Piezoelectric thin film preparation apparatus and method of preparing the same

Abstract

The application provides a piezoelectric thin film preparation device and a preparation method thereof. The piezoelectric thin film preparation device comprises a deposition growth cavity module and an annealing cavity structure. The deposition growth cavity module comprises at least an adhesion electrode deposition cavity structure, a buffer deposition cavity structure, a seed deposition cavity structure and a piezoelectric deposition cavity structure. The annealing cavity structure is configured to anneal at least the seed layer and / or the piezoelectric film layer to finally form the piezoelectric thin film. The piezoelectric thin film preparation device of the application additionally provides the seed deposition cavity structure, so that low-energy nucleation points can be formed on the surface of the buffer layer, so that the atoms of the piezoelectric film layer can be directly oriented and rapidly sputtered on the cell template, so as to reduce the nucleation activation energy, thereby effectively reducing the crystallization temperature of the atoms. At the same time, the annealing cavity structure can inject high temperature, so that the atoms can rapidly crystallize on the cell template, and the substrate still maintains low temperature in a short period of time, thereby reducing the influence on the substrate through the dual effects of rapid crystallization of the atoms and reduction of the nucleation activation energy.

Description

Technical Field

[0001] This application relates to the field of piezoelectric material equipment technology, and in particular to a piezoelectric thin film preparation device and its preparation method. Background Technology

[0002] Piezoelectric thin films are core materials for radio frequency filters, ultrasonic transducers, energy harvesters, and micro / nano sensors. Specifically, a piezoelectric thin film includes a substrate and functional layers such as the piezoelectric film layer deposited on the substrate.

[0003] Currently, the fabrication process of piezoelectric thin films is constrained by high-temperature processes. That is, the traditional crystallization temperature of functional films such as piezoelectric films is usually relatively high (e.g., above 600℃), while the melting point of the substrates used in some applications is usually relatively low. Therefore, it is impossible to deposit functional layers such as piezoelectric films on low-melting-point substrates to prepare piezoelectric thin films required for special applications. Summary of the Invention

[0004] The purpose of this application is to provide a piezoelectric thin film preparation device and method, which aims to solve the problem of how to deposit piezoelectric film layers on low-melting-point substrates to form piezoelectric thin films required for certain applications.

[0005] In a first aspect, embodiments of this application provide a piezoelectric thin film preparation apparatus, including a deposition growth chamber module and an annealing chamber structure; The deposition growth chamber module includes at least an adhesive electrode deposition chamber structure for depositing an adhesion layer on a substrate and depositing a bottom electrode layer on the adhesion layer, a buffer deposition chamber structure for depositing a buffer layer on the bottom electrode layer, a seed deposition chamber structure for depositing a seed layer on the buffer layer, and a piezoelectric deposition chamber structure for depositing a piezoelectric film layer on the seed layer; the annealing chamber structure is configured to anneal at least the seed layer and / or the piezoelectric film layer.

[0006] In some embodiments, the piezoelectric thin film preparation equipment further includes an in-situ detection module and a central control module electrically connected to the deposition growth chamber module and the in-situ detection module, respectively. The in-situ detection module is used to detect deposition information in the deposition growth chamber module, and the central control module controls the working state of the deposition growth chamber module according to the deposition information. The deposition information includes at least one of stress value, resistance information, film thickness information and temperature information.

[0007] In some embodiments, the in-situ detection module includes a stress detection element disposed within the seed deposition chamber structure and configured to detect the stress value of the seed layer. The central control module is used to control the seed deposition chamber structure to stop depositing the seed layer when the stress value is greater than a preset value, and to control the annealing chamber structure to perform stress annealing on the seed layer. And / or, the in-situ detection module further includes a resistance detection element disposed within the adhesive electrode deposition cavity structure, and configured to detect the resistance information of the adhesive layer and / or the bottom electrode layer; the central control module controls the start and stop of the adhesive electrode deposition cavity structure according to the resistance information; And / or, the in-situ detection module further includes a film thickness detection element disposed within the piezoelectric deposition cavity structure, the film thickness detection element being configured to detect the film thickness information of the piezoelectric film layer, and the central control module controlling the start and stop of the piezoelectric deposition cavity structure based on the film thickness information; And / or, the in-situ detection module further includes a temperature detection element disposed within the annealing chamber structure, the temperature detection element being configured to detect temperature information within the annealing chamber structure, and the central control module adjusting the annealing temperature within the annealing chamber structure according to the temperature information; And / or, the piezoelectric thin film preparation equipment further includes a resistance detection chamber module that can communicate with the deposition growth chamber module. The resistance detection chamber module is provided with a resistance detection device that is electrically connected to the central control module and is configured to perform resistance detection on at least the buffer layer, the seed layer, or the piezoelectric film layer transferred to the resistance detection chamber module to obtain a resistance result. The central control module controls the start and stop of the deposition growth chamber module according to the resistance result.

[0008] In some embodiments, the piezoelectric thin film preparation equipment includes a central control module, and a plasma detection element electrically connected to the central control module is disposed in the piezoelectric deposition cavity structure and configured to detect the ion concentration of the piezoelectric material in the piezoelectric deposition cavity structure. The central control module adjusts the working state of the piezoelectric deposition cavity structure according to the ion concentration.

[0009] In some embodiments, the piezoelectric deposition chamber structure is further provided with a flow detection element electrically connected to the central control module, which is configured to detect the flow rate of the reaction gas delivered to the piezoelectric deposition chamber structure, and the central control module controls the delivery flow rate of the reaction gas by comparing the flow rate with a preset flow rate range.

[0010] In some embodiments, the piezoelectric thin film preparation equipment includes a vacuum transfer chamber and an automatic transfer mechanism disposed within the vacuum transfer chamber; The vacuum transfer cavity is connected to the adhesive electrode deposition cavity structure, the buffer deposition cavity structure, the seed deposition cavity structure, the piezoelectric deposition cavity structure, and the annealing cavity structure in a switchable manner. The automatic transfer mechanism is used to transfer the substrate from any one of the adhesive electrode deposition cavity structure, the buffer deposition cavity structure, the seed deposition cavity structure, the piezoelectric deposition cavity structure, and the annealing cavity structure to another via the vacuum transfer cavity.

[0011] In some embodiments, the piezoelectric thin film preparation equipment includes a central control module, the automatic transfer mechanism includes a robotic arm, the robotic arm being electrically connected to the central control module; and / or, the vacuum transfer chamber is provided with control valves for controlling the on / off state between each of the adhesive electrode deposition chamber structure, the buffer deposition chamber structure, the seed deposition chamber structure, the piezoelectric deposition chamber structure, and the annealing chamber structure, the control valves being electrically connected to the central control module; And / or, the adhesive electrode deposition cavity structure, the buffer deposition cavity structure, the seed deposition cavity structure, the piezoelectric deposition cavity structure and the annealing cavity structure are arranged circumferentially around the vacuum transfer cavity.

[0012] In some embodiments, the piezoelectric thin film fabrication apparatus further includes a pretreatment front-end module configured to pretreat the substrate; A load locking chamber is provided between the pretreatment front-end module and the vacuum transfer chamber, and the load locking chamber is connected to both the pretreatment front-end module and the vacuum transfer chamber.

[0013] In some embodiments, both the buffer deposition cavity structure and the piezoelectric deposition cavity structure include a first cavity shell, a first sample platform disposed within the first cavity shell and used to support a substrate, a target platform used to support a target, a power supply structure used to apply an electric field to the target, and a first gas inlet disposed on the first cavity shell and used to allow a first working gas to enter into the first cavity shell. And / or, the seed deposition cavity structure includes a second cavity shell, a second sample platform disposed within the second cavity shell and used to support the substrate, a second gas inlet disposed on the second cavity shell and allowing the seed layer precursor to enter into the second cavity shell, and a second gas inlet disposed on the second cavity shell and allowing the second working gas to enter into the second cavity shell; And / or, the annealing chamber structure includes a third chamber shell, a third sample platform disposed within the third chamber shell and used to support the substrate, a heating assembly disposed on at least one side of opposite sides of the third sample platform, and a third gas inlet disposed on the third chamber shell and allowing the third working gas to enter into the third chamber shell; And / or, the adhesive electrode deposition cavity structure includes a fourth cavity shell, a fourth sample platform disposed within the fourth cavity shell, and a fourth gas inlet disposed on the fourth cavity shell and allowing a fourth working gas to enter into the fourth cavity shell.

[0014] Secondly, this application also provides a method for preparing a piezoelectric thin film using a piezoelectric thin film preparation device, comprising: The substrate is placed in the adhesive electrode deposition cavity structure, adhesive material is sputtered onto the substrate to form an adhesive layer, and then bottom electrode material is sputtered onto the adhesive layer to form a bottom electrode layer. A substrate with an adhesion layer and a bottom electrode layer is placed in a buffer deposition cavity structure, and a buffer material is deposited on the bottom electrode layer to form a buffer layer. A substrate with an adhesion layer, a bottom electrode layer and a buffer layer deposited is placed in a seed deposition chamber structure. Seed material is deposited on the buffer layer to form a seed layer. At the same time, the seed layer is placed in an annealing chamber structure for rapid crystallization annealing, and the annealing temperature is less than 450℃. A substrate with an adhesion layer, a bottom electrode layer, a buffer layer and a seed layer deposited is placed in a piezoelectric deposition cavity structure, and piezoelectric material is deposited on the seed layer to form a piezoelectric film layer. A substrate with deposited adhesive layer, bottom electrode layer, buffer layer, seed layer and piezoelectric film layer is placed in an annealing chamber structure for stress annealing.

[0015] The beneficial effects of this invention are: This application provides a piezoelectric thin film fabrication apparatus and a fabrication method thereof. The piezoelectric thin film fabrication apparatus includes a deposition growth chamber module and an annealing chamber structure. The deposition growth chamber module includes at least an adhesive electrode deposition chamber structure for depositing an adhesion layer on a substrate and depositing a bottom electrode layer on the adhesion layer, a buffer deposition chamber structure for depositing a buffer layer on the bottom electrode layer, a seed deposition chamber structure for depositing a seed layer on the buffer layer, and a piezoelectric deposition chamber structure for depositing a piezoelectric film layer on the seed layer. The annealing chamber structure is configured to anneal at least the seed layer and / or the piezoelectric film layer to facilitate the final formation of a piezoelectric thin film with excellent performance.

[0016] In other words, compared to traditional piezoelectric thin film fabrication methods that require high temperatures and long crystallization times, which can negatively impact the substrate, the piezoelectric thin film fabrication equipment of this application features an additional seed deposition chamber structure. This allows the formation of low-energy nucleation points on the surface of the buffer layer, effectively creating a unit cell template for the crystallization of the piezoelectric film atoms. This facilitates the direct, directional, and rapid sputtering of piezoelectric film atoms onto the unit cell template, reducing the nucleation activation energy and thus effectively lowering the atomic crystallization temperature. Simultaneously, a high temperature is injected through the annealing chamber structure, enabling rapid crystallization of atoms on the unit cell template, while the substrate remains at a low temperature for a short period. Ultimately, this achieves the goal of fabricating a piezoelectric film on a low-melting-point substrate to form the desired piezoelectric thin film. Attached Figure Description

[0017] To more clearly illustrate the technical solutions of the embodiments of this application, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 2 This is a structural diagram of the piezoelectric thin film prepared by the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 3 This is a structural diagram of the vacuum transfer cavity of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 4 This is a schematic diagram of the seed deposition chamber structure of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 5 This is a schematic diagram of the annealing chamber structure of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 6 This is a schematic diagram of the piezoelectric deposition cavity structure or buffer deposition cavity structure of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 7 This is a schematic diagram of the adhesion electrode deposition cavity structure of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 8 This is a schematic diagram of the load locking chamber of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 9 This is a schematic diagram of the circuit structure of the piezoelectric thin film preparation equipment shown in the embodiments of this application; Figure 10 This is a flowchart illustrating the method for preparing piezoelectric thin films using piezoelectric thin film preparation equipment, as shown in the embodiments of this application. Figure 11-12 This is a flowchart illustrating the method for starting and ending vacuuming in the piezoelectric deposition chamber structure of the piezoelectric thin film preparation apparatus shown in the embodiments of this application. Figure 13-14 This is a flowchart illustrating the method for transferring a substrate using an automatic transfer mechanism in the piezoelectric thin film fabrication equipment shown in the embodiments of this application. Figure 15 This is a flowchart illustrating the method for depositing a film layer using the adhesive electrode deposition cavity structure of the piezoelectric thin film preparation apparatus shown in the embodiments of this application. Figure 16 A flowchart illustrating the method for creating a cavity in the piezoelectric thin film preparation apparatus shown in the embodiments of this application; Figures 17-18A flowchart illustrating the method for vacuuming and opening the load locking chamber of the piezoelectric thin film device shown in the embodiments of this application.

[0019] Figure label: 100. Deposition growth chamber module; 101. Substrate; 102. Adhesion layer; 103. Bottom electrode layer; 104. Buffer layer; 105. Seed layer; 106. Piezoelectric film layer; 107. Top electrode layer; 110. Adhesion electrode deposition chamber structure; 111. Dry pump; 112. Pre-pump valve; 113. Full-scale gauge inlet valve; 114. Fore-stage valve; 115. Gate valve; 116. Molecular pump; 117. Process gauge inlet valve; 118. Fourth chamber shell; 11 9. Fourth sample platform; 109. Fourth gas inlet; 120. Buffer deposition chamber structure; 130. Seed deposition chamber structure; 140. Piezoelectric deposition chamber structure; 141. Second chamber shell; 142. Second sample platform; 143. Second gas inlet; 144. Second gas inlet; 145. Second outlet; 150. Annealing chamber structure; 151. Third chamber shell; 152. Third sample platform; 153. Heating assembly; 154. Third gas inlet; 155. Third outlet; 300. In-situ detection module; 310. Stress detection element; 320. Resistance detection element; 330. Film thickness detection element; 340. Temperature detection element; 350. Plasma detection element; 360. Flow detection element; 400. Central control module; 500. Resistance detection chamber module; 510. Resistance detection device; 600. Vacuum transfer chamber; 610. Control valve; 620. Robotic arm; 700. Pretreatment Front-end module; 710, load locking chamber; 711, load locking outer shell; 712, load platform; 810, first chamber shell; 811, first sample platform; 812, target platform; 813, power supply structure; 814, first gas inlet; 815, first outlet; 816, motor; 817, heating element; 818, flow meter; 819, diaphragm valve; 900, target baffle; 910, source bottle; 920, magnetic switch; 930, pressure switch. Detailed Implementation

[0020] In the embodiments of this application, the terms "first," "second," "third," "fourth," "fifth," and "sixth" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined with "first," "second," "third," "fourth," "fifth," and "sixth" may explicitly or implicitly include one or more of that feature.

[0021] In embodiments of this application, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes that element.

[0022] Reference Figures 1 to 8 As shown in the figure, this application provides a piezoelectric thin film preparation device, including a deposition growth chamber module 100 and an annealing chamber structure 150.

[0023] The deposition growth chamber module 100 includes at least an adhesive electrode deposition chamber structure 110 for depositing an adhesion layer 102 on a substrate 101 and depositing a bottom electrode layer 103 on the adhesion layer 102, a buffer deposition chamber structure 120 for depositing a buffer layer 104 on the bottom electrode layer 103, a seed deposition chamber structure 130 for depositing a seed layer 105 on the buffer layer 104, and a piezoelectric deposition chamber structure 140 for depositing a piezoelectric film layer 106 on the seed layer 105. The annealing chamber structure 150 is configured to anneal at least the seed layer 105 and / or the piezoelectric film layer 106.

[0024] In a specific implementation, the adhesive electrode deposition cavity structure 110 can be configured with a metal target for sputtering and depositing the adhesive layer 102 and a metal target for depositing the bottom electrode layer 103, so that the adhesive layer 102 can be sputtered and deposited on the substrate 101 in sequence, and then the bottom electrode layer 103 can be sputtered and deposited on the adhesive layer 102.

[0025] For example, the metal target used to form the adhesion layer 102 can be titanium (Ti), and the metal target used to form the bottom electrode layer 103 can be platinum (Pt). It should be noted that the purpose of depositing the adhesion layer 102 first is to improve the interlayer bonding force between the substrate 101 and the bottom electrode layer 103, and to avoid bonding failure due to chemical inertness.

[0026] For the buffer deposition cavity structure 120, an oxide target is disposed therein for depositing a buffer layer 104 with a specific lattice constant to achieve lattice matching and diffusion barrier with the bottom electrode layer 103. For example, the oxide target can be lanthanum nickelate (LaNiO3), strontium ruthenium ruthenium oxide (SrRuO3), or aluminum oxide (Al2O3).

[0027] For the seed deposition cavity structure 130, an ultrathin (e.g., 1 nm-10 nm) seed layer material is deposited. This seed layer material grows layer by layer within the seed deposition cavity structure 130, forming a seed layer 105, i.e., a unit cell template, for the directional sputtering of atoms of subsequent piezoelectric materials. This reduces the nucleation activation energy of atoms, thereby effectively lowering the temperature for atomic crystallization. For example, the seed layer material can be titanium dioxide (TiO2), lead zirconate titanate (PZT), or scandium aluminum nitride (AlScN).

[0028] For the piezoelectric deposition cavity structure 140, it can be equipped with replaceable rotating composite targets, such as Pb(Zr,Ti)O3 targets, Pb(Mg1 / 3Nb2 / 3)O3-PbTiO3 targets, and AlSc alloy targets (where the Sc content is adjustable). By switching different rotating composite targets, substrates 101, and introducing different reactive gases (O2 or N2), PZT, PMNT (full name is Pb(Mg1 / 3Nb2 / 3)O3-PbTiO3 target, lead magnesium niobate-lead titanate), or AlScN can be deposited within the same piezoelectric deposition cavity structure 140.

[0029] For the annealing chamber structure 150, high-power halogen lamps or laser arrays are typically used for rapid (millisecond to second-level) heating, with a maximum temperature of up to 800°C. This annealing chamber structure 150 is mainly used to control the crystallization and stress of the piezoelectric film, i.e., to rapidly heat-treat the deposited piezoelectric film layer 106, inducing crystallization of the piezoelectric material or repairing defects. Furthermore, oxygen can be introduced into the annealing chamber structure 150 to rapidly oxidize the deposited adhesion layer 102 and bottom electrode layer 103, forming a dense TiO2 layer at the interface between the adhesion layer 102 and the bottom electrode layer 103, preventing the downward diffusion of metal elements from the bottom electrode layer 103.

[0030] By performing different operations in the different cavity modules described above using the substrate 101, a complete piezoelectric thin film can be obtained by annealing in the annealing cavity structure 150 and then forming a top electrode layer 107.

[0031] In summary, compared to traditional piezoelectric thin film fabrication methods that require high temperatures and long crystallization times, which can negatively impact the substrate, the piezoelectric thin film fabrication equipment in this embodiment additionally incorporates a seed deposition chamber structure 130. This allows the formation of low-energy nucleation points on the surface of the buffer layer 104, effectively creating a unit cell template for the crystallization of atoms in the piezoelectric film layer 106. This facilitates the direct, directional, and rapid sputtering of atoms from the piezoelectric film layer 106 onto the unit cell template, reducing the nucleation activation energy and thus effectively lowering the atomic crystallization temperature. Simultaneously, high temperatures are injected through the annealing chamber structure 150, enabling rapid crystallization of atoms on the unit cell template, while the substrate 101 remains at a low temperature for a short period. This ultimately enables the fabrication of the piezoelectric film layer 106 on the low-melting-point substrate 101, followed by the deposition of a top electrode layer 107 on top of the piezoelectric film layer 106 to form the desired piezoelectric thin film.

[0032] Reference Figures 1 to 9 As shown, in some embodiments, the piezoelectric thin film preparation equipment further includes an in-situ detection module 300 and a central control module 400 electrically connected to the deposition growth chamber module 100 and the in-situ detection module 300, respectively. The in-situ detection module 300 is used to detect deposition information in the deposition growth chamber module 100, and the central control module 400 receives the deposition information and controls the working state of the deposition growth chamber module 100 according to the deposition information. The deposition information includes at least one of stress value, resistance information, film thickness information and temperature information.

[0033] The residual stress and preferred orientation of piezoelectric films have a decisive influence on their performance. Current fabrication processes largely rely on post-processing characterization (such as XRD and laser bending) to obtain deposition information like residual stress, making real-time monitoring, feedback, and timely adjustments during fabrication impossible. This results in long process development cycles and large fluctuations in yield. Therefore, in this embodiment, an in-situ detection module 300 detects the deposition information within the deposition growth chamber module 100 and feeds it back to the central control module 400. The central control module 400 can control the operating state of the deposition growth chamber module 100 based on the deposition information, thereby achieving real-time monitoring, feedback, and adjustment during the fabrication process, ultimately effectively improving the yield of piezoelectric films.

[0034] Reference Figure 1 , Figure 9 As shown, in some embodiments, the in-situ detection module 300 includes a stress detection element 310 disposed in the seed deposition chamber structure 130 and configured to detect the stress value of the seed layer 105. The central control module 400 is used to control the seed deposition chamber structure 130 to stop depositing the seed layer 105 when the stress value is greater than a preset value, and to control the annealing chamber structure 150 to perform stress annealing on the seed layer 105.

[0035] In practice, a stress detection element 310 is installed in the seed deposition chamber structure 130 to detect and acquire the stress value of the seed layer 105 in real time. If the stress value is less than the preset value, it means that the stress is within a reasonable range, and the deposition process of the seed layer 105 does not need to be interfered with. If the detected stress value is greater than the preset value, it means that the stress is too high, and the deposition operation of the seed layer 105 needs to be stopped. The substrate 101 with part of the seed layer 105 deposited is transferred to the annealing chamber structure 150 for rapid annealing to eliminate the stress. After the stress is eliminated to a reasonable range, it is returned to the seed deposition chamber structure 130 to continue deposition. The above operation is repeated until the film thickness of the deposited seed layer 105 reaches the preset thickness value, at which point the deposition is stopped and the next process begins.

[0036] For example, the stress detection element 310 may be an in-situ optical stress sensor.

[0037] Reference Figure 1 , Figure 9 As shown, in some embodiments, the in-situ detection module 300 further includes a resistance detection element 320 disposed in the adhesive electrode deposition cavity structure 110 and configured to detect the resistance information of the adhesive layer 102 and / or the bottom electrode layer 103; the central control module 400 controls the start and stop of the adhesive electrode deposition cavity structure 110 according to the resistance information.

[0038] In this embodiment, in order to know in a timely manner whether the resistance value of the bottom electrode layer 103 or the adhesive layer 102 is within the preset resistance range, a resistance detection element 320 can be provided in the adhesive electrode deposition cavity structure 110 to detect the resistance value of the bottom electrode layer 103 or the adhesive layer 102 in real time. This means that the electrical performance of the bottom electrode layer 103 or the adhesive layer 102 can be known in advance, and subsequent operations on the unqualified bottom electrode layer 103 or the adhesive layer 102 can be stopped in advance when the deposition resistance is found to be unqualified, so as to save subsequent processes and reduce processing costs.

[0039] For example, the resistance sensing element 320 can be an in-situ resistivity monitor.

[0040] Reference Figure 1 , Figure 9 As shown, in some embodiments, the in-situ detection module 300 further includes a film thickness detection element 330 disposed in the piezoelectric deposition cavity structure 140. The film thickness detection element 330 is configured to detect the film thickness information of the piezoelectric film layer 106, and the central control module 400 controls the start and stop of the piezoelectric deposition cavity structure 140 according to the film thickness information.

[0041] In practice, to obtain real-time information on whether the thickness of the piezoelectric film layer 106 has reached the preset thickness, a film thickness detection element 330 can be installed within the piezoelectric deposition cavity structure 140 to detect the film thickness of the piezoelectric film layer 106 in real time. When the film thickness has not reached the preset thickness value, the piezoelectric deposition cavity structure 140 is controlled to continue the deposition operation of the piezoelectric film layer 106. When the film thickness is detected to have reached the preset thickness value, the piezoelectric deposition cavity structure 140 can be controlled to stop the deposition operation of the piezoelectric film layer 106, and the next process can proceed.

[0042] For example, the film thickness detection element 330 can be an ellipsometer.

[0043] Reference Figure 1 , Figure 9 As shown, in some embodiments, the in-situ detection module 300 further includes a temperature detection element 340 disposed within the annealing chamber structure 150. The temperature detection element 340 is configured to detect temperature information within the annealing chamber structure 150. The central control module 400 adjusts the annealing temperature within the annealing chamber structure 150 according to the temperature information to adjust the annealing temperature within the annealing chamber structure 150 to the most reasonable temperature range, which is beneficial to improving the performance and yield of the piezoelectric film layer 106 obtained after final annealing.

[0044] By combining the above-described control operations, the piezoelectric thin film preparation equipment of this embodiment can precisely control the residual stress of the final piezoelectric thin film from the traditional hundreds of MPa (usually tensile stress) to near zero or even a moderate compressive stress, greatly improving the adhesion and crack resistance of the piezoelectric thin film. Simultaneously, the aforementioned detection and control operations enable "global visualization" of the piezoelectric thin film growth process, transforming the traditional "deposition-characterization-trial and error" cycle into an intelligent process of "real-time monitoring-online feedback-instant optimization," significantly shortening the process development cycle of new materials and ensuring high batch-to-batch consistency.

[0045] Reference Figure 1 , Figure 9 As shown, in some embodiments, the piezoelectric thin film preparation equipment may also include a resistance detection chamber module 500 that can be communicated with the deposition growth chamber module 100. The resistance detection chamber module 500 is provided with a resistance detection device 510 that is electrically connected to the central control module 400. It is configured to perform resistance detection on at least the buffer layer 104, seed layer 105, or piezoelectric film layer 106 transferred to the resistance detection chamber module 500 to obtain the resistance result. The central control module 400 controls the start and stop of the deposition growth chamber module 100 according to the resistance result.

[0046] That is, an additional resistance detection cavity module 500 is set up to perform resistance detection on at least the deposited buffer layer 104, seed layer 105 and piezoelectric film layer 106, so as to know in time whether the electrical performance is qualified, and to realize real-time monitoring of each film layer after multiple processes.

[0047] For example, the resistance sensing device 510 can be a four-point probe sheet resistance meter.

[0048] It should be noted that each cavity module needs to be set to a vacuum state. In order to avoid atmospheric exposure and contamination, the resistance detection cavity module 500 is also set to a vacuum state. This achieves the switching of the vacuum environment of the substrate 101 with the corresponding film layer deposited in the vacuum state, so as to eliminate interface contamination and oxidation caused by atmospheric exposure, and significantly improve the interface quality and performance reliability of the final piezoelectric film.

[0049] In the actual preparation of aluminum nitride-based (AlN / AlScN) piezoelectric thin films, the doping concentration of Sc (scandium) needs to be increased to 30% or even higher to obtain a high piezoelectric response. However, at high Sc contents, rock salt phase (non-piezoelectric phase) is easily formed, which leads to a decrease in film quality.

[0050] Therefore, in this embodiment, the piezoelectric thin film preparation equipment includes a central control module 400. A plasma detection element 350, electrically connected to the central control module 400, is disposed within the piezoelectric deposition cavity structure 140 and configured to detect the ion concentration of the piezoelectric material within the piezoelectric deposition cavity structure 140. The central control module 400 adjusts the operating state of the piezoelectric deposition cavity structure 140 according to the ion concentration to achieve stable and uniform delivery of Sc ions, etc. Combined with rapid low-temperature annealing (≤450℃) of the annealing cavity structure 150, the formation of the rock salt phase is effectively suppressed, resulting in a single-phase AlScN thin film with a Sc concentration exceeding 40% and a strong texture, significantly improving the piezoelectric coefficient.

[0051] It should be noted that, for the deposition operation of the piezoelectric film layer 106, the ions formed after the metal target is ionized are deposited on the seed layer 105 to form the piezoelectric film layer 106. At this time, the concentration of ions can be detected by the plasma detection element 350 to ensure the stable and uniform delivery of Sc ions, etc.

[0052] For example, the plasma detection element 350 can be a mass spectrometer.

[0053] Reference Figure 1 , Figure 9As shown, in some embodiments, a flow detection element 360 electrically connected to the central control module 400 is also provided in the piezoelectric deposition cavity structure 140. It is configured to detect the flow rate of the reaction gas delivered to the piezoelectric deposition cavity structure 140. The central control module 400 controls the delivery flow rate of the reaction gas by comparing the flow rate with a preset flow rate range. By controlling the flow rate of the reaction gas, the growth rate of the piezoelectric film layer 106 can also be indirectly realized to adapt to the ion delivery rate of the piezoelectric material, so as to ultimately form a piezoelectric film layer 106 with excellent performance.

[0054] For example, the flow sensing element 360 can be a mass flow meter.

[0055] Reference Figure 1 , Figure 3 As shown, in some embodiments, the piezoelectric thin film preparation equipment includes a vacuum transfer chamber 600 and an automatic transfer mechanism disposed within the vacuum transfer chamber 600.

[0056] The vacuum transfer cavity 600 can be switched on and off with the adhesive electrode deposition cavity structure 110, the buffer deposition cavity structure 120, the seed deposition cavity structure 130, the piezoelectric deposition cavity structure 140, and the annealing cavity structure 150, respectively.

[0057] An automatic transfer mechanism is used to transfer any one of the substrate 101 self-adhesive electrode deposition cavity structure 110, buffer deposition cavity structure 120, seed deposition cavity structure 130, piezoelectric deposition cavity structure 140 and annealing cavity structure 150 to another via a vacuum transfer cavity 600.

[0058] In other words, in this embodiment of the piezoelectric thin film preparation equipment, since the deposition operations of each process need to be carried out in a vacuum environment to avoid atmospheric pollution, a vacuum transfer cavity 600 is set up. For example, when it is necessary to transfer the substrate 101 with the deposited bottom electrode layer 103 to the buffer deposition cavity structure 120 for the deposition of the buffer layer 104, the vacuum transfer cavity 600 can be connected to the adhesive electrode deposition cavity structure 110 first, and the substrate 101 with the deposited bottom electrode layer 103 in the adhesive electrode deposition cavity structure 110 can be automatically transferred to the vacuum transfer cavity 600 by an automatic transfer mechanism. Then, the connection between the vacuum transfer cavity 600 and the adhesive electrode deposition cavity structure 110 is disconnected, and the vacuum transfer cavity 600 is connected to the buffer deposition cavity structure 120. Then, the substrate 101 with the deposited bottom electrode layer 103 is automatically transported to the buffer deposition cavity structure 120 by an automatic transfer mechanism for the corresponding deposition operation.

[0059] The entire process can be automated, saving manpower and all operations are completed in a vacuum environment. Therefore, it can avoid problems such as interface oxidation, adsorption of impurities, and serious deterioration of film adhesion and electrical properties (such as increased leakage current and aggravated polarization fatigue).

[0060] For example, the transfer process of substrate 101 between other cavity modules can be referred to the above description, and will not be repeated here.

[0061] Reference Figure 1 , Figure 3 As shown, in some embodiments, the piezoelectric thin film preparation equipment includes a central control module 400, and the automatic transfer mechanism includes a robot arm 620, which is electrically connected to the central control module 400.

[0062] In a specific implementation, for example, when it is necessary to transfer the substrate 101 with the deposited bottom electrode layer 103 to the buffer deposition cavity structure 120 to deposit the buffer layer 104, the vacuum transfer cavity 600 can be connected to the adhesive electrode deposition cavity structure 110 first. The central control module 400 controls the robot 620 to pick up the substrate 101 with the deposited bottom electrode layer 103 in the adhesive electrode deposition cavity structure 110 and put it into the vacuum transfer cavity 600, and then pick it up and place it into the buffer deposition cavity structure 120 for the corresponding deposition operation.

[0063] For example, the robot 620 can be a commonly used multi-axis robot, which may include a base, multiple mechanical axes and joints connecting two adjacent mechanical axes. One of the two robot arms at the far ends is hinged to the base, and the free end of the other robot arm can be equipped with an electric gripper to realize the automatic gripping and placing of the substrate 101.

[0064] Reference Figure 1 , Figure 3 As shown, in some embodiments, the adhesive electrode deposition cavity structure 110, buffer deposition cavity structure 120, seed deposition cavity structure 130, piezoelectric deposition cavity structure 140 and annealing cavity structure 150 can be arranged around the vacuum transfer cavity 600 along the circumferential spacing of the vacuum transfer cavity 600. This facilitates the transfer operation between the vacuum transfer cavity 600 and the substrate 101 in each cavity module, and makes the structure of the entire piezoelectric film layer 106 preparation device more regular and compact.

[0065] Furthermore, when there are a large number of cavity structures, a vacuum transfer cavity 600 can be provided, including two interconnected cavities, such as... Figure 3 As shown, this allows for the arrangement of multiple cavity structures around the vacuum transfer cavity 600.

[0066] Reference Figure 1 , Figure 3As shown, in some embodiments, a control valve 610 is provided between the vacuum transfer chamber 600 and the adhesive electrode deposition chamber structure 110, the buffer deposition chamber structure 120, the seed deposition chamber structure 130, the piezoelectric deposition chamber structure 140, and the annealing chamber structure 150 to control their on / off states. The control valve 610 is electrically connected to the central control module 400 to automatically control the on / off states between the vacuum transfer chamber 600 and the adhesive electrode deposition chamber structure 110, the buffer deposition chamber structure 120, the seed deposition chamber structure 130, the piezoelectric deposition chamber structure 140, and the annealing chamber structure 150, thereby saving manpower and improving transfer efficiency.

[0067] For example, the control valve 610 may be a vacuum valve plate.

[0068] Reference Figure 1 As shown, in some embodiments, the piezoelectric thin film fabrication apparatus further includes a pretreatment front-end module 700 configured to pretreat the substrate 101; A load locking chamber 710 is provided between the pretreatment front-end module 700 and the vacuum transfer chamber 600. The load locking chamber 710 is connected to both the pretreatment front-end module 700 and the vacuum transfer chamber 600.

[0069] In practice, the preprocessing front-end module 700 is located at the atmospheric end and is used for preprocessing operations such as loading / unloading, pre-alignment, and initial cleaning of the substrate 101. The preprocessing front-end module is connected to the vacuum transfer chamber 600 through the load locking chamber 710, enabling safe and efficient transfer of the substrate 101 from the atmosphere to the high vacuum environment.

[0070] Specifically, the pre-processing front-end module 700 mainly includes a loading structure, a pre-aligner, a robot, and a cleaning unit. The loading structure loads the substrate 101, the robot picks up and places the substrate 101 between the load locking chamber 710 and the pre-aligner, the pre-aligner aligns the substrate 101, and the cleaning unit cleans the substrate 101.

[0071] Reference Figure 8 As shown, the load locking chamber 710 may specifically include a load locking housing 711 and a load platform 712 disposed within the load locking housing 711. It is mainly used for loading and unloading the substrate 101. The load locking chamber 710 can also be connected to the vacuum transfer chamber 600 via a control valve 610. Furthermore, an infrared sensor can be installed within the load locking chamber 710 to monitor the loading or unloading position of the substrate 101.

[0072] Reference Figure 6As shown, in some embodiments, both the buffer deposition cavity structure 120 and the piezoelectric deposition cavity structure 140 include a first cavity shell 810, a first sample platform 811 disposed within the first cavity shell 810 and used to support the substrate 101, a target platform 812 used to support the target, a power supply structure 813 used to apply an electric field to the target, and a first gas inlet 814 disposed on the first cavity shell 810 and used to allow the first working gas to enter into the first cavity shell 810.

[0073] For example, regarding the piezoelectric deposition cavity structure 140 for depositing the piezoelectric film layer 106, it mainly adopts magnetron sputtering technology to adapt to the co-deposition requirements of multi-component target materials for piezoelectric materials. The core working principle is: in a high vacuum environment (vacuum degree 10... - ³~10 -5 Under the influence of electric field (e.g., Ti), an electric field is applied to the target material (e.g., Ti) on the target platform 812 through a power supply structure 813 (e.g., radio frequency or DC power supply), causing the first working gas (e.g., Ar) in the first cavity shell 810 to be ionized into plasma. High-energy ions in the plasma bombard the target surface at high speed under the action of the electric field, causing target atoms, ions, or molecules to detach from the target surface through momentum transfer (sputtering effect), forming a gas-phase atomic beam. The gas-phase atomic beam moves directionally to the pretreated substrate 101 surface, and through nucleation, growth, and film formation processes, a dense piezoelectric film layer 106 with good lattice matching with the substrate is deposited. After deposition, the substrate 101 with the piezoelectric film layer 106 can be transferred to the vacuum transfer cavity 600 through the first outlet 815 on the first cavity shell 810.

[0074] The deposition principle and process of other films, such as buffer layer 104, are the same as those of the deposition principle and process of piezoelectric film layer 106 described above, and will not be repeated in this embodiment.

[0075] In this embodiment, for the multi-component (Pb / Zr / Ti, La / Ni / O) co-deposition requirements of multi-component piezoelectric materials (such as PZT, LNO), a multi-target independent power control structure can be configured in the first cavity shell 810. By precisely controlling the sputtering power of each target, the chamber temperature, and the working gas flow rate, the controllable co-deposition of multi-component atoms can be achieved, ensuring the uniformity of the thin film composition.

[0076] Reference Figure 4As shown, in some embodiments, the seed deposition chamber structure 130 includes a second chamber shell 141, a second sample platform 142 disposed within the second chamber shell 141 for supporting the substrate, a second gas inlet 143 disposed on the second chamber shell 141 for allowing the seed layer precursor to enter the second chamber shell 141, and a second gas inlet 144 disposed on the second chamber shell 141 for allowing the second working gas to enter the second chamber shell 141. After deposition, the substrate 101 with the seed layer 105 can be transferred to the vacuum transfer chamber 600 through the second outlet 145 on the second chamber shell 141.

[0077] The seed deposition chamber structure 130 is a preparation chamber for a multi-element piezoelectric material interface transition layer, a doped modification layer, and a dense passivation layer. Its core working principle is self-confined surface reaction, a precise deposition technique at the single-atom level. The specific process involves: in a medium-high vacuum environment (vacuum degree 10... - ²~10 -4 Pa) and a set temperature, setting two or more of the following: Figure 4 The seed layer precursors (including a first precursor and a second precursor) in the source bottle 910 are sequentially and pulsedly introduced into the second chamber shell 141 through the second gas inlet 144. Simultaneously, the second chamber shell 141 is purged by a second working gas (an inert gas, such as N2 or Ar), achieving two or more alternating surface reactions. Each reaction cycle deposits only a single atomic layer or a single molecular layer film. Specifically: First precursor pulse introduction: The first precursor in one of the two source bottles 910 undergoes chemical adsorption with the surface active sites of the buffer layer 104 to form a saturated adsorption layer, and the excess first precursor is purged out.

[0078] Second precursor pulse introduction: The second precursor in one of the two source bottles 910 undergoes a solid-phase chemical reaction with the first precursor adsorbed on the surface of the buffer layer 104 to form a single-atom layer of the target thin film, and the reaction byproducts are purged out; the above cycle is repeated to achieve layer-by-layer controllable growth of the seed layer 105.

[0079] The seed deposition cavity structure 130 is adapted to the ultra-thin, dense, and shape-preserving requirements of the interface layer in the preparation of piezoelectric materials. It can accurately prepare nanoscale seed layers 105 (such as TiO2, LNO and other buffer layers), improve the interfacial bonding force and lattice matching between the piezoelectric film layer 106 and the substrate 101 / bottom electrode layer 103, and the deposition process has no step coverage blind zone, making it suitable for the preparation of thin films on complex structure substrates.

[0080] Reference Figure 5As shown, in some embodiments, the annealing chamber structure 150 includes a third chamber shell 151, a third sample platform 152 disposed in the third chamber shell 151 and used to support the substrate 101, a heating assembly 153 disposed on at least one side of the opposite sides of the third sample platform 152, and a third gas inlet 154 disposed on the third chamber shell 151 and allowing a third working gas to enter into the third chamber shell 151. After annealing, the piezoelectric film can be discharged through the third outlet 155 disposed on the third chamber shell 151.

[0081] The annealing chamber structure 150 is a post-processing modification chamber for multi-element piezoelectric material thin films. It is a core functional unit for solving problems such as lattice distortion, incomplete crystal phase, and stress concentration in PVD / ALD deposited thin films. The core working principle is as follows: Under vacuum or a third working gas (such as N2, O2, Ar, to meet the oxygen vacancy compensation requirements of piezoelectric materials), a non-contact rapid heating component 153 (such as a halogen lamp or an infrared quartz lamp) rapidly heats the substrate 101 on which the piezoelectric film layer 106 is deposited, causing the piezoelectric film to reach the set annealing temperature (300~800℃, to meet the crystal phase transformation temperature of PZT / LNO piezoelectric materials) in a short time (heating rate 10~200℃ / s, holding time several seconds to several minutes, cooling rate 50~300℃ / s). During the holding stage, lattice rearrangement, preferred crystal phase growth, stress release, and oxygen vacancy repair are completed. Then, rapid cooling is used to suppress excessive grain growth.

[0082] Compared to traditional furnace annealing, the rapid thermal cycling characteristics of the annealing chamber structure 150 effectively prevent interdiffusion between the substrate 101 and the piezoelectric film layer 106, ensuring interface clarity. Simultaneously, it precisely controls the crystal phase (such as the perovskite phase of PZT) and grain size of the piezoelectric film, improving its piezoelectric properties (such as piezoelectric strain constant and dielectric constant). Furthermore, the third chamber shell 151 is equipped with a temperature sensing element 340, enabling regional uniformity control of the annealing temperature and preventing cracking and warping of the film due to thermal stress.

[0083] In summary, the piezoelectric thin film preparation equipment of this embodiment uses a vacuum transfer chamber 600 as a transfer chamber connected to each cavity shell, integrating the adhesive electrode deposition cavity structure 110, buffer deposition cavity structure 120, seed deposition cavity structure 130, piezoelectric deposition cavity structure 140, and annealing cavity structure 150 into a single unit. Each cavity module independently performs its corresponding preparation process. At the same time, through the coordinated transport of the vacuum transfer chamber, the entire process of preparing multi-element piezoelectric materials (such as PZT and LNO-based piezoelectric / epitaxy layer materials) from the pretreatment of the substrate 101 to the finished piezoelectric thin film is carried out in a continuous vacuum. This effectively avoids the oxidation and contamination of the piezoelectric thin film surface by the atmospheric environment, and improves the uniformity of material composition, interfacial bonding force, and piezoelectric properties.

[0084] Reference Figure 7 As shown, the adhesive electrode deposition cavity structure 110 includes a fourth cavity shell 118, a fourth sample platform 119 disposed within the fourth cavity shell 118, and a fourth gas inlet 109 disposed on the fourth cavity shell 118 and allowing a fourth working gas to enter into the fourth cavity shell 118, thereby forming an adhesive layer 102 and a bottom electrode layer 103. (Refer to...) Figure 1 As shown, the adhesive electrode deposition cavity structure 110 can be a single cavity structure, or multiple different cavity structures can be selected for different target materials to achieve the required target material deposition operation.

[0085] The overall working principle of the piezoelectric thin film preparation equipment in this embodiment is as follows: After the piezoelectric thin film preparation equipment is started, the vacuum transfer chamber 600, the adhesive electrode deposition chamber structure 110, the buffer deposition chamber structure 120, the seed deposition chamber structure 130, the piezoelectric deposition chamber structure 140, and the annealing chamber structure 150 are first evacuated to ensure that each chamber reaches the vacuum level required for the corresponding process. The vacuum transfer chamber is maintained at 10... -3 ~10 -4 The high vacuum transition environment of Pa is maintained by the adhesion electrode deposition cavity structure 110, the buffer deposition cavity structure 120, and the piezoelectric deposition cavity structure 140 for 10 days. -3 ~10 -5 The high-vacuum deposition environment of Pa, the seed deposition cavity structure is maintained at 130. -2 ~10 -4 The medium-high vacuum deposition environment is maintained at Pa. The annealing chamber structure 150 maintains a vacuum or a set protective atmosphere (N2, O2, Ar). The vacuum status of each chamber is monitored and controlled in real time by an independent vacuum control system to ensure process stability.

[0086] Specifically, in combination Figure 6 The structure of the piezoelectric deposition chamber 140 shown is described, and the vacuuming operation procedure is as follows: Figure 11-12 As shown, for example, the operation of starting and ending vacuuming in piezoelectric deposition cavity structure 140 is illustrated below: (Refer to...) Figure 11 The vacuuming process shown is as follows: First, close the control valve 610 between the piezoelectric deposition chamber structure 140 and the vacuum transfer chamber 600; turn on the dry pump (PUMP) 111; open the pre-evacuation valve 112; and open the full-scale gauge inlet valve 113, making the vacuum level in the piezoelectric deposition chamber structure 140 less than or equal to 10 Pa. Then, close the pre-evacuation valve 112; open the inlet valve 114 and delay for 3 seconds; open the gate valve 115; and turn on the molecular pump 116, ultimately maintaining the vacuum level in the piezoelectric deposition chamber structure 140 at 10 Pa. -3 ~10 -5 Pa. (Refer to) Figure 12As shown, when the vacuuming operation is to be ended, the slide gate valve 115 can be closed, then the molecular pump (i.e., TMP) 116 can be turned off. After the molecular pump 116 stops rotating, the fore-stage valve 114 can be closed, then the dry pump 111 can be turned off, and the full-scale gauge fore-stage valve 113 can be closed to end the vacuuming operation.

[0087] In addition, combined Figure 7 The structure of the adhesive electrode deposition cavity 110 shown is described, and the deposition operation is performed according to the following reference. Figure 15 The following is a brief description, using the adhesive electrode deposition cavity structure 110 to achieve the adhesive layer 102 as an example: First, the motor 816 driving the rotation of the fourth sample platform 119 is turned on. Then, the heating element 817 (such as a resistance wire or thermocouple) heating the fourth sample platform 119 is turned on. After the temperature reaches the preset value, the flow meter 818 is turned on, the diaphragm valve 819 is turned on, the full-scale gauge inlet valve 113 is turned off, the process gauge inlet valve 117 is turned on, the target baffle 900 carrying the target material is turned on, and the power supply structure 813 is started to turn on the radio frequency or DC source, applying an electric field to the target material (such as Ti) on the target material platform, so that the fourth working gas (such as Ar) in the fourth cavity shell 118 is ionized into plasma. The high-energy ions in the plasma bombard the target surface at high speed under the action of the electric field, and the target atoms, ions or molecules are detached from the target surface through momentum transfer (sputtering effect), forming a gas phase atomic beam. A gas-phase atomic beam is directed to the surface of a pretreated substrate 101, and through nucleation, growth, and film formation processes, a dense adhesion layer 102 with good lattice matching with the substrate is deposited.

[0088] In addition, the transfer process of substrate 101 is as follows Figure 13-14 The following is a brief description, using the transfer of substrate 101 from the adhesive electrode deposition cavity structure 110 to the vacuum transfer cavity 600, and the transport of substrate 101 transferred to the vacuum transfer cavity 600 to the buffer deposition cavity structure 120 as examples: First, refer to Figure 13 As shown, ensure that the pressure difference between the vacuum transfer chamber 600 and the adhesive electrode deposition chamber structure 110 is less than or equal to 10 Pa. Then, open the control valve 610 between the vacuum transfer chamber 600 and the adhesive electrode deposition chamber structure 110. When the control valve 610 is opened, determine that the z-axis position of the robot arm has dropped to the bottom and that the substrate 101 is now inside the adhesive electrode deposition chamber structure 110. Next, the robot arm extends and rises to the top of the z-axis, grabs the substrate 101, and returns to its original position. After the robot arm returns to the vacuum transfer chamber 600, close the control valve 610 between the vacuum transfer chamber 600 and the adhesive electrode deposition chamber structure 110.

[0089] Next, refer to Figure 14As shown, ensure that the pressure difference between the vacuum transfer chamber 600 and the buffer deposition chamber structure 120 is less than or equal to 10 Pa. Then, open the control valve 610 between the vacuum transfer chamber 600 and the buffer deposition chamber structure 120. After the control valve 610 is opened, determine that the z-axis position of the robot arm has risen to the top and that the substrate 101 is on the robot arm. Next, the robot arm extends and descends to the bottom of the z-axis and places the substrate 101 in the buffer deposition chamber structure 120. Then, the robot arm returns to its original position. After the robot arm returns to its original position, close the control valve 610 between the vacuum transfer chamber 600 and the buffer deposition chamber structure 120.

[0090] It should be noted that the above-mentioned position determination process can use infrared monitoring technology such as image acquisition elements to obtain position information and send it to the central control module 400. The central control module 400 then determines whether the position is in the preset position in order to proceed with the next step.

[0091] In addition, refer to Figure 16 The flowchart of the cavity opening method is shown below. For example, taking the removal of the piezoelectric film layer 106 after the annealing of the annealing chamber structure 150 as an example, the process is as follows: First, determine whether the vacuum in the annealing chamber structure 150 has ended. Then, determine whether the vacuum in the vacuum transfer chamber 600 has ended. Next, determine whether the pressure difference between the annealing chamber structure 150 and the vacuum transfer chamber 600 is less than or equal to 10 Pa. Then, open the control valve 610 between the two. Determine whether the pressure difference between the vacuum transfer chamber 600 and the load locking chamber 710 is less than 10 Pa. If so, open the control valve 610 between the vacuum transfer chamber 600 and the load locking chamber 710, close the angle valve of the load locking chamber, close the dry pump of the load locking chamber, open the diaphragm valve of the load locking chamber, determine whether the pressure switch detects atmospheric pressure, close the diaphragm valve of the load locking chamber, and close the control valve 610 between the load locking chamber 710 and the vacuum transfer chamber 600. This completes the cavity opening operation.

[0092] In addition, refer to Figure 17-18 The vacuum process and opening process of the load locking chamber 710 are shown. (Refer to...) Figure 17 As shown, the vacuum process is as follows: Close the top cover of the load locking chamber 710, determine that the magnetic switch 920 has engaged, turn on the dry pump in the load locking chamber, open the angle valve in the load locking chamber, and end the vacuum process when the vacuum level is less than 10 Pa. (Refer to...) Figure 18 As shown, the opening process is as follows: close the angle valve, open the load locking chamber diaphragm valve, the pressure switch 930 closes the load locking chamber diaphragm valve after detecting atmospheric pressure, the magnetic switch 920 leaves and cannot open the angle valve, and finally the process ends.

[0093] Finally, the preparation process of the piezoelectric thin film in this embodiment is briefly described as follows: The substrate 101, after pretreatment (such as cleaning, drying, and surface activation), is first sent into the vacuum transfer cavity 600. The magnetic levitation / robotic arm type automatic transfer mechanism in the vacuum transfer cavity 600, under non-contact and precise positioning control, transfers the substrate 101 to the adhesion electrode deposition cavity structure 110 and the buffer deposition cavity structure 120 for sequential magnetron sputtering deposition. In a high vacuum environment, plasma is formed by ionizing the inert working gas through an RF / DC power supply. The plasma bombards the multi-component target material at high speed, causing the target material atoms / ions / molecules to sputter and form a gas phase beam, which is directionally deposited onto the substrate surface to prepare the adhesion layer 102, the bottom electrode layer 103, and the buffer layer 104 required for the multi-component piezoelectric material. During the deposition process, the content of each component is precisely controlled through a multi-target independent power control structure to ensure the uniformity of the thin film composition.

[0094] After the deposition process of buffer layer 104 is completed, the automatic transfer mechanism transfers the substrate 101 from the buffer deposition cavity structure 120 to the seed deposition cavity structure 130. Based on the principle of self-limiting surface reaction, the seed deposition cavity structure 130 sequentially and in a pulsed manner introduces two or more seed layer precursors at a set substrate temperature. At the same time, it is purged with inert gas, so that the seed layer precursors undergo chemical adsorption and solid-phase reaction on the surface of buffer layer 104 in sequence. In each reaction cycle, a single atomic layer / monomer layer film is deposited. This process is repeated to prepare an ultrathin, dense seed layer 105 with good shape preservation, which improves the interfacial bonding force and lattice matching between piezoelectric film layer 106 and substrate 101 / bottom electrode layer 103, and eliminates the step coverage blind zone.

[0095] Next, after the seed layer 105 deposition process is completed, the automatic transfer mechanism transfers the substrate 101 from the seed deposition chamber structure 130 to the annealing chamber structure 150. The annealing chamber structure 150 initiates a rapid thermal annealing process. Under vacuum or protective atmosphere, the substrate 101 and the piezoelectric film layer 106 are rapidly heated / cooled (heating rate 10~200℃ / s, cooling rate 50~300℃ / s) through a non-contact rapid heating component 153 (halogen lamp, infrared quartz lamp). This allows the piezoelectric film to complete lattice rearrangement, preferential crystal phase growth, stress release, and oxygen vacancy repair under set temperature (300~800℃) and short-time holding conditions. This solves problems such as lattice distortion, incomplete crystal phase, and stress concentration in PVD / ALD deposited films, further improving the piezoelectric properties, dielectric properties, and structural stability of the multi-element piezoelectric material.

[0096] After the annealing process in the annealing chamber structure 150 is completed, the automatic transfer mechanism transfers the finished piezoelectric film layer 106 from the annealing chamber structure 150 back to the vacuum transfer chamber 600, and finally sends it out of the equipment through the discharge gate valve, completing the integrated preparation process of the entire piezoelectric film. Throughout the preparation process, the vacuum transfer chamber 600 maintains a high vacuum transition state. Each process chamber is sealed and isolated from the vacuum transfer chamber 600 through control valves such as ultra-high vacuum gate valves 610. This allows for independent process debugging and maintenance of a single chamber while the other chambers operate normally without interference, effectively improving the operating efficiency, flexibility, and stability of the equipment, and adapting to the needs of large-scale, high-precision preparation of multi-element piezoelectric materials.

[0097] Reference Figure 10 As shown, this embodiment provides a method for preparing a piezoelectric thin film, which is carried out using the aforementioned piezoelectric thin film preparation equipment. The specific preparation method includes the following steps: S101: Place the substrate 101 in the adhesive electrode deposition cavity structure 110, sputter adhesive material onto the substrate 101 to form an adhesive layer 102, and then sputter bottom electrode material onto the adhesive layer 102 to form a bottom electrode layer 103. S102: Place the substrate 101 with the adhesion layer 102 and the bottom electrode layer 103 deposited in the buffer deposition cavity structure 120, and deposit buffer material on the bottom electrode layer 103 to form a buffer layer 104. S103: The substrate 101, on which the adhesion layer 102, the bottom electrode layer 103 and the buffer layer 104 are deposited, is placed in the seed deposition chamber structure 130. Seed material is deposited on the buffer layer 104 to form a seed layer 105. At the same time, the seed layer 105 is placed in the annealing chamber structure 150 for rapid crystallization annealing, and the annealing temperature is less than 450°C. S104: Place the substrate 101, on which the adhesion layer 102, bottom electrode layer 103, buffer layer 104 and seed layer 105 are deposited, into the piezoelectric deposition cavity structure 140, and deposit piezoelectric material onto the seed layer 105 to form a piezoelectric film layer 106. S105: The substrate 101, on which the adhesion layer 102, the bottom electrode layer 103, the buffer layer 104, the seed layer 105 and the piezoelectric film layer 106 are deposited, is placed in the annealing chamber structure 150 for stress annealing to finally prepare a piezoelectric film.

[0098] Specifically, in step S101, the substrate 101, pretreated by the pretreatment front-end module 700, is first placed in the vacuum transfer chamber 600. Then, the central control module 400 opens the control valve 610 between the adhesion electrode deposition chamber structure 110 and the vacuum transfer chamber 600. The central air module then controls a robotic arm to transport the substrate 101 into the adhesion electrode deposition chamber structure 110 and closes the control valve 610. The substrate 101 then undergoes deposition of the adhesion layer 102 and the bottom electrode layer 103 in the vacuum environment of the adhesion electrode deposition chamber structure 110, thus forming a substrate 101 with the adhesion layer 102 and the bottom electrode layer 103. The specific deposition process is as follows: the adhesion layer 102 is formed by sputtering and depositing the adhesion material onto the substrate 101 using a target containing the adhesion material arranged within the adhesion electrode deposition chamber structure 110. Then, the bottom electrode layer 103 is formed by sputtering and depositing the bottom electrode layer 103 material onto the adhesion layer 102 using a target containing the bottom electrode layer 103 material. After deposition is completed, resistance can be measured to determine the pass rate. Once the pass rate is achieved, the process can proceed to the next step.

[0099] In step S102, the central control module 400 first opens the control valve 610 between the adhesive electrode deposition chamber structure 110 and the vacuum transfer chamber 600. Then, the robot arm 620 is controlled to transport the substrate 101 with the deposited adhesive layer 102 and bottom electrode layer 103 into the vacuum transfer chamber 600. Then, the control valve 610 between the adhesive electrode deposition chamber structure 110 and the vacuum transfer chamber 600 is closed, and the control valve 610 between the buffer deposition chamber structure 120 and the vacuum transfer chamber 600 is opened. The robot arm 620 is controlled to transport the substrate 101 with the deposited adhesive layer 102 and bottom electrode layer 103 into the buffer layer 104 deposition chamber structure. After that, the control valve 610 between the vacuum transfer chamber 600 and the buffer chamber module is closed, so that the substrate 101 can deposit the buffer layer 104 in the buffer deposition chamber structure 120 to form a substrate 101 with the buffer layer 104. The specific deposition process is as follows: an oxide target material is sputtered onto the bottom electrode layer 103 through the buffer deposition chamber structure 120 to form a buffer layer 104. After deposition, resistance measurement can be performed to determine the pass rate. If the pass rate is met, the process can proceed to the next step.

[0100] In step S103, the central control module 400 first opens the control valve 610 between the buffer deposition chamber structure 120 and the vacuum transfer chamber 600. Then, the robot arm 620 is controlled to transport the substrate 101 with the deposited adhesion layer 102, bottom electrode layer 103, and buffer layer 104 into the vacuum transfer chamber 600. Next, the control valve 610 between the buffer deposition chamber structure 120 and the vacuum transfer chamber 600 is closed, and the control valve 610 between the seed deposition chamber structure 130 and the vacuum transfer chamber 600 is opened. The robot arm 620 is then controlled to transport the substrate 101 with the deposited adhesion layer 102, bottom electrode layer 103, and buffer layer 104 into the seed deposition chamber structure 130 for seed layer 105 deposition, thus forming a substrate 101 with seed layer 105. Specifically, the deposition process involves sputtering a seed material target disposed within the seed deposition chamber structure 130 onto the buffer layer 104 to form the seed layer 105. After deposition is completed, resistance can be measured to determine the pass rate. Once the pass rate is achieved, the process can proceed to the next step.

[0101] In step S103, the stress value of the seed layer 105 can be detected and obtained in real time by the stress detection element 310, so as to realize real-time detection, feedback and adjustment in the preparation process, and ultimately effectively improve the yield of piezoelectric film.

[0102] In step S104, the central control module 400 first opens the control valve 610 between the seed deposition chamber structure 130 and the vacuum transfer chamber 600. Then, the robot arm 620 is controlled to transport the substrate 101 with the deposited adhesive layer 102, bottom electrode layer 103, buffer layer 104 and seed layer 105 into the vacuum transfer chamber 600. Then, the control valve 610 between the seed deposition chamber structure 130 and the vacuum transfer chamber 600 is closed and the control valve 610 between the piezoelectric deposition chamber structure 140 and the vacuum transfer chamber 600 is opened. The robot arm 620 is controlled to transport the substrate 101 with the deposited adhesive layer 102, bottom electrode layer 103, buffer layer 104 and seed layer 105 into the piezoelectric deposition chamber structure 140 for the deposition of the piezoelectric film layer 106, so as to form a substrate 101 with the piezoelectric film layer 106. The specific deposition process is as follows: a piezoelectric material target is sputtered onto the seed layer 105 through the piezoelectric deposition cavity structure 140 to form a piezoelectric film layer 106. After deposition, resistance measurement can be performed to determine the pass rate. If the pass rate is met, the process can proceed to the next step.

[0103] In step S104, to obtain real-time information on whether the thickness of the piezoelectric film layer 106 has reached the preset thickness, the thickness of the piezoelectric film layer 106 can be detected in real time by the film thickness detection element 330. When the film thickness has not reached the preset thickness value, the piezoelectric deposition chamber structure 140 is controlled to continue the deposition operation of the piezoelectric film layer 106. When the film thickness is detected to reach the preset final value, the piezoelectric deposition chamber structure 140 can be controlled to stop the deposition operation of the piezoelectric film layer 106, and the next process can be carried out. At the same time, when preparing the aluminum nitride-based (AlN / AlScN) piezoelectric thin film, the ion concentration of the piezoelectric material in the piezoelectric deposition chamber structure 140 is detected by the plasma detection element 350 to achieve stable and uniform transport of Sc ions, which is beneficial to effectively suppress the formation of rock salt phase and significantly improve the piezoelectric coefficient.

[0104] In step S105, the central control module 400 first opens the control valve 610 between the piezoelectric deposition chamber structure 140 and the vacuum transfer chamber 600. Then, the robot arm 620 is controlled to transport the substrate 101, which has deposited the adhesion layer 102, the bottom electrode layer 103, the buffer layer 104, the seed layer 105, and the piezoelectric film layer 106, into the vacuum transfer chamber 600. Then, the control valve 610 between the piezoelectric deposition chamber structure 140 and the vacuum transfer chamber 600 is closed, and the control valve 610 between the annealing chamber structure 150 and the vacuum transfer chamber 600 is opened. The robot arm 620 is then controlled to transport the substrate 101, which has deposited the adhesion layer 102, the bottom electrode layer 103, the buffer layer 104, the seed layer 105, and the piezoelectric film layer 106, into the annealing chamber structure 150 for annealing to form the final required piezoelectric film.

[0105] In this embodiment, the temperature of the annealing chamber structure 150 can be set to below 450 degrees Celsius, which can not only meet the requirements of crystallization at a lower temperature but also meet the temperature requirements of stress annealing.

[0106] In step S105, the temperature information inside the annealing chamber structure 150 is detected by the temperature detection element 340 in order to adjust the annealing temperature inside the annealing chamber structure 150, thereby improving the performance and yield of the piezoelectric film obtained after final annealing.

[0107] In the description of the embodiments of this application, specific features, structures, materials or characteristics may be combined in any suitable manner in one or more embodiments or examples.

[0108] The above are merely specific 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 piezoelectric thin film preparation apparatus, characterized in that, include: The deposition growth cavity module includes at least an adhesive electrode deposition cavity structure for depositing an adhesion layer on a substrate and depositing a bottom electrode layer on the adhesion layer, a buffer deposition cavity structure for depositing a buffer layer on the bottom electrode layer, a seed deposition cavity structure for depositing a seed layer on the buffer layer, and a piezoelectric deposition cavity structure for depositing a piezoelectric film layer on the seed layer. The annealing chamber structure is configured to anneal at least the seed layer and / or the piezoelectric film layer.

2. The piezoelectric thin film preparation equipment according to claim 1, characterized in that, The piezoelectric thin film preparation equipment also includes an in-situ detection module and a central control module that is electrically connected to the deposition growth chamber module and the in-situ detection module, respectively. The in-situ detection module is used to detect deposition information within the deposition growth chamber module, and the central control module is used to control the working state of the deposition growth chamber module based on the deposition information; wherein, the deposition information includes at least one of stress value, resistance information, film thickness information, and temperature information.

3. The piezoelectric thin film preparation equipment according to claim 2, characterized in that, The in-situ detection module includes a stress detection element disposed within the seed deposition chamber structure and is configured to detect the stress value of the seed layer. The central control module is used to control the seed deposition chamber structure to stop deposition when the stress value is greater than a preset value, and to control the annealing chamber structure to perform stress annealing on the seed layer. And / or, the in-situ detection module further includes a resistance detection element disposed within the adhesive electrode deposition cavity structure and configured to detect the resistance information of the adhesive layer and / or the bottom electrode layer, and the central control module is used to control the start and stop of the adhesive electrode deposition cavity structure according to the resistance information; And / or, the in-situ detection module further includes a film thickness detection element disposed within the piezoelectric deposition cavity structure, the film thickness detection element being configured to detect the film thickness information of the piezoelectric film layer, and the central control module being used to control the start and stop of the piezoelectric deposition cavity structure according to the film thickness information; And / or, the in-situ detection module further includes a temperature detection element disposed within the annealing chamber structure, the temperature detection element being configured to detect temperature information within the annealing chamber structure, and the central control module being used to adjust the annealing temperature within the annealing chamber structure according to the temperature information; And / or, the piezoelectric thin film preparation equipment further includes a resistance detection chamber module that can communicate with the deposition growth chamber module. The resistance detection chamber module is provided with a resistance detection device that is electrically connected to the central control module and is configured to perform resistance detection on the buffer layer, the seed layer, or the piezoelectric film layer transferred to the resistance detection chamber module to obtain a resistance result. The central control module is used to control the start and stop of the deposition growth chamber module according to the resistance result.

4. The piezoelectric thin film preparation apparatus according to any one of claims 1 to 3, characterized in that, The piezoelectric thin film preparation equipment includes a central control module. A plasma detection element electrically connected to the central control module is provided in the piezoelectric deposition cavity structure and is configured to detect the ion concentration of the piezoelectric material in the piezoelectric deposition cavity structure. The central control module is used to adjust the working state of the piezoelectric deposition cavity structure according to the ion concentration.

5. The piezoelectric thin film preparation equipment according to claim 4, characterized in that, The piezoelectric deposition chamber structure is also provided with a flow detection element electrically connected to the central control module, and is configured to detect the flow rate of the reaction gas delivered to the piezoelectric deposition chamber structure. The central control module controls the delivery flow rate of the reaction gas by comparing the flow rate with a preset flow rate range.

6. The piezoelectric thin film preparation apparatus according to any one of claims 1 to 3, characterized in that, The piezoelectric thin film preparation equipment includes a vacuum transfer chamber and an automatic transfer mechanism disposed within the vacuum transfer chamber; The vacuum transfer cavity is connected to the adhesive electrode deposition cavity structure, the buffer deposition cavity structure, the seed deposition cavity structure, the piezoelectric deposition cavity structure, and the annealing cavity structure in a switchable manner. The automatic transfer mechanism is used to transfer the substrate from any one of the adhesive electrode deposition cavity structure, the buffer deposition cavity structure, the seed deposition cavity structure, the piezoelectric deposition cavity structure, and the annealing cavity structure to another via the vacuum transfer cavity.

7. The piezoelectric thin film preparation equipment according to claim 6, characterized in that, The piezoelectric thin film preparation equipment includes a central control module; The automated transfer mechanism includes a robotic arm, which is electrically connected to the central control module; and / or, a control valve is provided between the vacuum transfer chamber and each of the adhesive electrode deposition chamber structure, the buffer deposition chamber structure, the seed deposition chamber structure, the piezoelectric deposition chamber structure, and the annealing chamber structure to control their on / off states, and the control valve is electrically connected to the central control module. And / or, the adhesive electrode deposition cavity structure, the buffer deposition cavity structure, the seed deposition cavity structure, the piezoelectric deposition cavity structure and the annealing cavity structure are arranged circumferentially around the vacuum transfer cavity.

8. The piezoelectric thin film preparation equipment according to claim 6, characterized in that, The piezoelectric thin film preparation equipment further includes a pretreatment front-end module, configured to pretreat the substrate; A load locking chamber is provided between the pretreatment front-end module and the vacuum transfer chamber, and the load locking chamber is connected to both the pretreatment front-end module and the vacuum transfer chamber.

9. The piezoelectric thin film preparation apparatus according to any one of claims 1 to 3, characterized in that, Both the buffer deposition cavity structure and the piezoelectric deposition cavity structure include a first cavity shell, a first sample platform disposed within the first cavity shell and used to support the substrate, a target platform used to support the target material, a power supply structure used to apply an electric field to the target material, and a first gas inlet disposed on the first cavity shell and used to allow the first working gas to enter into the first cavity shell. And / or, the seed deposition cavity structure includes a second cavity shell, a second sample platform disposed within the second cavity shell and used to support the substrate, a second gas inlet disposed on the second cavity shell and allowing the seed layer precursor to enter into the second cavity shell, and a second gas inlet disposed on the second cavity shell and allowing the second working gas to enter into the second cavity shell; And / or, the annealing chamber structure includes a third chamber shell, a third sample platform disposed within the third chamber shell and used to support the substrate, a heating assembly disposed on at least one side of the opposite sides of the third sample platform, and a third gas inlet disposed on the third chamber shell and allowing a third working gas to enter into the third chamber shell. And / or, the adhesive electrode deposition cavity structure includes a fourth cavity shell, a fourth sample platform disposed within the fourth cavity shell, and a fourth gas inlet disposed on the fourth cavity shell and allowing a fourth working gas to enter into the fourth cavity shell.

10. A method for preparing a piezoelectric thin film using the piezoelectric thin film preparation equipment according to any one of claims 1 to 9, characterized in that, include: The substrate is placed in the adhesive electrode deposition cavity structure, adhesive material is sputtered onto the substrate to form an adhesive layer, and then bottom electrode material is sputtered onto the adhesive layer to form a bottom electrode layer. A substrate with an adhesion layer and a bottom electrode layer is placed in a buffer deposition cavity structure, and a buffer material is deposited on the bottom electrode layer to form a buffer layer. A substrate with an adhesion layer, a bottom electrode layer and a buffer layer deposited is placed in a seed deposition chamber structure. Seed material is deposited on the buffer layer to form a seed layer. At the same time, the seed layer is placed in an annealing chamber structure for rapid crystallization annealing, and the annealing temperature is less than 450℃. A substrate with an adhesion layer, a bottom electrode layer, a buffer layer and a seed layer deposited is placed in a piezoelectric deposition cavity structure, and piezoelectric material is deposited on the seed layer to form a piezoelectric film layer. A substrate with deposited adhesive layer, bottom electrode layer, buffer layer, seed layer and piezoelectric film layer is placed in an annealing chamber structure for stress annealing.

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