Method for preparing near-stoichiometric yttrium oxide coating at high deposition rate as well as product and application of near-stoichiometric yttrium oxide coating

Abstract

The invention discloses a method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate as well as a product and application of the near-stoichiometric yttrium oxide coating, and relates to the technical field of semiconductors. The yttrium oxide coating is prepared by adopting a physical vapor deposition intermediate-frequency reaction magnetron sputtering technology, and the oxygen flow and the target voltage are dynamically regulated and controlled through a closed-loop feedback control system, so that the target material works in a transition area between a metal mode and an oxidation mode. The target material is located between a metal mode and an oxidation mode, the deposition efficiency of the coating is remarkably improved, and the coating has the near-stoichiometric ratio characteristic and better mechanical and corrosion-resistant performance.

Description

Technical Field

[0001] This invention relates to the field of semiconductor technology, and in particular to a method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates, as well as the products and applications thereof. Background Technology

[0002] As integrated circuit process nodes continue to advance towards the nanometer scale, plasma etching has become a key technology in semiconductor manufacturing. However, during the etching process, high-energy plasma not only erodes the reaction chamber components and shortens their lifespan, but also generates etching residues. If these residues are not effectively removed, they adhere to the chamber walls and contribute to particle formation. When the wafer is moved or gas is injected, sudden pressure changes can trigger shock waves or gas viscosity forces, causing particles to suspend and potentially migrate to the wafer surface. Transient electric fields can also generate electromagnetic stress, keeping residues suspended in the gas phase for extended periods. If plasma has not yet formed or the ion sheath layer is thin, these residues will adhere to the wafer surface, affecting etching accuracy. Depositing a plasma-resistant thin film on the chamber walls is an effective strategy to mitigate particle contamination.

[0003] Yttrium oxide (Y₂O₃), as a typical rare-earth oxide, has exhibited excellent etching resistance in fluorine-containing and argon plasma environments. In fluorine-based plasma etching, oxide ceramics typically undergo fluorination reactions with reactive species such as fluorine radicals and fluoride ions. After plasma irradiation etching, the mechanical properties of Y₂O₃ films decrease in the early stages of etching due to nanoscale surface pits. As etching progresses, a protective passivation layer forms on the surface, not only preventing further etching but also improving the flexural strength of the material. Y₂O₃ films can be deposited using various techniques, among which physical vapor deposition (PVD) is widely used due to its excellent controllability. In oxide reactive magnetron sputtering, the conversion of the target to "oxide mode" is a key factor limiting deposition efficiency. Although the metal mode has a high deposition rate, it is difficult to obtain stoichiometric films; while the oxide mode can obtain stoichiometric films, the deposition rate is extremely low. Therefore, how to achieve high-speed deposition of stoichiometric oxide films remains a core technical challenge that urgently needs to be overcome. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates, as well as the products and applications thereof, to solve the problems existing in the prior art.

[0005] To achieve the above objectives, the present invention provides the following solution: One of the technical solutions of the present invention is a method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate, comprising the following steps: using a Y target as a sputtering cathode, depositing a near-stoichiometric yttrium oxide coating on the substrate surface by mid-frequency reactive magnetron sputtering; During the deposition of near-stoichiometric yttrium oxide coating, a closed-loop feedback control system is used to dynamically regulate oxygen flow and target voltage, enabling the target to operate in the transition region between metallic and oxide modes. Dynamic control of oxygen flow rate and target voltage includes: lower limit of oxygen 0~2 sccm, upper limit of oxygen 3~6 sccm, and target voltage -210~-345V.

[0006] This invention employs physical vapor deposition (PVD) with mid-frequency reactive magnetron sputtering to prepare yttrium oxide coatings. A closed-loop feedback control system dynamically regulates oxygen flow and target voltage, allowing the target to operate in the transition region between metallic and oxide modes. This target-intermediate positioning significantly improves coating deposition efficiency and imparts near-stoichiometric characteristics, along with enhanced mechanical and corrosion resistance properties.

[0007] Further, the steps for depositing a near-stoichiometric yttrium oxide coating include: setting the target voltage to -210 to -345 V, the lower oxygen limit to 0 to 2 sccm, the upper oxygen limit to 3 to 6 sccm, the cathode sputtering power to 200 to 400 W, the substrate bias voltage to -300 to 0 V, and evacuating the reaction chamber to a vacuum level of 3 × 10⁻⁶ V. -5 ~7×10 -5 After Pa, argon and oxygen are introduced. Once the gas pressure in the reaction chamber reaches 0.2 ~ 1 Pa, the intermediate frequency power supply and closed-loop feedback control system are turned on, and the substrate bias is opened to perform reactive sputtering.

[0008] Furthermore, the temperature of the substrate during reactive sputtering is 25~400℃.

[0009] Furthermore, the deposition rate of the near-stoichiometric yttrium oxide coating is not less than 25 nm / min.

[0010] Preferably, the flow rate of the argon gas is 33 sccm.

[0011] Preferably, the reactive sputtering time for depositing a near-stoichiometric yttrium oxide coating is 60 min.

[0012] Preferably, the deposition of a yttrium metal transition layer on the substrate surface is included before depositing a near-stoichiometric yttrium oxide coating.

[0013] Preferably, the step of depositing the yttrium metal transition layer includes: setting the substrate temperature to 25~400℃, setting the cathode sputtering power to 200~400W, setting the substrate bias voltage to -300~0V, and evacuating the reaction chamber to a vacuum level of 3×10⁻⁶. -5 ~7×10 -5After Pa, argon gas is introduced. Once the gas pressure in the reaction chamber reaches 0.1~0.9 Pa, the intermediate frequency power supply is turned on and the substrate bias is applied to perform reactive sputtering.

[0014] Preferably, the reactive sputtering time for depositing the yttrium metal transition layer is 0 to 6 minutes.

[0015] Preferably, the thickness of the yttrium metal transition layer is 0~0.2μm.

[0016] Furthermore, before depositing a near-stoichiometric yttrium oxide coating on the substrate surface or before depositing a yttrium metal transition layer on the substrate surface, the process also includes glow discharge cleaning and ion bombardment treatment of the substrate.

[0017] Preferably, the method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate further includes the following steps: The substrate is loaded into the reaction chamber of the physical vapor deposition equipment and heated to 25~400℃; The substrate is subjected to glow discharge cleaning and ion bombardment treatment; A yttrium metal transition layer is deposited on the surface of the substrate; A near-stoichiometric yttrium oxide coating is deposited on the surface of the yttrium metal transition layer.

[0018] Furthermore, the glow discharge cleaning step includes: evacuating the reaction chamber to a vacuum level of 8 × 10⁻⁶. -4 ~1×10 -3 Pa, introduce argon gas, set the gas pressure to 0.5~2Pa, turn on the substrate bias voltage, set the substrate bias voltage to -900~-700V, and perform glow discharge cleaning on the substrate for 30 minutes.

[0019] Furthermore, the ion bombardment treatment steps include: introducing argon gas, setting the gas pressure to 0.5~1Pa, turning on the ion source, setting the ion source power to 1~5kW, turning on the substrate bias voltage, setting the substrate bias voltage to -800~-300V, and performing ion bombardment treatment on the substrate for 15min.

[0020] Preferably, two Y targets are provided, that is, two Y targets are used as sputtering cathodes.

[0021] Preferably, the duty cycle of both Y targets is 50% during the deposition of a near-stoichiometric yttrium oxide coating.

[0022] Preferably, the reaction chamber is provided with a sample disk for loading the substrate, and two Y-target sputtering cathodes are provided above the sample disk. The two Y-target sputtering cathodes are circular twin cathodes, and the circular twin cathodes are symmetrically distributed about the vertical axis of the sample disk.

[0023] Preferably, the angle between the circular twin cathode and the perpendicular bisector of the sample disk is 70~75°; the distance between the circular twin cathode (center point M) and the substrate surface (e.g., ...) Figure 1 (As shown by the gray arrow) is 7~10cm.

[0024] Preferably, the substrate includes an aluminum alloy substrate, a quartz glass substrate, or a single-crystal silicon wafer substrate.

[0025] The second technical solution of the present invention: a near-stoichiometric yttrium oxide coating prepared by the method described above for preparing near-stoichiometric yttrium oxide coatings at high deposition rates.

[0026] Furthermore, the near-stoichiometric yttrium oxide coating contains 40-43 at.% Y and 57-60 at.% O; in atomic percentage, O / Y = 1.3-1.5.

[0027] Furthermore, the thickness of the near-stoichiometric yttrium oxide coating is 1~2 μm.

[0028] The third technical solution of the present invention: the application of a near-stoichiometric yttrium oxide coating as described above in the preparation of a semiconductor etching machine cavity or internal components.

[0029] The present invention discloses the following technical effects: This invention employs physical vapor deposition (PVD) with mid-frequency reactive magnetron sputtering to prepare yttrium oxide coatings. By dynamically controlling the oxygen flow rate and target voltage through a closed-loop feedback control system, the target material operates in the transition region between metallic and oxide modes. This achieves a dense, near-stoichiometric yttrium oxide coating with high deposition efficiency, resulting in a film with excellent mechanical properties, such as high hardness, high elastic modulus, and strong corrosion resistance due to its dense microstructure.

[0030] The method of the present invention can prepare yttrium oxide coatings, achieving a deposition rate of not less than 25 nm / min while obtaining coatings with near stoichiometry and an O / Y ratio of 1.3 to 1.5. Attached Figure Description

[0031] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0032] Figure 1 This is a schematic diagram of the circular twin cathode and deposition equipment used in the method of preparing near-stoichiometric yttrium oxide coatings at high deposition rates according to the present invention.

[0033] Figure 2 The curve shows the hysteresis curve of the reaction between the Y-target voltage and oxygen flow rate.

[0034] Figure 3 The deposition rate of the yttrium oxide coatings prepared in Examples 1-3 and Comparative Examples 1-2 is expressed as the O / Y ratio.

[0035] Figure 4 The hardness and elastic modulus of the yttrium oxide coatings prepared in Examples 1-3 and Comparative Examples 1-2 are shown.

[0036] Figure 5 The images show the morphology and cross-sectional profiles of the yttrium oxide coated and uncoated aluminum alloy substrates prepared in Examples 1, 3, and Comparative Example 2 after Ar plasma etching.

[0037] Figure 6 The etching rates of the yttrium oxide coatings and uncoated aluminum alloy substrates prepared in Examples 1, 3, and Comparative Example 2 during Ar plasma etching are shown. Detailed Implementation

[0038] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0039] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Any stated value or intermediate value within a stated range, as well as each smaller range between any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0040] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0041] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be obvious to those skilled in the art. This specification and embodiments are merely exemplary.

[0042] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0043] It should be noted that any aspects not described in detail in this invention are conventional practices in the field and are not the focus of this invention.

[0044] As a first aspect of the present invention, the present invention provides a method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate, comprising the following steps: using a Y target as a sputtering cathode, depositing a near-stoichiometric yttrium oxide coating on a substrate surface by mid-frequency reactive magnetron sputtering; During the deposition of near-stoichiometric yttrium oxide coating, a closed-loop feedback control system is used to dynamically regulate oxygen flow and target voltage, enabling the target to operate in the transition region between metallic and oxide modes. Dynamic control of oxygen flow rate and target voltage includes: lower limit of oxygen 0~2 sccm, upper limit of oxygen 3~6 sccm, and target voltage -210~-345V.

[0045] This invention employs physical vapor deposition (PVD) with mid-frequency reactive magnetron sputtering to prepare yttrium oxide coatings. A closed-loop feedback control system dynamically regulates oxygen flow and target voltage, allowing the target to operate in the transition region between metallic and oxide modes. This target-intermediate positioning significantly improves coating deposition efficiency and imparts near-stoichiometric characteristics, along with enhanced mechanical and corrosion resistance properties.

[0046] As an embodiment of the present invention, the substrate includes an aluminum alloy substrate, a quartz glass substrate, or a single-crystal silicon wafer substrate.

[0047] As a preferred embodiment of the present invention, the method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate further includes the following steps: The substrate is loaded into the reaction chamber of the physical vapor deposition equipment and heated to 25~400℃; The substrate is subjected to glow discharge cleaning and ion bombardment treatment; A yttrium metal transition layer is deposited on the surface of the substrate; A near-stoichiometric yttrium oxide coating is deposited on the surface of the yttrium metal transition layer.

[0048] In a preferred embodiment of the present invention, when the substrate is an aluminum alloy substrate, before loading the substrate into the reaction chamber of the physical vapor deposition equipment, the method further includes: polishing the substrate to achieve a mirror finish; then ultrasonically cleaning the substrate to be deposited in a metal cleaning agent solution and anhydrous ethanol to remove impurities and contaminants adsorbed on the surface; and finally, removing and drying the substrate.

[0049] As an embodiment of the present invention, the glow discharge cleaning step includes: evacuating the reaction chamber to a vacuum level of 8×10⁻⁶. -4 ~1×10 -3 Pa, introduce argon gas, set the gas pressure to 0.5~2Pa, turn on the substrate bias voltage, set the substrate bias voltage to -900~-700V, and perform glow discharge cleaning on the substrate for 30 minutes.

[0050] In a preferred embodiment of the present invention, the glow discharge cleaning step includes: evacuating the reaction chamber to a vacuum level of 8.5 × 10⁻⁶. -4 ~9.5×10 -4 Pa, introduce argon gas, set the gas pressure to 0.7~1.3Pa, turn on the substrate bias voltage, set the substrate bias voltage to -850~-750V, and perform glow discharge cleaning on the substrate for 30 minutes.

[0051] Under the above conditions, glow discharge cleaning can effectively remove organic matter, oxide layer and other contaminants from the substrate surface, providing a clean surface for subsequent film deposition. It can also provide a rough surface to provide more bonding points for the film, which helps to improve the adhesion of the film.

[0052] As an embodiment of the present invention, the steps of the ion bombardment treatment include: introducing argon gas, setting the gas pressure to 0.5~1Pa, turning on the ion source, setting the ion source power to 1~5kW, turning on the substrate bias voltage, setting the substrate bias voltage to -800~-300V, and performing ion bombardment treatment on the substrate for 15min.

[0053] As a preferred embodiment of the present invention, the steps of the ion bombardment treatment include: introducing argon gas, setting the gas pressure to 0.6~0.8Pa, turning on the ion source, setting the ion source power to 2~3kW, turning on the substrate bias voltage, setting the substrate bias voltage to -600~-400V, and performing ion bombardment treatment on the substrate for 15min.

[0054] Under the above conditions, ion bombardment treatment can not only clean the substrate surface and remove the oxide layer and contaminants, but also increase the surface roughness.

[0055] As an embodiment of the present invention, the step of depositing a yttrium metal transition layer includes: setting the substrate temperature to 25~400℃, setting the cathode sputtering power to 200~400W, setting the substrate bias voltage to -300~0V, and evacuating the reaction chamber to a vacuum level of 3×10⁻⁶. -5 ~7×10 -5 After Pa, argon gas is introduced. Once the gas pressure in the reaction chamber reaches 0.1~0.9 Pa, the intermediate frequency power supply is turned on and the substrate bias is applied to perform reactive sputtering.

[0056] In a preferred embodiment of the present invention, the step of depositing the yttrium metal transition layer includes: setting the substrate temperature to 25~350℃, setting the cathode sputtering power to 250~350W, setting the substrate bias voltage to -200~0V, and evacuating the reaction chamber to a vacuum level of 4×10⁻⁶. -5 ~6×10 -5 After Pa, argon gas is introduced. Once the gas pressure in the reaction chamber reaches 0.4~0.6 Pa, the intermediate frequency power supply is turned on and the substrate bias is applied to perform reactive sputtering.

[0057] In a preferred embodiment of the present invention, the reactive sputtering time during the deposition of the yttrium metal transition layer is 0 to 6 minutes.

[0058] In a preferred embodiment of the present invention, the thickness of the yttrium metal transition layer is 0~0.2μm; exemplary thicknesses are 0.05μm, 0.10μm or 0.18μm, and are not limited to the above examples.

[0059] It should be noted that depositing a yttrium metal transition layer on the substrate, followed by the deposition of yttrium oxide, can improve the interfacial bonding between the yttrium oxide film and the substrate.

[0060] As an embodiment of the present invention, the step of depositing a near-stoichiometric yttrium oxide coating includes: setting the target voltage to -210~-345V, the lower limit of oxygen to 0~2sccm, the upper limit of oxygen to 3~6sccm, the cathode sputtering power to 200~400W, the substrate bias voltage to -300~0V, and evacuating the reaction chamber to a vacuum level of 3×10⁻⁶. -5 ~7×10 -5 After Pa, argon and oxygen are introduced. When the gas pressure in the reaction chamber reaches 0.2~1 Pa, the intermediate frequency power supply and closed-loop feedback control system are turned on and the substrate bias is turned on to carry out reactive sputtering. The temperature of the substrate during the reactive sputtering process is 25~400℃.

[0061] The present invention provides a method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates. The coating is prepared by physical vapor deposition. The oxygen flow rate and target control voltage are dynamically adjusted by a closed-loop feedback control system, so that the target material works in the transition region between the metal mode and the oxidation mode. A dense near-stoichiometric yttrium oxide coating is obtained at high deposition efficiency, thereby giving the film excellent mechanical properties, such as high hardness, high elastic modulus and strong corrosion resistance due to its dense structure.

[0062] Substrate bias is a crucial parameter in physical vapor deposition (PVD), especially when controlling the energy of the substrate surface and the quality of the deposited film is necessary during the deposition process. Substrate bias typically refers to the voltage applied to the substrate, which controls charge accumulation on the substrate surface, the dynamics of deposited particles, and the properties of the film. Generally, a negative bias voltage (negative substrate bias) is applied to the substrate, making the substrate the cathode. In this case, ions from the source are accelerated and bombard the substrate surface, increasing particle energy and improving the quality, adhesion, and density of the deposited film. Preferably, the substrate bias voltage is set to -200 to 0 V. Appropriate bias voltage promotes the migration of deposited atoms, contributing to a higher coating deposition rate.

[0063] As a preferred embodiment of the present invention, the step of depositing a near-stoichiometric yttrium oxide coating includes: setting the target voltage to -280~-320V, the lower limit of oxygen to 0~1sccm, the upper limit of oxygen to 4~5sccm, the cathode sputtering power to 200~400W, the substrate bias voltage to -200~0V, and evacuating the reaction chamber to a vacuum level of 4×10⁻⁶. -5 ~6×10 -5 After Pa, argon and oxygen are introduced. Once the gas pressure in the reaction chamber reaches 0.4~0.6 Pa, the intermediate frequency power supply and closed-loop feedback control system are turned on, and the substrate bias voltage is opened to perform reactive sputtering. The temperature of the substrate during the reactive sputtering process is 25~350℃.

[0064] Among these factors, appropriate sputtering power is used to ensure that the deposited particles have sufficient energy for uniform deposition and crystallization. A high vacuum level in the reaction chamber reduces interference from oxygen impurities in the coating, ensuring that the O / Y ratio is close to the stoichiometric ratio.

[0065] In a preferred embodiment of the present invention, the argon gas flow rate is 33 sccm when depositing a near-stoichiometric yttrium oxide coating.

[0066] In a preferred embodiment of the present invention, the reaction sputtering time is 60 min when depositing a near-stoichiometric yttrium oxide coating.

[0067] In a preferred embodiment of the present invention, two Y targets are provided.

[0068] In a preferred embodiment of the present invention, the duty cycle of both Y targets is 50% during the deposition of a near-stoichiometric yttrium oxide coating.

[0069] As a preferred embodiment of the present invention, such as Figure 1 (A schematic diagram of the circular twin cathode and deposition equipment used in the method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates) shows that the reaction chamber is provided with a sample disk for loading the substrate, and two Y-target sputtering cathodes are provided above the sample disk. The two Y-target sputtering cathodes are circular twin cathodes, and the circular twin cathodes are symmetrically distributed about the vertical axis of the sample disk.

[0070] It should be noted that a closed-loop feedback control system is an automated control system used to monitor and adjust various parameters during the deposition process in real time to ensure coating quality. Closed-loop feedback control systems are typically based on sensor feedback mechanisms, enabling the deposition process to dynamically adjust according to target setpoints, thereby achieving high-precision thin film preparation. In the PVD process, the type and flow rate of gases have a significant impact on the composition and quality of the film. The closed-loop feedback control system monitors gas flow rate and pressure, adjusting gas flow control valves or flow meters to maintain the required atmospheric conditions. When the target voltage increases, it indicates a shift to the target metal mode. Subsequently, the closed-loop feedback control system gradually increases the oxygen flow rate. Once the target is detected to have entered the oxide mode, causing a voltage drop, the oxygen flow rate immediately decreases. The specific feedback hysteresis curve is shown below. Figure 2 As shown. In this invention, the closed-loop feedback control system sets the target voltage to -210~-345V, the lower oxygen limit to 0~2sccm, and the upper oxygen limit to 3~6sccm in control mode. Preferably, the closed-loop feedback control system sets the target voltage to -280~-320V, the lower oxygen limit to 0~1sccm, and the upper oxygen limit to 4~5sccm in control mode. Sufficient oxygen partial pressure is beneficial to the growth of face-centered cubic close-packed crystal structures, while excessively high oxygen partial pressure can easily cause poisoning of the target surface. A high deposition rate needs to be maintained under a certain oxygen partial pressure. This invention, through high-frequency monitoring and adjustment, enables the target to operate stably in the transition region between the metallic and oxide modes, ensuring a near-stoichiometric coating ratio and a high deposition rate.

[0071] Additionally, it should be noted that twin cathodes typically refer to the use of two cathode targets of the same or different materials during sputtering deposition, which are sputtered alternately in parallel. In the twin cathode system of this invention, a medium-frequency power pulse mode is adopted, and Y targets of the same composition alternately serve as cathodes within one voltage cycle. By having the twin cathodes work alternately as cathodes, the electrostatic charge accumulated on the target surface due to the deposition of non-conductive materials during oxide deposition is neutralized, eliminating target poisoning that affects the stability of insulating film deposition and creating a stable deposition environment for Y2O3 thin film materials.

[0072] As an embodiment of the present invention, the angle between the circular twin cathode and the perpendicular bisector of the sample disk is 70~75°; the distance between the circular twin cathode and the substrate surface is 7~10cm.

[0073] In a preferred embodiment of the present invention, the angle between the circular twin cathode and the perpendicular bisector of the sample disk is 75°; the distance between the circular twin cathode and the substrate surface is 8~9cm.

[0074] Circular twin cathodes can eliminate target poisoning, which affects the stability of insulating film deposition. Currently, the preferred angle between the circular twin cathode and the sample disk, as well as the height of the circular twin cathode, can enhance the ionization and energy of deposited ions, thereby improving the compactness of the deposited film.

[0075] As an embodiment of the present invention, the temperature of the sample disk is 25~400℃ (to heat the substrate), preferably 25~350℃, and the sample disk is rotated to ensure uniform heating of the substrate.

[0076] As an embodiment of the present invention, the deposition rate of the near-stoichiometric yttrium oxide coating is not less than 25 nm / min.

[0077] As a second aspect of the present invention, the present invention provides a near-stoichiometric yttrium oxide coating prepared by the method described above for preparing near-stoichiometric yttrium oxide coatings at high deposition rates.

[0078] As an embodiment of the present invention, the content of Y element in the near stoichiometric yttrium oxide coating is 40~43 at.% and the content of O element is 57~60 at.%; in atomic percentage, O / Y = 1.3~1.5.

[0079] As an embodiment of the present invention, the thickness of the near stoichiometric yttrium oxide coating is 1~2 μm, and exemplary thicknesses are 1.50 μm, 1.86 μm or 1.92 μm, and are not limited to the above examples.

[0080] As a third aspect of the invention, the invention provides the application of the near-stoichiometric yttrium oxide coating as described above in the preparation of a semiconductor etching machine cavity or internal components.

[0081] The near-stoichiometric yttrium oxide coating is used to prepare a plasma-resistant etching material for use in the cavity or internal components of a semiconductor etching machine. The internal components of the etching machine include a viewing window, a gas dispersion disk, a nozzle, an insulating ring, a cover plate, a focusing ring, and an electrostatic chuck. The near-stoichiometric yttrium oxide coating prepared by the method of this invention achieves a deposition rate of not less than 25 nm / min, with an O / Y ratio of 1.3 to 1.5. The target material is positioned between the metallic and oxide modes, significantly improving the coating deposition efficiency and giving the coating better mechanical and corrosion resistance properties.

[0082] The technical solution of the present invention will be further described below with reference to specific embodiments.

[0083] In the following embodiments, comparative examples and test examples of the present invention, if room temperature is involved, it specifically refers to 25~30℃.

[0084] All raw materials used in the following embodiments, comparative examples and test examples of this invention are commercially available products.

[0085] The following embodiments of the present invention illustrate the structure of the circular twin cathode used to prepare near-stoichiometric yttrium oxide coatings at high deposition rates, and the schematic diagram of the deposition equipment (medium-frequency reactive magnetron sputtering equipment) as shown in the figures. Figure 1 As shown, the reaction chamber is equipped with a sample disk for loading the substrate. Above the sample disk are two Y-target sputtering cathodes, which are circular twin cathodes. The circular twin cathodes are symmetrically distributed about the perpendicular bisector of the sample disk. The angle between the circular twin cathodes and the perpendicular bisector of the sample disk is 75°. The distance between the circular twin cathodes and the surface of the substrate is 8.5 cm.

[0086] Example 1 A method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates includes the following steps: (1) Substrate pretreatment and installation The substrate was selected from aluminum alloy (16mm×16mm×4mm). The substrate was polished using polishing cloth and polishing fluid, achieving a mirror finish with a roughness of 40nm. After polishing, the aluminum alloy substrate was ultrasonically cleaned in a metal cleaning solution for 20 minutes, followed by ultrasonic cleaning in anhydrous ethanol for 20 minutes to remove surface-adsorbed impurities and contaminants. After completion, the aluminum alloy substrate was removed, dried, and loaded into the reaction chamber of the physical vapor deposition equipment, specifically placed at the center of the sample tray within the reaction chamber.

[0087] (2) Perform glow discharge cleaning and ion bombardment treatment on the substrate. The vacuum level in the reaction chamber was evacuated to 9 × 10⁻⁶ at room temperature. -4 At 100 sccm, argon gas was introduced, and the pressure was set to 1.0 Pa. The rotation speed of the sample tray was set to 20 rpm. The substrate bias was turned on and set to -800 V. The substrate was then subjected to glow discharge cleaning for 30 minutes. Next, the substrate was subjected to ion bombardment treatment. The argon gas flow rate was adjusted to 70 sccm, and the pressure was set to 0.7 Pa. After the pressure stabilized at the set value, the ion source was turned on, and the ion source power was set to 2.5 kW. The substrate bias was turned on and set to -500 V. The substrate was then subjected to ion bombardment treatment for 15 minutes.

[0088] (3) Deposit a yttrium metal transition layer on the substrate surface At room temperature, the rotation speed of the rotating frame (i.e., the sample disk) was set to 20 rpm, the cathode sputtering power of the intermediate frequency power supply was set to 300 W, the duty cycle of both Y targets was set to 50%, the substrate bias voltage was set to -100 V, and the vacuum level in the reaction chamber was evacuated to 5 × 10⁻⁶. -5 After Pa, 33 sccm of argon gas was introduced. After the gas pressure in the reaction chamber stabilized at 0.5 Pa (the gas pressure stabilized at 0.5 Pa during sputtering), the intermediate frequency power supply was turned on and the substrate bias was turned on. Reactive sputtering was performed for 3 minutes to deposit a yttrium metal transition layer with a thickness of 0.1 μm on the substrate surface.

[0089] (4) Deposit yttrium oxide coating on the surface of yttrium metal transition layer Under room temperature conditions and in closed-loop feedback control mode, the target voltage was set to -300V, the lower oxygen limit was set to 0 sccm, and the upper oxygen limit was set to 5 sccm. The intermediate frequency power supply was set to 300W for cathode sputtering, the duty cycle of both Y targets was set to 50%, and the substrate bias was set to 0V. The rotation speed of the rotating frame (i.e., the sample tray) was set to 20 rpm. The vacuum in the reaction chamber was evacuated until it reached a vacuum level of 5 × 10⁻⁶. -5 Argon gas at 33 sccm and oxygen gas were introduced. After the gas pressure in the reaction chamber stabilized at 0.5 Pa (the gas pressure stabilized at 0.5 Pa during the reactive sputtering process), the intermediate frequency power supply and closed-loop feedback control system were turned on, and the substrate bias was opened. Reactive sputtering was performed for 60 minutes to deposit a yttrium oxide coating on the surface of the yttrium metal transition layer. The thickness of the obtained yttrium oxide coating was measured to be 1.86 µm.

[0090] The elemental composition and deposition rate of the yttrium oxide coating prepared in this embodiment were analyzed, and the results are as follows: Figure 3As shown, the yttrium oxide coating contains 42.45 at.% Y and 57.55 at.% O, with an O / Y ratio (atomic percentage) of 1.36. The deposition rate of the yttrium oxide coating is approximately 31 nm / min.

[0091] The hardness and elastic modulus of the yttrium oxide coating prepared in this embodiment were tested according to ISO 14577 standard, and the results are as follows: Figure 4 As shown, the yttrium oxide coating has a hardness of 13.26 GPa and an elastic modulus of 190.0 GPa.

[0092] Example 2 A method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates includes the following steps: (1) Substrate pretreatment and installation The substrate was selected from aluminum alloy (16mm×16mm×4mm). The substrate was polished using polishing cloth and polishing fluid, achieving a mirror finish with a roughness of 40nm. After polishing, the aluminum alloy substrate was ultrasonically cleaned in a metal cleaning solution for 20 minutes, followed by ultrasonic cleaning in anhydrous ethanol for 20 minutes to remove surface-adsorbed impurities and contaminants. After completion, the aluminum alloy substrate was removed, dried, and loaded into the reaction chamber of the physical vapor deposition equipment, specifically placed at the center of the sample tray within the reaction chamber.

[0093] (2) Perform glow discharge cleaning and ion bombardment treatment on the substrate. The vacuum level in the reaction chamber was evacuated to 9 × 10⁻⁶ at room temperature. -4 At 100 sccm, argon gas was introduced, and the pressure was set to 1.0 Pa. The rotation speed of the sample tray was set to 20 rpm. The substrate bias was turned on and set to -800 V. The substrate was then subjected to glow discharge cleaning for 30 minutes. Next, the substrate was subjected to ion bombardment treatment. The argon gas flow rate was adjusted to 70 sccm, and the pressure was set to 0.7 Pa. After the pressure stabilized at the set value, the ion source was turned on, and the ion source power was set to 2.5 kW. The substrate bias was turned on and set to -500 V. The substrate was then subjected to ion bombardment treatment for 15 minutes.

[0094] (3) Deposit a yttrium metal transition layer on the substrate surface At room temperature, the rotation speed of the rotating frame (i.e., the sample disk) was set to 20 rpm, the cathode sputtering power of the intermediate frequency power supply was set to 300 W, the duty cycle of both Y targets was set to 50%, the substrate bias voltage was set to -100 V, and the vacuum level in the reaction chamber was evacuated to 5 × 10⁻⁶. -5After Pa, 33 sccm of argon gas was introduced. Once the gas pressure in the reaction chamber stabilized at 0.5 Pa, the intermediate frequency power supply was turned on and the substrate bias was applied. Reaction sputtering was performed for 3 minutes to deposit a 0.1 μm thick yttrium metal transition layer on the substrate surface.

[0095] (4) Deposit yttrium oxide coating on the surface of yttrium metal transition layer Under room temperature conditions and in closed-loop feedback control mode, the target voltage was set to -300V, the lower oxygen limit to 0 sccm, and the upper oxygen limit to 5 sccm. The intermediate frequency power supply was set to a cathode sputtering power of 300W, the duty cycle of both Y targets to 50%, and the substrate bias to -200V. The rotating frame (sample tray) speed was set to 20 rpm. The reaction chamber was evacuated until a vacuum of 5 × 10⁻⁶ was achieved. -5 Argon gas at 33 sccm and oxygen gas were introduced. After the gas pressure in the reaction chamber stabilized at 0.5 Pa, the intermediate frequency power supply and closed-loop feedback control system were turned on, and the substrate bias voltage was opened. Reactive sputtering was performed for 60 minutes to deposit a yttrium oxide coating on the surface of the yttrium metal transition layer. The thickness of the obtained yttrium oxide coating was measured to be 1.92 µm.

[0096] The elemental composition and deposition rate of the yttrium oxide coating prepared in this embodiment were analyzed, and the results are as follows: Figure 3 As shown, the yttrium oxide coating contains 41.83 at.% Y and 58.17 at.% O, with an O / Y ratio (atomic percentage) of 1.39. The deposition rate of the yttrium oxide coating is approximately 32 nm / min.

[0097] The hardness and elastic modulus of the yttrium oxide coating prepared in this embodiment were tested according to ISO 14577 standard, and the results are as follows: Figure 4 As shown, the yttrium oxide coating has a hardness of 11.56 GPa and an elastic modulus of 189.7 GPa.

[0098] Example 3 A method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates includes the following steps: (1) Substrate pretreatment and installation Aluminum alloy was selected as the substrate. The substrate was polished using polishing cloth and polishing fluid, achieving a mirror finish with a roughness of 40 nm. The polished aluminum alloy substrate was then ultrasonically cleaned in a metal cleaning solution for 20 minutes, followed by ultrasonic cleaning in anhydrous ethanol for another 20 minutes to remove surface-adsorbed impurities and contaminants. After completion, the aluminum alloy substrate was removed, dried, and loaded into the reaction chamber of the physical vapor deposition (PVD) equipment. Specifically, the aluminum alloy substrate was placed at the center of the sample tray in the reaction chamber, and the sample tray heating temperature was set to 300°C. The substrate was heated to 300°C using the sample tray, which was rotated (at 20 rpm) during the heating process to ensure uniform heating. (Subsequent glow discharge cleaning, ion bombardment treatment, deposition of the yttrium metal transition layer, and deposition of the yttrium oxide coating were all performed under these conditions of sample tray heating at 300°C and rotation at 20 rpm.)

[0099] (2) Perform glow discharge cleaning and ion bombardment treatment on the substrate. Evacuate until the vacuum level in the reaction chamber reaches 9×10 -4 At 100 sccm, argon gas was introduced at a pressure of 1.0 Pa. The substrate bias was turned on and set to -800 V. The substrate was then subjected to glow discharge cleaning for 30 minutes. Next, the substrate was subjected to ion bombardment treatment. The argon gas flow rate was adjusted to 70 sccm, and the pressure was set to 0.7 Pa. After the pressure stabilized at the set value, the ion source was turned on with a power of 2.5 kW. The substrate bias was turned on and set to -500 V. The substrate was then subjected to ion bombardment treatment for 15 minutes.

[0100] (3) Deposit a yttrium metal transition layer on the substrate surface The rotation speed of the rotating frame (i.e., the sample tray) was set to 20 rpm, the sample tray heating temperature was set to 300℃ (i.e., the substrate temperature was 300℃), the intermediate frequency power supply cathode sputtering power was set to 300W, the duty cycle of both Y targets was set to 50%, the substrate bias voltage was set to -100V, and the vacuum in the reaction chamber was evacuated until the vacuum level reached 5×10⁻⁶. -5 After Pa, 33 sccm of argon gas was introduced. Once the gas pressure in the reaction chamber stabilized at 0.5 Pa, the intermediate frequency power supply was turned on and the substrate bias was applied. Reaction sputtering was performed for 3 minutes to deposit a 0.1 μm thick yttrium metal transition layer on the substrate surface.

[0101] (4) Deposit yttrium oxide coating on the surface of yttrium metal transition layer The rotating frame (sample tray) was set to rotate at 20 rpm, and the sample tray heating temperature was set to 300℃. Under the closed-loop feedback control system, the target voltage was set to -300V, the lower oxygen limit to 0 sccm, and the upper oxygen limit to 5 sccm. The intermediate frequency power supply was set to a cathode sputtering power of 300W, the duty cycle of both Y targets was set to 50%, and the substrate bias voltage was set to 0V. The reaction chamber was evacuated until the vacuum level reached 5 × 10⁻⁶. -5 Argon gas at 33 sccm and oxygen gas were introduced. After the gas pressure in the reaction chamber stabilized at 0.5 Pa, the intermediate frequency power supply and closed-loop feedback control system were turned on, and the substrate bias voltage was opened. Reactive sputtering was performed for 60 minutes to deposit a yttrium oxide coating on the surface of the yttrium metal transition layer. The thickness of the obtained yttrium oxide coating was measured to be 1.50 µm.

[0102] The elemental composition and deposition rate of the yttrium oxide coating prepared in this embodiment were analyzed, and the results are as follows: Figure 3 As shown, the yttrium oxide coating contains 41.47 at.% Y and 58.53 at.% O, with an O / Y ratio (atomic percentage) of 1.41. The deposition rate of the yttrium oxide coating is approximately 25 nm / min.

[0103] The hardness and elastic modulus of the yttrium oxide coating prepared in this embodiment were tested according to ISO 14577 standard, and the results are as follows: Figure 4 As shown, the yttrium oxide coating has a hardness of 13.20 GPa and an elastic modulus of 222.0 GPa.

[0104] Comparative Example 1 A method for preparing yttrium oxide coatings using a Y-target in a near-metallic mode comprises the following steps: (1) Substrate pretreatment and installation The substrate was made of aluminum alloy. Polishing was performed using a polishing cloth and polishing fluid, achieving a mirror finish with a roughness of 40 nm. The polished aluminum alloy substrate was then ultrasonically cleaned in a metal cleaning solution for 20 minutes, followed by ultrasonic cleaning in anhydrous ethanol for another 20 minutes to remove surface-adsorbed impurities and contaminants. After completion, the aluminum alloy substrate was removed, dried, and loaded into the reaction chamber of the physical vapor deposition equipment, specifically placed at the center of the sample tray within the reaction chamber.

[0105] (2) Perform glow discharge cleaning and ion bombardment treatment on the substrate. The vacuum level in the reaction chamber was evacuated to 9 × 10⁻⁶ at room temperature. -4At 100 sccm, argon gas was introduced, and the pressure was set to 1.0 Pa. The rotation speed of the sample tray was set to 20 rpm. The substrate bias was turned on and set to -800 V. The substrate was then subjected to glow discharge cleaning for 30 minutes. Next, the substrate was subjected to ion bombardment treatment. The argon gas flow rate was adjusted to 70 sccm, and the pressure was set to 0.7 Pa. After the pressure stabilized at the set value, the ion source was turned on, and the ion source power was set to 2.5 kW. The substrate bias was turned on and set to -500 V. The substrate was then subjected to ion bombardment treatment for 15 minutes.

[0106] (3) Deposit a yttrium metal transition layer on the substrate surface At room temperature, the rotation speed of the rotating frame (i.e., the sample disk) was set to 20 rpm, the cathode sputtering power of the intermediate frequency power supply was set to 300 W, the duty cycle of both Y targets was set to 50%, the substrate bias voltage was set to -100 V, and the vacuum level in the reaction chamber was evacuated to 5 × 10⁻⁶. -5 After Pa, 33 sccm of argon gas was introduced. Once the gas pressure in the reaction chamber stabilized at 0.5 Pa, the intermediate frequency power supply was turned on and the substrate bias was applied. Reaction sputtering was performed for 3 minutes to deposit a 0.1 μm thick yttrium metal transition layer on the substrate surface.

[0107] (4) Deposit yttrium oxide coating on the surface of yttrium metal transition layer The oxygen flow rate was set to 2.6 sccm at room temperature. The intermediate frequency power supply was set to 300W for cathode sputtering, the duty cycle of both Y targets was set to 50%, and the substrate bias voltage was set to 0V. The rotation speed of the rotating frame (i.e., the sample tray) was set to 20 rpm. The vacuum level in the reaction chamber was evacuated to 5 × 10⁻⁶. -5 The reaction chamber was pressurized with 33 sccm of argon and 2.6 sccm of oxygen. After the pressure inside the chamber stabilized at 0.5 Pa, the intermediate frequency power supply was turned on, and reactive sputtering was performed for 40 minutes to deposit a yttrium oxide coating on the surface of the yttrium metal transition layer. The thickness of the obtained yttrium oxide coating was measured to be 2.64 µm.

[0108] The elemental composition and deposition rate of the yttrium oxide coating prepared in this comparative example were analyzed, and the results are as follows: Figure 3 As shown, the yttrium oxide coating contains 50.99 at.% Y and 49.01 at.% O, with an O / Y ratio (atomic percentage) of 0.96. The deposition rate of the yttrium oxide coating is approximately 66 nm / min.

[0109] The hardness and elastic modulus of the yttrium oxide coating prepared in this comparative example were tested according to ISO 14577 standard, and the results are as follows: Figure 4 As shown, the yttrium oxide coating has a hardness of 5.74 GPa and an elastic modulus of 113.1 GPa.

[0110] Comparative Example 2 A method for preparing yttrium oxide coatings using a Y-target in near-oxidation mode comprises the following steps: (1) Substrate pretreatment and installation The substrate was made of aluminum alloy. Polishing was performed using a polishing cloth and polishing fluid, achieving a mirror finish with a roughness of 40 nm. The polished aluminum alloy substrate was then ultrasonically cleaned in a metal cleaning solution for 20 minutes, followed by ultrasonic cleaning in anhydrous ethanol for another 20 minutes to remove surface-adsorbed impurities and contaminants. After completion, the aluminum alloy substrate was removed, dried, and loaded into the reaction chamber of the physical vapor deposition equipment, specifically placed at the center of the sample tray within the reaction chamber.

[0111] (2) Perform glow discharge cleaning and ion bombardment treatment on the substrate. The vacuum level in the reaction chamber was evacuated to 9 × 10⁻⁶ at room temperature. -4 At 100 sccm, argon gas was introduced, and the pressure was set to 1.0 Pa. The rotation speed of the sample tray was set to 20 rpm. The substrate bias was turned on and set to -800 V. The substrate was then subjected to glow discharge cleaning for 30 minutes. Next, the substrate was subjected to ion bombardment treatment. The argon gas flow rate was adjusted to 70 sccm, and the pressure was set to 0.7 Pa. After the pressure stabilized at the set value, the ion source was turned on, and the ion source power was set to 2.5 kW. The substrate bias was turned on and set to -500 V. The substrate was then subjected to ion bombardment treatment for 15 minutes.

[0112] (3) Deposit a yttrium metal transition layer on the substrate surface At room temperature, the rotation speed of the rotating frame (i.e., the sample disk) was set to 20 rpm, the cathode sputtering power of the intermediate frequency power supply was set to 300 W, the duty cycle of both Y targets was set to 50%, the substrate bias voltage was set to -100 V, and the vacuum level in the reaction chamber was evacuated to 5 × 10⁻⁶. -5 After Pa, 33 sccm of argon gas was introduced. Once the gas pressure in the reaction chamber stabilized at 0.5 Pa, the intermediate frequency power supply was turned on and the substrate bias was applied. Reaction sputtering was performed for 3 minutes to deposit a 0.1 μm thick yttrium metal transition layer on the substrate surface.

[0113] (4) Deposit yttrium oxide coating on the surface of yttrium metal transition layer The oxygen flow rate was set to 3.6 sccm at room temperature. The intermediate frequency power supply was set to 300W for cathode sputtering, the duty cycle of both Y targets was set to 50%, and the substrate bias voltage was set to 0V. The rotation speed of the rotating frame (i.e., the sample tray) was set to 20 rpm. The vacuum level in the reaction chamber was evacuated to 5 × 10⁻⁶. -5The reaction chamber was pressurized with 33 sccm of argon and 3.6 sccm of oxygen. After the pressure inside the chamber stabilized at 0.5 Pa, the intermediate frequency power supply was turned on, and reactive sputtering was performed for 120 minutes to deposit a yttrium oxide coating on the surface of the yttrium metal transition layer. The thickness of the obtained yttrium oxide coating was measured to be approximately 0.36 µm.

[0114] The elemental composition and deposition rate of the yttrium oxide coating prepared in this comparative example were analyzed, and the results are as follows: Figure 3 As shown, the yttrium oxide coating contains 50.99 at.% Y and 49.01 at.% O, with an O / Y ratio (atomic percentage) of 0.96. The deposition rate of the yttrium oxide coating is approximately 3 nm / min.

[0115] The hardness and elastic modulus of the yttrium oxide coating prepared in this comparative example were tested according to ISO 14577 standard, and the results are as follows: Figure 4 As shown, the yttrium oxide coating has a hardness of 4.19 GPa and an elastic modulus of 133.9 GPa.

[0116] Test Example 1 Plasma etching tests were conducted on the yttrium oxide coated and uncoated aluminum alloy substrates prepared in Examples 1, 3, and Comparative Example 2. The etching parameters were: ion source power: 1500W, bias voltage: -200V, Ar: 150sccm, gas pressure: 0.8Pa, and time: 40min. The test results are as follows: Figure 5 and Figure 6 As shown.

[0117] Figure 5 The images show the morphology and cross-sectional profiles of the yttrium oxide coated and uncoated aluminum alloy substrates prepared in Examples 1, 3, and Comparative Example 2 after Ar plasma etching.

[0118] Figure 6 The etching rates of the yttrium oxide coatings and uncoated aluminum alloy substrates prepared in Examples 1, 3, and Comparative Example 2 during Ar plasma etching are shown.

[0119] The results show that: The etching depth of the uncoated aluminum alloy substrate is approximately 478.32 nm.

[0120] In Example 1, the etching depth of the yttrium oxide coating obtained on the surface of the aluminum alloy substrate was approximately 44.20-242.74 nm.

[0121] In Example 3, the etching depth of the yttrium oxide coating obtained on the surface of the aluminum alloy substrate was approximately 46.05 nm.

[0122] The etching depth of the yttrium oxide coating obtained on the surface of the aluminum alloy substrate in Comparative Example 2 was approximately 120.68-262.88 nm.

[0123] A comprehensive comparison shows that the near-stoichiometric yttrium oxide coatings prepared at high deposition rates in Examples 1 and 3 have significantly smaller etching depths than the yttrium oxide coatings prepared with the target material in near-metal and near-oxidation modes in Comparative Example 2. This indicates that the near-stoichiometric yttrium oxide coatings prepared at high deposition rates in this invention can effectively resist etching by Ar plasma.

[0124] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims

1. A method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate, characterized in that, The process includes the following steps: using a Y target as the sputtering cathode, a near-stoichiometric yttrium oxide coating is deposited on the substrate surface by mid-frequency reactive magnetron sputtering; During the deposition of near-stoichiometric yttrium oxide coating, a closed-loop feedback control system is used to dynamically regulate oxygen flow and target voltage, enabling the target to operate in the transition region between metallic and oxide modes. Dynamic control of oxygen flow rate and target voltage includes: lower limit of oxygen 0~2 sccm, upper limit of oxygen 3~6 sccm, and target voltage -210~-345V.

2. The method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates as described in claim 1, characterized in that, The steps for depositing a near-stoichiometric yttrium oxide coating include: setting the target voltage to -210~-345V, the lower oxygen limit to 0~2sccm, the upper oxygen limit to 3~6sccm, the cathode sputtering power to 200~400W, the substrate bias voltage to -300~0V, and evacuating the reaction chamber to a vacuum level of 3×10⁻⁶. -5 ~7×10 -5 After Pa, argon and oxygen are introduced. Once the gas pressure in the reaction chamber reaches 0.2 ~ 1 Pa, the intermediate frequency power supply and closed-loop feedback control system are turned on, and the substrate bias is opened to perform reactive sputtering.

3. The method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates as described in claim 2, characterized in that, The temperature of the substrate during reactive sputtering is 25~400℃; And / or, the deposition rate of the near-stoichiometric yttrium oxide coating is not less than 25 nm / min.

4. The method for preparing near-stoichiometric yttrium oxide coatings at high deposition rates as described in claim 1, characterized in that, The deposition of a near-stoichiometric yttrium oxide coating also includes the deposition of a yttrium metal transition layer on the substrate surface.

5. The method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate as described in claim 4, characterized in that, The steps for depositing the yttrium metal transition layer include: setting the substrate temperature to 25~400℃, setting the cathode sputtering power to 200~400W, setting the substrate bias voltage to -300~0V, and evacuating the reaction chamber to a vacuum level of 3×10⁻⁶. -5 ~7×10 -5 After Pa, argon gas is introduced. Once the gas pressure in the reaction chamber reaches 0.1~0.9 Pa, the intermediate frequency power supply is turned on and the substrate bias is applied to perform reactive sputtering.

6. The method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate as described in claim 1 or claim 4, characterized in that, Before depositing a near-stoichiometric yttrium oxide coating on the substrate surface or before depositing a yttrium metal transition layer on the substrate surface, the process also includes glow discharge cleaning and ion bombardment treatment of the substrate.

7. The method for preparing a near-stoichiometric yttrium oxide coating at a high deposition rate as described in claim 6, characterized in that, The glow discharge cleaning step includes: evacuating the reaction chamber to a vacuum level of 8 × 10⁻⁶. -4 ~1×10 -3 Pa, introduce argon gas, set the gas pressure to 0.5~2 Pa, turn on the substrate bias voltage, set the substrate bias voltage to -900~-700V, and perform glow discharge cleaning on the substrate for 30 minutes; And / or, the steps of the ion bombardment treatment include: introducing argon gas, setting the gas pressure to 0.5~1Pa, turning on the ion source, setting the ion source power to 1~5kW, turning on the substrate bias voltage, setting the substrate bias voltage to -800~-300V, and performing ion bombardment treatment on the substrate for 15min.

8. A near-stoichiometric yttrium oxide coating prepared by the method for preparing near-stoichiometric yttrium oxide coatings at a high deposition rate as described in any one of claims 1 to 7.

9. The near-stoichiometric yttrium oxide coating as described in claim 8, characterized in that, The near-stoichiometric yttrium oxide coating contains 40-43 at.% Y and 57-60 at.% O; the O / Y ratio is 1.3-1.5 in atomic percentage.

10. The application of a near-stoichiometric yttrium oxide coating as described in any one of claims 8 to 9 in the fabrication of a semiconductor etching machine cavity or internal components.

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