A method for analyzing chemical structure evolution of perovskite solar cells in space environment in vacuum in situ

Abstract

This invention discloses a method for in-situ vacuum chemical structure evolution analysis of perovskite solar cells under space environment effects, belonging to the technical field of in-situ vacuum chemical structure evolution analysis of batteries. The method includes the following steps: Based on an ultra-high vacuum interconnected integrated device, the perovskite solar cell is mounted on a flag-shaped sample holder, and a vacuum operation is performed; when the vacuum reaches a preset level, it is transferred to the sample placement position in the sample chamber via a sample transfer rod; then, it is transferred to a comprehensive environmental simulation chamber for environmental simulation processing via a robotic arm; after the environmental simulation processing is completed, it is transferred to the sample placement position in the transfer chamber of an X-ray photoelectron spectrometer, and then transferred to the X-ray photoelectron spectrometer for in-situ chemical structure evolution analysis. This invention can avoid the additional effects of water / oxygen in the natural environment on perovskite solar cell materials and restore their structural evolution law under the influence of various extreme space environmental factors.

Description

Technical Field

[0001] This invention belongs to the field of vacuum in-situ chemical structure evolution analysis technology for batteries, and particularly relates to a method for vacuum in-situ chemical structure evolution analysis of perovskite solar cells under space environment effects. Background Technology

[0002] Perovskite solar cells, as a popular research material system in third-generation solar cells, have attracted considerable attention due to their advantages such as low manufacturing cost, simple fabrication process, environmental friendliness, and high conversion efficiency. They hold the potential to replace first- and second-generation solar cells in the aerospace field, becoming a new energy supply material for airships, drones, spacecraft, and the International Space Station. However, to advance the application of perovskite solar cells in the aerospace field, it is necessary to explore their environmental effects under extreme space environments, mainly including obtaining the evolution laws and mechanisms of their microstructure under various single or coupled space environmental factors.

[0003] Among various microstructural characterization methods for perovskite solar cells, obtaining the evolution of their chemical structure is an essential means of revealing their space environment effects. It allows for precise determination of the existence state and concentration distribution of each element in the perovskite solar cell, as well as the chemical composition and chemical state changes at the interfaces of each functional layer. This information is of great guiding significance for optimizing device structure and fabrication processes, and for revealing the stability and photoelectric performance of perovskite solar cell materials.

[0004] While some research has focused on the evolution mechanism of the chemical structure of perovskite solar cell materials / devices under space environmental factors such as vacuum, high and low temperatures, particle irradiation, and electromagnetic radiation, all research paradigms are based on chemical structure characterization independent of the fabrication equipment or environmental simulation devices. Specifically, these studies often involve environmental treatment of materials or devices in ground-based space environment simulation devices, followed by removal from the simulated vacuum chamber and placement in structural characterization equipment for characterization and analysis. This results in perovskite solar cell materials / devices being exposed to the natural environment for short or long periods during the transfer process. Because their sensitivity to environmental factors such as water, oxygen, and light leads to additional performance degradation effects, it is impossible to obtain the true chemical structure evolution patterns under the influence of the space environment. This, to some extent, limits the acquisition of the true chemical structure evolution process and the elucidation of the evolution mechanism of perovskite solar cells under extreme space environments.

[0005] Therefore, there is an urgent need to provide a vacuum in-situ chemical structure evolution analysis method for perovskite solar cells to address space environment effects. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention proposes a vacuum in-situ chemical structure evolution analysis method for perovskite solar cells under space environment effects. By connecting environmental simulation equipment and chemical structure characterization equipment, an integrated ultra-high vacuum system is constructed. This ensures the continuity of the ultra-high vacuum environment for perovskite solar cell materials throughout the entire process from environmental simulation to chemical structure characterization, avoiding additional effects caused by water / oxygen in the natural environment. This allows for the reconstruction of the structural evolution law under the influence of various extreme space environment factors, thereby solving the problems existing in the prior art.

[0007] To achieve the above objectives, this invention provides a method for in-situ vacuum chemical structure evolution analysis of perovskite solar cells under space environment effects, comprising the following steps:

[0008] Based on the ultra-high vacuum interconnection integrated device, the perovskite solar cell was installed on the flag-shaped sample holder and a vacuuming operation was performed.

[0009] When the vacuum reaches the preset level, the flag-shaped sample holder is transferred to the sample placement position in the sample cavity based on the sample transfer rod;

[0010] The flag-shaped sample holder is transferred from the sample storage position in the sample cavity to the integrated environmental simulation chamber for environmental simulation processing based on the rotation of the robotic arm.

[0011] After the environmental simulation process is completed, the flag-shaped sample holder is returned to the sample storage position in the transfer cavity of the X-ray photoelectron spectrometer.

[0012] The flag-shaped sample holder is transferred from the sample storage position in the transfer cavity of the X-ray photoelectron spectrometer to the X-ray photoelectron spectrometer for in-situ chemical structure evolution analysis.

[0013] Optionally, the flag-shaped sample holder is placed in the cavity of the ultra-high vacuum interconnection integrated device.

[0014] Optionally, the perovskite solar cell is prepared in a glove box before being mounted onto the flag-shaped sample holder.

[0015] Optionally, before mounting the perovskite solar cell onto the flag-shaped sample holder and performing the vacuuming operation, the process further includes: filling the sample cavity with Ar gas to break the vacuum until the door between the glove box and the sample cavity is opened.

[0016] Optionally, the sample transfer rod includes a first sample transfer rod and a second sample transfer rod;

[0017] The process of mounting the perovskite solar cell onto the flag-shaped sample holder and performing a vacuuming operation includes: placing the flag-shaped sample holder in the sample parking position of the first sample transfer rod and performing a vacuuming operation.

[0018] Optionally, when the vacuum reaches a preset level, the process of transferring the flag-shaped sample holder to the sample storage position of the sample cavity based on the sample transfer rod includes: transferring the flag-shaped sample holder from the sample storage position of the first sample transfer rod to the sample storage position of the sample cavity based on the second sample transfer rod.

[0019] Optionally, the transfer path for conveying the flag-shaped sample holder from the sample placement position in the sample cavity to the integrated environmental simulation chamber based on the rotation of the robotic arm is as follows:

[0020] The flag-shaped sample holder is picked up from the sample storage position in the sample chamber by the robotic arm of UFO0 and transferred to the sample storage position between UFO0 and UFO1. The flag-shaped sample holder is then transferred to the sample storage position between UFO1 and UFO2 by the robotic arm of UFO1. Finally, the flag-shaped sample holder is transferred to the integrated environmental simulation chamber by the robotic arm of UFO2.

[0021] Optionally, before transferring the flag-shaped sample holder from the sample storage position of the sample cavity to the integrated environmental simulation chamber for environmental simulation processing based on the rotation of the robotic arm, the method further includes: opening the gate valve between the sample cavity and the UFO0, and removing the flag-shaped sample holder from the sample storage position of the sample cavity by the robotic arm.

[0022] Optionally, the process of transferring the flag-shaped sample holder from the sample placement position in the transfer cavity of the X-ray photoelectron spectrometer to the X-ray photoelectron spectrometer includes: lowering the sample placement position in the transfer cavity of the X-ray photoelectron spectrometer to the height of the high-temperature and high-pressure reaction cell based on the vertical sample rod, and then transferring the flag-shaped sample holder to the X-ray photoelectron spectrometer for testing based on the swing rod.

[0023] Optionally, the preset level of the vacuum is on the order of E-10 mbar.

[0024] Compared with the prior art, the present invention has the following advantages and technical effects:

[0025] The present invention proposes an ultra-high vacuum in-situ chemical structure evolution analysis method for perovskite solar cells under space environment effects. This method conducts ground-based space environment simulation experiments on perovskite solar cells. After completing the simulation experiments, in-situ chemical structure characterization under ultra-high vacuum conditions can be directly performed. This ensures that the perovskite solar cell material maintains the continuity of the ultra-high vacuum environment throughout the entire process from environmental simulation to chemical structure characterization, avoiding additional effects caused by water / oxygen in the natural environment. This allows for the reconstruction of its structural evolution law under the influence of various extreme space environment factors, and the acquisition of the true chemical structure evolution law under the influence of the space environment. Attached Figure Description

[0026] The accompanying drawings, which form part of this application, are used to provide a further understanding of this application. The illustrative embodiments and descriptions of this application are used to explain this application and do not constitute an undue limitation of this application. In the drawings:

[0027] Figure 1 This is a partial structural diagram of the ultra-high vacuum interconnection integrated device according to an embodiment of the present invention;

[0028] Figure 2 This is a schematic diagram of the structure of the ultra-high vacuum interconnection integrated device according to an embodiment of the present invention. Detailed Implementation

[0029] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. This application will now be described in detail with reference to the accompanying drawings and embodiments.

[0030] It should be noted that the steps shown in the flowchart in the accompanying drawings can be executed in a computer system such as a set of computer-executable instructions, and although a logical order is shown in the flowchart, in some cases the steps shown or described may be executed in a different order than that shown here.

[0031] Revealing the microscopic mechanisms of space environment effects on perovskite solar cell materials / devices is the cornerstone for their application in the aerospace field, determining the direction of their material design, structural optimization, and protective measures. Although ground-based simulation experiments of space environment for perovskite solar cell materials / devices have been successively launched, the additional effects caused by the discontinuous environment during the research on the environmental effects of perovskite solar cell materials / devices, resulting from the natural environment, have hindered the characterization of their chemical structure and the revelation of their microscopic mechanisms under the influence of the space environment.

[0032] To address the aforementioned problems, this invention proposes a method for in-situ chemical structure evolution analysis of perovskite solar cells under space environment effects in ultra-high vacuum, comprising the following steps:

[0033] Based on the ultra-high vacuum interconnection integrated device, the perovskite solar cell was installed on the flag-shaped sample holder and a vacuuming operation was performed.

[0034] When the vacuum reaches the preset level, the flag-shaped sample holder is transferred to the sample placement position of LL0 based on the sample transfer rod;

[0035] The flag-shaped sample holder is transferred from the sample parking position of the LL0 to the integrated environmental simulation chamber for environmental simulation processing based on the rotation of the robotic arm.

[0036] After the environmental simulation process is completed, the flag-shaped sample holder is returned to the sample storage position in the transfer cavity of the X-ray photoelectron spectrometer.

[0037] The flag-shaped sample holder is transferred from the sample storage position in the transfer cavity of the X-ray photoelectron spectrometer to the X-ray photoelectron spectrometer for in-situ chemical structure evolution analysis.

[0038] like Figures 1-2 As shown, this embodiment of the invention achieves continuity of the ultra-high vacuum environment in the preparation, environmental simulation, and chemical structure characterization process of perovskite solar cell materials by constructing an ultra-high vacuum interconnection integrated device, thus avoiding the influence of the natural environment and providing a reliable characterization and analysis method for studying the evolution of the chemical structure of perovskite solar cell materials / devices under the space environment effect.

[0039] As a specific embodiment, the process of installing perovskite solar cells onto flag-shaped sample holders and performing vacuuming operations based on the ultra-high vacuum interconnected integrated device includes: installing the perovskite solar cells prepared in the glove box onto structurally compatible flag-shaped sample holders in each cavity of the ultra-high vacuum interconnected integrated device; breaking the vacuum by filling the rapid sample introduction chamber 0 (LL0) with Ar gas until the door between the glove box and LL0 is opened; placing the flag-shaped sample holder in the sample parking position of the first sample transfer rod; closing the door; and performing vacuuming operations on LL0.

[0040] As a specific embodiment, when the vacuum reaches a preset level, the specific implementation process of transferring the flag-shaped sample holder to the sample parking position of LL0 based on the sample transfer rod includes: after the vacuum reaches the E-7mbar level, the sample is taken from the parking position on the first sample transfer rod through the second sample transfer rod and placed in the sample parking position of LL0.

[0041] As a specific embodiment, the specific implementation process of transferring the flag-shaped sample holder from the sample parking position of LL0 to the integrated environmental simulation chamber for environmental simulation processing based on the rotation of the robotic arm includes: opening the gate valve between LL0 and UFO0, and removing the sample from the sample parking position of LL0 through the robotic arm of UFO0; rotating the robotic arm to transfer the sample to the sample cavity between UFO0 and UFO1 for parking, grabbing the sample through the robotic arm of UFO1 and transferring it to the sample cavity between UFO1 and UFO2, and finally transferring the sample to the integrated environmental simulation chamber for environmental simulation processing through the robotic arm of UFO2; after the environmental simulation test is completed, the sample is returned along the original path to the sample cavity before UFO0 and UFO1 for parking, and then transferred to the transfer cavity of the X-ray photoelectron spectrometer through the robotic arm of UFO0.

[0042] As a specific embodiment, the specific implementation process of transferring the flag-shaped sample holder from the sample placement position in the transfer cavity of the X-ray photoelectron spectrometer to the X-ray photoelectron spectrometer for in-situ chemical structure evolution analysis includes: the robotic arm rotates to the transfer cavity and places the sample in the sample placement position of the transfer cavity of the X-ray photoelectron spectrometer; the placement position is lowered to the height of the high-temperature and high-pressure reaction cell by a vertical sample rod; the sample is then transferred to the X-ray photoelectron spectrometer for analysis by a swing rod.

[0043] Transfer path design: Perovskite solar cells are prepared in a gaseous environment protected by inert gas Ar. The obtained perovskite solar cell materials are transferred and moved between various ultra-high vacuum devices through structures such as sample transfer rods and robotic arms.

[0044] In summary, the method for analyzing the evolution of perovskite solar cell chemical structure in ultra-high vacuum under space environment effects proposed in this invention includes:

[0045] Space environment simulation test design: Perovskite solar cell materials / devices are transferred to a gas environment simulation chamber that interfaces with the interconnected system, which can simulate environmental factors such as vacuum, high and low temperatures, ultraviolet radiation, electron radiation, and atomic oxygen in space.

[0046] In-situ chemical structure characterization test design: After the perovskite solar cell materials / devices undergo environmental simulation tests in the gas integrated environment simulation chamber, the samples can be directly transferred to the X-ray photoelectron spectrometer through the circular sample transfer chamber, the lifting ladder structure, the sample transfer rod and the robotic arm for characterization tests of the material composition evolution under the influence of the space environment.

[0047] The perovskite solar cell space environment effect ultra-high vacuum in-situ chemical structure evolution analysis method proposed in this invention ensures that perovskite solar cells can be subjected to ground space environment simulation experiments without exposure to the atmosphere. After the simulation experiment is completed, in-situ chemical structure characterization under ultra-high vacuum environment can be directly performed, thereby eliminating the additional effects of the natural environment on the material during the process.

[0048] This invention provides a technical solution for obtaining the true chemical structure evolution of perovskite solar cell materials / devices under the influence of the space environment through in-situ chemical structure characterization technology. This avoids the additional effects of the natural environment and restores the true service evolution process of the chemical structure of perovskite solar cell materials / devices. This lays a solid foundation for revealing the space environment effects of perovskite solar cells and for their application in the aerospace field.

[0049] The above are merely preferred embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A method for analyzing chemical structure evolution of perovskite solar cells in space environment effect vacuum in-situ, characterized in that, The method comprises the following steps: Based on the ultra-high vacuum interconnection integrated device, the perovskite solar cell is installed on the flag-shaped sample holder, and vacuumizing operation is performed; When the vacuum reaches the preset level, the flag-shaped sample holder is transferred to the sample parking position of the sample chamber based on the sample transfer rod; Based on the mechanical arm rotation, the flag-shaped sample holder is transferred from the sample parking position of the sample chamber to the comprehensive environmental simulation cabin for environmental simulation processing; After the environmental simulation processing is completed, the flag-shaped sample holder is returned and transferred to the sample parking position of the sample transfer cavity of the X-ray photoelectron spectrometer; The flag-shaped sample holder is transferred from the sample parking position of the sample transfer cavity of the X-ray photoelectron spectrometer to the X-ray photoelectron spectrometer for in-situ chemical structure evolution analysis; The sample transfer rod comprises a first sample transfer rod and a second sample transfer rod; The process of installing the perovskite solar cell on the flag-shaped sample holder and performing vacuumizing operation comprises: placing the flag-shaped sample holder in the sample parking position of the first sample transfer rod for vacuumizing operation; When the vacuum reaches the preset level, the flag-shaped sample holder is transferred to the sample parking position of the sample chamber based on the sample transfer rod; The transfer path of the flag-shaped sample holder from the sample parking position of the sample chamber to the comprehensive environmental simulation cabin based on the mechanical arm rotation is: Open the gate valve between the sample chamber and UFO0, grab the flag-shaped sample holder from the sample parking position of the sample chamber by the mechanical arm of UFO0, transfer it to the sample parking position between UFO0 and UFO1, transfer the flag-shaped sample holder to the sample parking position between UFO1 and UFO2 by the mechanical arm of UFO1, and finally transfer the flag-shaped sample holder to the comprehensive environmental simulation cabin by the mechanical arm of UFO2.

2. The perovskite solar cell space environment effect vacuum in-situ chemical structure evolution analysis method according to claim 1, wherein the flag-shaped sample holder is placed in the cavity of the ultra-high vacuum interconnection integrated device.

3. The perovskite solar cell space environment effect vacuum in-situ chemical structure evolution analysis method according to claim 1, wherein before the perovskite solar cell is installed on the flag-shaped sample holder, the perovskite solar cell is prepared in a glove box.

4. The perovskite solar cell space environment effect vacuum in-situ chemical structure evolution analysis method according to claim 3, wherein before the perovskite solar cell is installed on the flag-shaped sample holder and vacuumizing operation is performed, Ar gas is filled in the sample chamber for vacuum breaking operation until the hatch between the glove box and the sample chamber is opened.

5. The perovskite solar cell space environment effect vacuum in-situ chemical structure evolution analysis method according to claim 1, wherein ​ ​ ​ Before the flag-shaped sample holder is transferred from the sample parking position of the sample cavity to the comprehensive environmental simulation cabin for environmental simulation treatment based on the rotation of the mechanical arm, further comprising: opening the gate valve between the sample cavity and the UFO0, and taking the flag-shaped sample holder from the sample parking position of the sample cavity by the mechanical arm.

6. The method of claim 1, wherein the method is characterized in that, The process of transferring the flag-shaped sample holder from the sample parking position of the X-ray photoelectron spectrometer transfer cavity to the X-ray photoelectron spectrometer comprises: lowering the sample parking position of the X-ray photoelectron spectrometer transfer cavity to the height of the high-temperature high-pressure reaction pool based on the vertical sample rod, and then transferring the flag-shaped sample holder to the X-ray photoelectron spectrometer to be tested based on the swing rod.

7. The method of claim 1, wherein the method is characterized in that, The preset magnitude of the vacuum is E-10 mbar.

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