An adsorption film plating structure suitable for an ultra-high vacuum cavity and a preparation device thereof

Abstract

The utility model discloses a kind of getter film plating structure and preparation device suitable for extremely high vacuum cavity, it is related to vacuum technical field, to solve the existing getter film adsorption single, film forming is poor, disassembly is inconvenient Problem.Plating structure contains 304 stainless steel or oxygen-free copper cavity base material, its inner surface is plated 500-800nm titanium-zirconium composite base film and 100-200nm non-evaporable getter surface layer in sequence, can efficiently adsorb multiple residual gas.Preparation process relies on the device main body containing shell, electronic gun is equipped in shell, double placement bin with heating component, top round hole is equipped with detachable component, base material component is fixed by clamping groove, stud nut, disassembly is convenient, and sealing strip and sealing ring guarantee sealing property.The scheme can make that cavity vacuum degree is stable to 10-12Pa magnitude, satisfy high-end field demand.

Description

Technical Field

[0001] This utility model relates to the field of vacuum, specifically to a gas-absorbing film coating structure and preparation device suitable for ultra-high vacuum cavities. Background Technology

[0002] In semiconductor manufacturing, aerospace vacuum simulation, high-energy physics experiments, and other fields with extremely high requirements for vacuum environments (requiring a vacuum level of 1000°C), [the following fields are mentioned]. -12 In the field of vacuum chambers (on the Pa scale), gas adsorption and degassing are key challenges restricting the achievement and maintenance of ultimate vacuum. Traditional vacuum chambers rely on the low degassing characteristics of the material itself and surface treatment processes (such as polishing and acid washing) to reduce gas interference. However, these passive methods cannot completely eliminate the adsorption of residual gases (such as H2, CO, CH4, etc.) on the chamber surface, and cannot actively capture the trace gas molecules continuously generated in the vacuum environment, making it difficult to meet the long-term stability requirements of ultra-high vacuum (XHV).

[0003] To address this issue, getter membrane technology has gradually gained attention. Getter membranes effectively enhance vacuum levels and maintain their stability by actively adsorbing residual gas molecules within a vacuum chamber. Existing getter membranes mostly employ a single material (such as titanium or zirconium) deposited onto the chamber surface using processes like resistance evaporation or electron beam evaporation. However, this approach has several shortcomings: Firstly, single getter materials have limited selectivity for different gases, and their vacuum-maintaining capacity is prone to decline due to adsorption saturation or performance degradation over long-term operation. Secondly, the coating process lacks targeted optimization; for example, resistance evaporation results in poor film uniformity, and electron beam evaporation fails to adequately control the film-substrate bonding strength. This makes it difficult for getter membranes to meet practical application requirements in ultra-high vacuum environments in terms of service life and reliability. Furthermore, the lack of design considerations for getter membrane regeneration further limits their adoption in ultra-high vacuum systems requiring long-term operation.

[0004] Therefore, there is an urgent need for a novel getter membrane coating structure and preparation device to solve the problems of limited adsorption performance of getter membrane materials, insufficient film performance due to defects in the coating process, and lack of regeneration design in existing technologies, so as to achieve ultra-high vacuum chambers at 10 -12 Long-term stable operation at the Pa level will drive technological development in related high-end fields. Utility Model Content

[0005] The purpose of this invention is to provide a gas-absorbing film coating structure and preparation device suitable for ultra-high vacuum cavities, so as to solve the problems mentioned in the background art.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a getter film coating structure suitable for ultra-high vacuum cavities, comprising a cavity substrate and a titanium-zirconium composite base film and a non-evaporable getter surface layer sequentially coated on the inner surface of the cavity substrate; the titanium-zirconium composite base film has a thickness of 500-800 nm, and the non-evaporable getter surface layer has a thickness of 100-200 nm.

[0007] Preferably, the cavity substrate is 304 stainless steel or oxygen-free copper.

[0008] A device for preparing a gas-seeking membrane suitable for an ultra-high vacuum cavity includes a main body, the main body including a shell, a circular hole on the top of the shell, a fixing hole on the outer surface of the circular hole, and a detachable component inside the circular hole, which can quickly disassemble the cavity substrate.

[0009] Preferably, the bottom of the housing is provided with a first placement chamber and a second placement chamber in sequence. The bottom of the second placement chamber is provided with a heating component for heating the metal material inside the second placement chamber. The bottom of the housing is provided with an inner cavity, and an electron gun is fixedly connected inside the inner cavity.

[0010] Preferably, the detachable mechanism includes a detachable component, the detachable component including a sealing plate, a sealing strip being adhered to the surface of the sealing plate, a sealing cylinder corresponding to the fixing hole being provided on the top of the sealing plate, an insertion block being provided at the bottom of the sealing plate, an insertion hole being provided in the middle of the sealing plate and the insertion block, and a plurality of slots located on the outer surface of the insertion hole being provided at the bottom of the insertion block, and a base material component being provided inside the slot.

[0011] Preferably, the substrate assembly includes a locking block, the bottom of which is integrally connected to the cavity substrate, a stud is provided at the top center of the cavity substrate, the stud is inserted into the insertion hole, a sealing ring is sleeved on the surface of the stud, and a nut is threaded onto the surface of the stud.

[0012] Preferably, a pipe is provided at the bottom of the housing, and the pipe is connected to the connecting pump.

[0013] Compared with the prior art, the beneficial effects of this utility model are: Comprehensive and durable adsorption performance to meet ultra-high vacuum requirements: Utilizing a dual-layer structure of "titanium-zirconium composite base film + non-evaporable getter surface layer," the titanium-zirconium composite base film (500-800nm) achieves efficient multi-gas capture thanks to titanium's strong adsorption of H2 and zirconium's high selectivity for CO and CH4. The non-evaporable getter surface layer (100-200nm) further enhances the adsorption capacity for residual gases. This dual-layer synergy ensures the cavity vacuum level is stably maintained at 10... -With an adsorption capacity on the order of ¹²Pa and an adsorption saturation period that is more than three times longer than that of a single-material getter membrane, it meets the long-term operational needs of fields such as semiconductor manufacturing and aerospace simulation.

[0014] Excellent film quality and strong film-substrate bonding: Relying on the coating method of electron gun and heating component working together, the electron gun precisely controls the evaporation rate, the heating component ensures uniform vaporization of metal materials, and the vacuum environment of the shell (connected pump to maintain low gas pressure in the cavity) makes the film thickness uniformity error ≤5%; At the same time, the titanium-zirconium composite base film has strong compatibility with 304 stainless steel / oxygen-free copper substrate, and the film-substrate bonding strength is improved by 40%, avoiding the risk of film peeling off under extremely high vacuum environment.

[0015] Easy and efficient assembly and disassembly, reducing operating costs: The detachable components are fixed by "slot positioning + stud fixing". The cavity base material is fixed by inserting the slot into the slot and the stud is inserted into the insertion hole and tightening the nut. When disassembling, simply loosen the nut to remove it. No complicated tools are required throughout the process. The assembly and disassembly efficiency is 2 times higher than the traditional fixing method. The double sealing design of sealing strip and sealing ring ensures that the shell still maintains high sealing performance after disassembly and assembly, avoiding damage from the vacuum environment. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the overall structure of this utility model; Figure 2 This is a side sectional view of the main body of the device of this utility model; Figure 3 This is a schematic diagram of the detachable mechanism structure of this utility model; Figure 4 This is a schematic diagram of the detachable component structure of this utility model; Figure 5 This is a schematic diagram of the substrate component structure of this utility model.

[0017] In the diagram: 1. Main body of the device; 11. Cavity; 12. Circular hole; 13. Fixing hole; 14. Inner cavity; 15. Electron gun; 16. First placement chamber; 17. Second placement chamber; 18. Heating component; 2. Detachable mechanism; 21. Detachable component; 211. Sealing plate; 212. Sealing cylinder; 213. Insertion block; 214. Slot; 215. Insertion hole; 22. Sealing strip; 23. Substrate assembly; 231. Stud; 232. Cavity substrate; 233. Locking block; 24. Nut; 25. Sealing ring. Detailed Implementation

[0018] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0019] In the description of this utility model, it should be noted that the terms "vertical", "up", "down", "horizontal", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0020] like Figure 1-5 As shown, this utility model provides a new technical solution, a getter film coating structure suitable for ultra-high vacuum cavities, including a cavity substrate 232 and a titanium-zirconium composite base film and a non-evaporable getter surface layer sequentially coated on the inner surface of the cavity substrate 232; the thickness of the titanium-zirconium composite base film is 500-800nm, and the thickness of the non-evaporable getter surface layer is 100-200nm.

[0021] The cavity substrate 232 is made of 304 stainless steel or oxygen-free copper.

[0022] A device for preparing a gas-absorbing membrane suitable for an ultra-high vacuum cavity includes a device body 1. The device body 1 includes a housing 11. A circular hole 12 is provided on the top of the housing 11. A fixing hole 13 is provided on the outer surface of the circular hole 12 on the top of the housing 11. A detachable component 21 is provided inside the circular hole 12, which can quickly disassemble the cavity substrate 232.

[0023] To prepare getter membranes, such as Figure 2 As shown, a first placement chamber 16 and a second placement chamber 17 are sequentially arranged at the bottom of the inner interior of the housing 11. The bottom of the second placement chamber 17 is provided with titanium and zirconium metal materials, and a heating component 18 is provided at the bottom of the second placement chamber 17. The heating component 18 is located inside the housing 11 and is used to heat the titanium and zirconium inside the second placement chamber 17. The heating component 18 is a mature existing technology, and its specific internal structure and working principle will not be described in detail here. An inner cavity 14 is provided at the bottom of the inner interior of the housing 11. An electron gun 15 is fixedly connected inside the inner cavity 14. The electron gun 15 is also a mature existing technology, and its specific internal structure and working principle will not be described in detail here.

[0024] To facilitate the disassembly of the cavity substrate 232, such as Figure 3-4As shown, the detachable mechanism 2 includes a detachable component 21, which includes a sealing plate 211 for sealing the sealing plate 211. The top of the sealing plate 211 is provided with a sealing cylinder 212 corresponding to the fixing hole 13, and the bottom of the sealing plate 211 is provided with an insertion block 213. The insertion block 213 is snapped into the round hole 12. An insertion hole 215 is provided between the sealing plate 211 and the insertion block 213. The bottom of the insertion block 213 is provided with a plurality of slots 214 located on the outer surface of the insertion hole 215. The substrate component 23 is provided inside the slot 214.

[0025] In order to fix the cavity substrate 232, such as Figure 3 and Figure 5 As shown, the substrate assembly 23 includes a locking block 233, which is snapped into the slot 214. The bottom of the locking block 233 is integrally connected to the cavity substrate 232. A stud 231 is provided at the top center of the cavity substrate 232. The stud 231 is inserted into the insertion hole 215. A sealing ring 25 is sleeved on the surface of the stud 231. The sealing ring 25 contacts the top of the housing 11. A nut 24 is threaded onto the surface of the stud 231. When it is necessary to fix the substrate assembly 23, the operator tightens the nut 24 with a tool.

[0026] In order to seal the sealing plate 211 to the top of the housing 11, a sealing strip 22 is adhered to the surface of the sealing plate 211.

[0027] In order to create a vacuum inside the housing 11, a pipe is provided at the bottom of the housing 11, and the pipe is connected to the connecting pump.

[0028] Working principle: Step S1: Pretreatment of cavity substrate 232: The inner surface of cavity substrate 232 is subjected to degreasing, pickling and vacuum baking in sequence; degreasing is performed by ultrasonic cleaning with ethanol-acetone mixed solution, pickling is performed by soaking in 5% dilute nitric acid solution, and vacuum baking is performed by heating the cavity substrate to 200-300℃ inside the vacuum baking oven and then keeping it at that temperature for 4 hours. Step S2, Installation of cavity substrate 232: Align the locking block 233 of cavity substrate 232 with the locking slot 214, fix cavity substrate 232 to the bottom of insertion block 213, tighten nut 24 on the surface of stud 231, insert insertion block 213 into round hole 12, insert fixing bolt inside sealing cylinder 212 and tighten, and finally insert plug at the top of sealing cylinder 212; Step S3: Preparation of titanium-zirconium composite substrate film: Titanium-zirconium composite substrate film is prepared by electron beam evaporation process, with electron beam power controlled at 1.5-2.0kW and evaporation rate at 5-8nm / s, so that the film thickness deviation is ≤5%; Step S4: Preparation of non-evaporable getter surface layer: The non-evaporable getter surface layer is prepared by magnetron sputtering, with the sputtering power adjusted to 300-400W and the argon pressure to 0.3-0.5Pa; Step S5: Intelligent control of process parameters: A real-time vacuum monitoring and online film thickness detection module is installed inside the cavity 11. During the coating process, when the vacuum level inside the cavity 11 is lower than 10... -6 The vapor deposition process automatically pauses when the vacuum level is reached (Pa) and restarts once the vacuum level is restored. Step S6: Getter membrane activation and regeneration design: An embedded nickel-chromium alloy heating component is set on the side wall of cavity 11. When the getter membrane is saturated with adsorption, the getter membrane is heated to 400-450℃ by the nickel-chromium alloy heating component and kept at this temperature for 2 hours to regenerate the getter. Step S7: Grinding of cavity substrate 232. After the air suction membrane is prepared, remove the detachable mechanism 2 and grind off the clip 233 and stud 231 with a grinder.

[0029] Electron beam evaporation process includes the following steps: Step S31: Connect the pump set and start it to create a vacuum environment inside the cavity 11; Step S32: Start the heating component 18 to transfer heat to the second placement chamber 17 through resistance heating. After the second placement chamber 17 absorbs heat, its temperature rises, thereby heating the metal material inside. Step S33: When the metal material is heated to a certain temperature, it will evaporate, forming evaporated metal atoms or molecules. These evaporated substances will move upward and eventually be deposited on the surface of the cavity substrate 232 located above, forming a thin film.

[0030] Step S34: Simultaneously, the electron gun 15 is activated, and the electron gun emits an electron beam. The electron beam is deflected under the magnetic field generated by the magnet and accurately bombards the metal material inside the second placement chamber 17. Step S35: The high energy of the electron beam rapidly heats the metal material to its evaporation temperature, causing it to evaporate and form an evaporated substance. This evaporated substance then moves toward the cavity substrate 232 and deposits on its surface, thereby forming the desired thin film.

[0031] The magnetron sputtering process includes the following steps: Step S41: Apply a DC or radio frequency electric field between the first placement chamber 16 and the cavity substrate 232 to ionize inert gases such as argon to generate plasma. Step S42, Ar ions formed after argon gas ionization + Under the action of an electric field, the material inside the first placement chamber 16 is bombarded at high speed, so that the atoms or molecules of the material gain enough energy to escape from the surface. Step S43: The escaped atoms or molecules fly in space and eventually deposit on the surface of the cavity substrate 232 to form a uniform thin film.

[0032] The getter film coating structure prepared through the above embodiments, after testing, can stably maintain the ultimate vacuum of the vacuum chamber at 10. -12 With a Pa level and a long service life of the getter membrane, it meets the long-term operation requirements of ultra-high vacuum systems.

[0033] In the description of this utility model, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0034] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A getter film coating structure suitable for ultra-high vacuum cavities, comprising a cavity substrate (232) and a titanium-zirconium composite base film and a non-evaporable getter surface layer sequentially coated on the inner surface of the cavity substrate (232), characterized in that: The thickness of the titanium-zirconium composite substrate film is 500-800 nm, and the thickness of the non-evaporable getter surface layer is 100-200 nm.

2. The gas-absorbing film coating structure suitable for ultra-high vacuum cavities according to claim 1, characterized in that: The cavity substrate (232) is 304 stainless steel or oxygen-free copper.

3. A device for preparing a gas-absorbing membrane suitable for ultra-high vacuum cavities, comprising a main body (1), characterized in that: The main body (1) of the device includes a housing (11), a round hole (12) is provided on the top of the housing (11), a fixing hole (13) is provided on the outer surface of the round hole (12) on the top of the housing (11), and a detachable component (21) is provided inside the round hole (12) so that the cavity substrate (232) can be quickly disassembled.

4. The apparatus for preparing a gas-absorbing membrane suitable for an ultra-high vacuum cavity according to claim 3, characterized in that: The bottom of the housing (11) is provided with a first placement chamber (16) and a second placement chamber (17) in sequence. The bottom of the second placement chamber (17) is provided with a heating component (18) for heating the metal material inside the second placement chamber (17). The bottom of the housing (11) is provided with an inner cavity (14), and an electron gun (15) is fixedly connected inside the inner cavity (14).

5. The apparatus for preparing a gas-absorbing membrane suitable for an ultra-high vacuum cavity according to claim 3, characterized in that: The detachable mechanism (2) includes a detachable component (21), which includes a sealing plate (211). A sealing strip (22) is bonded to the surface of the sealing plate (211). A sealing cylinder (212) corresponding to the fixing hole (13) is provided on the top of the sealing plate (211). An insertion block (213) is provided at the bottom of the sealing plate (211). An insertion hole (215) is provided in the middle of the sealing plate (211) and the insertion block (213). A plurality of slots (214) located on the outer surface of the insertion hole (215) are provided at the bottom of the insertion block (213). A substrate component (23) is provided inside the slot (214).

6. The apparatus for preparing a gas-seeking membrane suitable for an ultra-high vacuum cavity according to claim 5, characterized in that: The substrate assembly (23) includes a locking block (233), the bottom of which is integrally connected to the cavity substrate (232). A stud (231) is provided at the top center of the cavity substrate (232). The stud (231) is inserted into the insertion hole (215). A sealing ring (25) is fitted on the surface of the stud (231). A nut (24) is threaded onto the surface of the stud (231).

7. The apparatus for preparing a gas-absorbing membrane suitable for an ultra-high vacuum cavity according to claim 3, characterized in that: The bottom of the housing (11) is provided with a pipe, which is connected to the connecting pump.

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