isopropanol) as the solvent. The concentration is usually set at 10 mg / mL to 20 mg / mL. The following example uses a 15 mg / mL PEAI solution.
[0086] Robotic arm 3 picks up the slide, places it into spin coater 8, and starts vacuum. After the pipette is fitted with a new tip, 50 μL of passivation solution is drawn from well plate 5.
[0087] Spin coater 8 at 4000 rpm for 30 seconds. Approximately 10 seconds after spin coating begins (meaning within a reasonable error range, such as ±1 second), pipette the entire 50 μL passivation solution onto the center of the substrate at a constant speed, allowing it to spread evenly during high-speed spin coating.
[0088] After spin coating, robotic arm 3 moves the sample to heating stage 9 and anneals it at 100°C for 10 minutes to cure the passivation layer. After completion, the sample is returned to the material tray 7.
[0089] The entire process is executed automatically by software, and the drop timing is based on feedback from the spin coater to ensure an accuracy of ±0.2s.
[0090] In the above three-stage process, all actions are controlled by the platform software, including: Robotic arm 3 position control: using commands such as / moveTo to guide the movement from tray 7 to spin coater 8 to hot plate 9; Gripper control: using commands like / gripper / setGripperPosition and / gripper / getGripperStatus to manage substrate gripping and placement; Spin coater management: using commands like / pipette / picUpTip and / pipette / dropTip to automatically change the spin coater tip; Liquid suction / dispensing: using commands like / pipette / aspirate and / pipette / dispense to control the suction speed and volume; Spin coater 8 control: using commands like / spinCoater / setMultiStepParameter and / spinCoater / start to manage the spin speed sequence; Vacuum chuck control: using / spinCoater / suck to fix the substrate; Annealing process execution: Hot plate 9 is uniformly fixed at 100℃, and a timer ensures the accuracy of the annealing time. In actual operation, the temperature of hot plate 9 can be 90℃ or 110℃.
[0091] The software automatically schedules the next action based on the remaining time at each workstation. For example, if there is insufficient time left before the completion of the annealing process on hot station 9, the system will automatically "wait and pick up the film" instead of blindly starting a new process, thus avoiding insufficient annealing or excessive annealing time.
[0092] In the above embodiments, after completing the second or third round of processing, the platform can further call the detection module to evaluate the film-forming state of the sample. As one implementation method, during or after annealing, the sample is rapidly spectrally acquired by spectrometer 1 to obtain its absorption spectral characteristics or characteristic peak intensity information. Alternatively, a camera can be used to take pictures and perform RGB change analysis.
[0093] The software scheduling module compares the test results with a pre-set quality threshold. When the test results indicate that the film formation degree has not yet reached the expected standard, the scheduling module automatically determines that the annealing step of the sample needs to be adjusted, and extends the annealing time parameter of the sample accordingly, for example, by 2 to 5 minutes from the original setting of 10 minutes, until the test results meet the set conditions or reach the maximum allowable annealing time.
[0094] When the test results indicate that the sample film quality is significantly lower than the preset threshold and lacks further characterization value, the scheduling module can automatically cut off the subsequent testing process for that sample, reducing or skipping the spectral detection steps, and removing the sample from the current testing queue. Simultaneously, the system reorders or inserts other sample preparation or testing tasks based on the released workstation resources to improve overall equipment utilization and preparation throughput.
[0095] Through the aforementioned detection-judgment-feedback mechanism, the platform achieves dynamic adaptive scheduling of process parameters and task queues under multi-sample conditions without affecting the execution accuracy of time-sensitive steps.
[0096] The present invention brings the following effects: 1. Precise timing control: Dropping error ≤ ±0.2s, significantly better than manual control.
[0097] 2. High-throughput preparation: The next spin coating can be started during the annealing of one sheet, increasing the throughput by 2 to 5 times or more.
[0098] 3. High repeatability: The timing of dropping and spin coating is strictly consistent in the preparation of multiple samples.
[0099] 4. Flexible application: It can be automatically executed after different formulas and different testing strategies are set, and the process actions can be adaptively adjusted according to the test results.
[0100] 5. The platform is highly versatile: it can be quickly adapted to new material trays 7, gun head holders 4, and vessel layouts through teaching.
[0101] Figure 7 The diagram illustrates the execution time of multiple samples at several key steps. When preparing the 9th sample, the process is paused to wait for the annealing of the 1st sample to complete before restarting. The spin coating step in the diagram includes sample taking, nozzle mounting, liquid aspiration, liquid dispensing, and spin coating on a uniform platform. The total spin coating cycle is 40s spin coating + 25s for pre- and post-processing overhead = 65s. During annealing, each sample is annealed for 600s ± 30s. Other samples can continue spin coating during annealing, but if the remaining annealing time is less than the execution cycle of the next spin coating step, the scheduler will automatically delay the start of the next spin coating step to ensure complete annealing.
[0102] like Figure 8 As shown, the controller may include: a processor 1001, such as a central processing unit (CPU), a communication bus 1002, a user interface 1003, a network interface 1004, and a memory 1005. The communication bus 1002 is used to enable communication between these components. The user interface 1003 may include a display screen or an input unit such as a keyboard; optionally, the user interface 1003 may also include a standard wired interface or a wireless interface. The network interface 1004 may optionally include a standard wired interface or a wireless interface (such as a Wi-Fi interface). The memory 1005 may be a high-speed random access memory (RAM) or a stable non-volatile memory (NVM), such as a disk drive. The memory 1005 may also optionally be a storage device independent of the aforementioned processor 1001.
[0103] Those skilled in the art will understand that Figure 8 The structure shown does not constitute a limitation on the user behavior recognition device and may include more or fewer components than shown, or combine certain components, or have different component arrangements.
[0104] The memory 1005, which serves as a storage medium, may include an operating system, a data storage module, a network communication module, a user interface module, and a perovskite thin film-based preparation control method program.
[0105] The network interface 1004 is mainly used for data communication with the network server; the user interface 1003 is mainly used for data interaction with the user; the processor 1001 and the memory 1005 in the controller of the present invention can be set in the controller, and the controller calls the perovskite thin film preparation control method program stored in the memory 1005 through the processor 1001, and executes the perovskite thin film preparation control method provided in the embodiment of the present invention.
[0106] The above description is merely an exemplary embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the contents of the present invention specification and drawings under the technical concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.
Claims
1. A method for controlling the preparation of perovskite thin films, characterized in that, Includes the following steps: A sample task queue is loaded, wherein each sample task includes a preparation execution step, the preparation execution step includes a first preparation step and a second preparation step executed sequentially, and the time sensitivity of the first preparation step is greater than the time sensitivity of the second preparation step; The pre-completion second step task and the pre-start first step task are determined according to the sample task queue; the remaining step duration of the second preparation step in the pre-completion second step task is calculated; When the duration of the remaining steps exceeds the execution duration of the first preparation step in the pre-start first step task, the pre-start first step task is controlled to start execution.
2. The method for controlling the preparation of perovskite thin films as described in claim 1, characterized in that, The preparation execution steps further include a third preparation step, and the time sensitivity of the second preparation step is greater than that of the third preparation step; After calculating the remaining time of the second preparation step in the pre-completion second step task, the method further includes: When the remaining step duration is less than or equal to the execution duration of the first preparation step in the pre-start first step task, the pre-start third step task is determined according to the sample task queue. When the remaining steps take longer than the duration of the third preparation step in the pre-start third step task, the pre-start third step task is controlled to start execution.
3. The method for controlling the preparation of perovskite thin films as described in claim 2, characterized in that, The first preparation step includes a spin coating step for forming a thin film on the sample. The first preparation step is performed continuously until the preset execution time of the first preparation step is reached. The second preparation step includes an annealing step to solidify the film, and the execution time of the second preparation step meets a preset adjustment range; The third preparation step includes cooling and / or spectral measurement. When the robotic arm is detected to be in an idle period, and the idle period is longer than the duration of the third preparation step, the third preparation step is controlled to start execution.
4. The method for controlling the preparation of perovskite thin films as described in claim 3, characterized in that, The method for controlling the preparation of the perovskite thin film further includes: The film-forming state parameters of the sample are obtained during the annealing step; The control parameters of the current annealing step are adjusted according to the film-forming state parameters and the first preset threshold so that the sample obtains an annealing treatment that is suitable for its film-forming state.
5. The method for controlling the preparation of perovskite thin films as described in claim 3, characterized in that, The method for controlling the preparation of the perovskite thin film further includes: After the annealing step is completed, obtain the film-forming state parameters of the sample; The film-forming state parameters are compared with a second preset threshold. When the film-forming state parameter is lower than the second preset threshold, the sample is determined to have defects, and subsequent testing steps for the sample are reduced or skipped; and / or, the control parameters of the annealing step for the same batch of samples are adjusted.
6. The method for controlling the preparation of perovskite thin films as described in claim 4 or 5, characterized in that, The film-forming state parameters include color space parameters and / or spectral response characteristics.
7. The method for controlling the preparation of perovskite thin films as described in claim 1, characterized in that, The method for controlling the preparation of the perovskite thin film further includes: The first step pre-completion task is determined based on the sample task queue; Check whether the equipment resources required for the process after the first preparation step in the first step pre-completion task are idle. If so, continue to execute the process after the first preparation step after completing the first preparation step.
8. The method for controlling the preparation of perovskite thin films as described in claim 1, characterized in that, Each of the sample tasks includes at least one of a first-round process task, a second-round process task, and a third-round process task: the first-round process task, the second-round process task, and the third-round process task each include the preparation execution steps; The first round of process tasks includes a first spin coating step and a first annealing step, which are executed sequentially to form a SAMs layer on the sample; The second round of process tasks includes a second spin coating step and a second annealing step, which are executed sequentially to form a perovskite master layer on the sample; The third round of process tasks includes a third spin coating step and a third annealing step executed sequentially, used to form a passivation layer on the sample; The first preparation step includes a first spin coating step, a second spin coating step, or a third spin coating step; the second preparation step includes a first annealing step, a second annealing step, or the third annealing step.
9. The method for controlling the preparation of perovskite thin films as described in claim 1, characterized in that, During the first preparation step, the robotic arm is controlled to perform only operations related to the first preparation step; The first preparation step includes dropping liquid, the triggering time of which is calculated in advance, and the triggering time error of the liquid is controlled to be ≤ ±0.2s.
10. A perovskite thin film preparation control platform, characterized in that, include: A robotic arm, including grippers for picking up and placing samples; A pipette is used for drawing and dispensing solutions. Pipe tip holder, used to hold pipette tips; Orifice plates are used to hold solutions. Trash cans are used to store discarded gun barrels; A tray for holding samples; Spin coater, used to achieve spin coating; A heated stage for sample annealing; and, The controller is used to control the robotic arm, pipette, spin coater, and hot plate; The controller includes a memory, a processor, and a program for a perovskite thin film preparation control method stored in the memory and executable on the processor. When the program for the perovskite thin film preparation control method is executed by the processor, it implements the steps of the perovskite thin film preparation control method as described in any one of claims 1 to 9.