Method and device for plating non-evaporable getter films in pipeline with high length-diameter ratio and small aperture in batches
By designing batch coating devices and optimization processes, the difficulty of centering target materials in vacuum chambers with high aspect ratio and small pore diameters is solved, and the problem of background vacuum difference is achieved, efficient and stable batch preparation of non-evaporative getter films is achieved, improving the stability of the vacuum environment and film quality.
Patent Information
- Application Number
- CN202510666074.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-22
- Publication Date
- 2025-08-12
AI Technical Summary
In a vacuum chamber with small pore diameters with high aspect ratio, the traditional non-evaporative getter film coating process has problems such as difficulty in centering the target material, poor background vacuum, film uniformity and inefficiency, and it is difficult to meet the needs of batch preparation.
A batch coating device including the upper cavity and the lower cavity is designed, using concentric tube assembly and solenoid structure, combining radio frequency magnetron sputtering and DC magnetron sputtering technology to optimize cleaning, installation, leakage detection and air extraction and baking processes to realize multi-station batch coating.
It improves the quality and performance of the film, ensures stable coating in a vacuum chamber with a high aspect ratio, improves production efficiency, and reduces the risk of residual gases to the film, and is suitable for particle accelerators and other high vacuum environment fields.
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Figure CN120464974A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of particle accelerator and vacuum technology, and in particular to a method and device for batch coating non-evaporable getter films in a small-aperture pipeline with a high aspect ratio. Background Art
[0002] Synchrotron radiation sources, as advanced scientific research tools, have undergone several generations of development since the mid-20th century. Entering the 21st century, the pre-research and construction of fourth-generation synchrotron radiation sources has become a hot topic in the international particle accelerator community. These include MAX IV in Sweden, Sirius in Brazil, the European Synchrotron Radiation Source (ESRF) EBS, the Advanced Photon Source (APS U) in the United States, and the High Energy Synchrotron Radiation Source (HEPS) in China. Their design and construction aims to produce synchrotron radiation with ultra-low beam emittance, higher brightness, and enhanced spatial coherence to contribute to national economic development and cutting-edge scientific research. In the design of fourth-generation synchrotron radiation sources, the aperture of the quadrupole iron magnet is designed to be smaller to generate a high-gradient focusing magnetic field, which significantly limits the lateral dimensions of the vacuum chamber. Due to the conductance limitations and insufficient installation space of the small-aperture vacuum chamber, coupled with the increased dynamic air load caused by surface outgassing caused by synchrotron radiation and high-energy particle bombardment, traditional centralized vacuum pumping solutions are unable to maintain the vacuum environment required for normal accelerator operation. Therefore, the development of new and efficient ultra-high vacuum generation technologies is urgently needed.
[0003] Distributed pumping technologies (such as non-evaporable getter (NEG) films) have become a key solution to these problems. Activated NEG films exhibit distributed pumping capabilities unrestricted by conductance, along with very low photoinduced desorption yield (PSD), electroinduced desorption yield (ESD), and secondary electron yield (SEY). These films are becoming a key technology for addressing conductance limitations in small-aperture vacuum chambers, effectively improving the vacuum distribution within the storage ring and achieving the ultra-high vacuum environment required for its normal operation. Among various NEG material systems, TiZrV alloy films dominate accelerator vacuum systems due to their low activation temperature (full activation after 24 hours at 180°C). With the development of large-scale vacuum systems, the number of required coating vacuum chambers continues to increase. This places higher demands on the fabrication of NEG films, including improving quality and performance while maintaining efficiency in batch production, a significant challenge.
[0004] As the length of small-aperture vacuum chambers increases, coating processes and technologies within high-aspect-ratio small-aperture vacuum chambers face numerous challenges, such as difficulty centering the target, poor background vacuum, and reduced film uniformity. Considering the demands of batch coating, new technical contradictions have gradually emerged during the upgrade from traditional single-station coating systems to multi-station batch coating systems: as the number of vacuum components increases, the original vacuum acquisition scheme struggles to meet the background vacuum required for coating; the traditional straight-segment electrode structure cannot adapt to a multi-station layout, requiring redesign and optimization of the electrode configuration. Therefore, there is an urgent need to achieve efficient and uniform preparation of non-evaporable getter films through the coordinated optimization of process parameters and equipment structure.
[0005] Currently, the magnetron sputtering coating process for non-evaporable getter films faces the following major technical bottlenecks: First, the use of twisted wire as a sputtering target results in variations in the sputtering yields of Ti, Zr, and V, leading to deviations from the designed film composition. Furthermore, the linear deposition characteristics of magnetron sputtering result in uneven distribution of the film's chemical composition, directly impacting the film's performance consistency. Second, the coating system's poor background vacuum severely restricts the performance and use of non-evaporable getter films. Furthermore, during the initial stages of magnetron sputtering, the plasma discharge is unstable, prone to sparking, and further deteriorates film quality. Summary of the Invention
[0006] The object of the present invention is to overcome the above-mentioned drawbacks and provide a device for batch coating non-evaporable getter films in small-diameter pipes with high aspect ratio.
[0007] To achieve the above-mentioned purpose, the present invention adopts the following technical scheme: comprising an upper cavity and a lower cavity which are concentrically arranged and both are sealed structures, a tube assembly is provided between the upper cavity and the lower cavity to connect the two, the upper cavity is connected to a first sputtering ion pump, a first thin film vacuum gauge, a first cold cathode ionization vacuum gauge, a first all-metal angle valve and an observation window; the lower cavity is connected to a second sputtering ion pump, a second thin film vacuum gauge, a second cold cathode ionization vacuum gauge, a second all-metal angle valve and an all-metal micro-leak valve, the first all-metal angle valve and the second all-metal angle valve are connected to the molecular ion pump through an upper bellows and a lower bellows respectively. The pump unit is connected, the all-metal micro-leakage valve is connected to the air source through a stainless steel air pipe, and the lower cavity is placed on the ground through a supporting foot; the pipe assembly is evenly arranged in at least four groups along the circumference, and each group of the pipe assembly includes an upper transition bellows, an electrode, an upper transition pipe, a pipe to be coated, a lower transition pipe and a lower transition bellows that are sequentially connected from top to bottom; the electrode threaded rod inside the electrode is connected to the upper end of the titanium-zirconium-vanadium alloy target through a connector, the lower end of the titanium-zirconium-vanadium alloy target is a cantilevered end, and the titanium-zirconium-vanadium alloy target passes through the upper transition pipe, the pipe to be coated, the lower transition pipe and the lower transition bellows in sequence; It also includes a solenoid located between the upper cavity and the lower cavity and sleeved on the tube assembly, a gap is left between the inner wall of the solenoid and the tube assembly, and the solenoid is concentric with the upper cavity, and the solenoid is fixed to the ground through a support frame.
[0008] The support frame includes a frame body with an overall trapezoidal structure, a top plate fixed to the top of the frame body, and a support plate located inside the frame body, wherein: a through hole for the solenoid to pass through is opened at the center of the top plate, the support plate is an annular structure, and the support plate and the top of the frame body are connected by a threaded rod, the bottom of the solenoid is placed on the support plate, and the bottom of the upper cavity rests on the top of the solenoid through a support assembly; the support assembly is evenly distributed in four groups along the circumference of the solenoid, each group of support assemblies includes a support base and two columns, the support base is an overall arc-shaped bent structure, including an arc plate arranged in the horizontal direction and an arc baffle folded downward along the inner arc surface of the arc plate, the arc plate is mounted on the upper surface of the solenoid, and the arc baffle is attached to the inner wall of the solenoid; the upper and lower ends of the two columns are respectively fixed to the bottom of the upper cavity and the upper plate surface of the arc plate.
[0009] The four groups of pipe assemblies are connected by a fixing device, which includes a fixing column arranged in a vertical direction, and the two ends of the fixing column are respectively connected to the bottom surface of the upper cavity and the fixed base, and the fixing base is disc-shaped and located at the center of the inner circle of the support plate. The fixing base is provided with a U-shaped hole for the pipe assembly to pass through, and the fixing base is fixed to the flange welding block on the lower transition pipe; the fixing device also includes a positioning plate mounted on the fixing column, and the positioning plate is a cross-shaped structure, and a central positioning hole matching the fixing column is provided at the center thereof, and its four ends are respectively provided with pipe positioning holes for the four groups of pipe assemblies to pass through, and the positioning plates are arranged in two groups along the up and down directions, and the two groups of positioning plates are respectively connected to the upper transition pipe and the lower transition pipe of the pipe assembly through right-angle connectors.
[0010] The electrode comprises a vacuum chamber, an electrode threaded rod, an electrode conductive part, a conductive welding part and a high-voltage electrode head; the vacuum chamber is in a three-way shape as a whole, and is connected by a vertical cavity and a horizontal cavity, wherein: the two ends of the vertical cavity are respectively connected to the upper transition bellows and the upper transition pipe, and the horizontal cavity is connected to the high-voltage electrode head; the electrode threaded tube is located in the vertical cavity and is concentrically arranged with the vertical cavity, the upper end of the electrode threaded rod is connected to the flange structure at the upper end of the vertical cavity through a nut and a gasket, and the lower end of the electrode threaded tube is threadedly connected to the connector; The electrode conduction rod is sleeved on the electrode threaded tube and threadedly connected to the electrode threaded tube. The electrode conduction rod has an inverted T-shaped structure as a whole, consisting of a columnar body and a circular base. The conductive welding part includes a rod body section, which is located in the horizontal cavity and concentrically arranged with the horizontal cavity. One end of the rod body section is provided with a cylindrical section perpendicular to it, and the cylindrical section is sleeved on the columnar body of the electrode conduction rod, and the other end of the rod body section is threadedly matched with the electrode rod in the high-voltage electrode head. The rod body section and the electrode threaded tube of the conductive welding part are both sleeved with a ceramic tube.
[0011] The upper transition bellows, electrode, upper transition pipe, pipe to be coated, lower transition pipe, and connection ends of the lower transition bellows are all flange structures. The upper transition bellows is connected to the CF vacuum flange at the bottom of the upper cavity, and the lower transition bellows is connected to the CF vacuum flange at the top of the lower cavity. The L / D of the pipeline to be coated is ≥20; the nominal pumping speed of the first sputtering ion pump is 100 L / s, and the nominal pumping speed of the second sputtering ion pump is 200 L / s.
[0012] Another object of the present invention is to provide a method for batch coating non-evaporable getter films in small-diameter pipes with high aspect ratios, comprising the following steps: S1: Cleaning the pipe to be coated; S2: connecting the upper transition bellows, the electrode, the upper transition pipe, the cleaned pipe to be coated, the lower transition pipe and the lower transition bellows in sequence to form a pipe assembly; S3: Install the tube assembly between the upper cavity and the lower cavity to complete the assembly of the coating device; S4: Connect the helium mass spectrometer leak detector to the lower bellows to perform a leak test on the coating device. When the leak rate is less than the set value, remove the helium mass spectrometer leak detector. S5: Connect the upper bellows and the lower bellows to the molecular pump unit at the same time to perform vacuuming until the vacuum degree at the pump port of the molecular pump unit reaches the set value; S6: baking and keeping the tube assembly, the upper cavity, the lower cavity, the first sputtering ion pump, and the second sputtering ion pump warm; S7: While S6 is baking and keeping warm, the first sputtering ion pump and the second sputtering ion pump are bombarded by a high-voltage power supply to perform a degassing treatment. The bombardment mode is "flash". When the upper cavity, the lower cavity and the tube assembly begin to cool down, the baking of the first sputtering ion pump and the second sputtering ion pump is stopped, the first all-metal angle valve and the second all-metal angle valve are closed to isolate the molecular pump unit, and the first sputtering ion pump and the second sputtering ion pump are started to evacuate the film coating device to a limit vacuum of ≤5E-8 Pa. S8: Radio frequency magnetron cleaning of the coating pipe and titanium zirconium vanadium alloy target; S9: Use DC magnetron sputtering to coat the pipe to be coated.
[0013] In the above-mentioned S1, the cleaning comprises the following steps: S1.1: First, place the pipe to be coated in the cleaning solution and clean its inner and outer surfaces with a dust-free cloth to remove surface impurities and oxide layers. Then, rinse the remaining cleaning solution on the pipe to be coated with running deionized water. S1.2: Transfer the pipe to be coated into the passivation solution for passivation, and then rinse the residual passivation solution on the pipe with running deionized water; S1.3: Use flowing compressed nitrogen to dry the inner and outer surfaces of the pipe to be coated; S1.4: Perform a visual inspection to ensure that there are no obvious stains, water spots, or scratches on the inner surface of the pipe to be coated.
[0014] In S1.1, the cleaning solution is a 10-15% concentration of copper acid cleaning solution and deionized water, and the cleaning time is 15-20 minutes; in S1.2, the passivation solution is a 5% concentration of ammonium citrate and deionized water, and the passivation time is 15 minutes; in S1.3, the pressure of the flowing compressed nitrogen is 0.5 MPa.
[0015] In S6, the pipe to be coated in the pipe assembly is baked at 180°C and kept warm for 24 hours; the remaining components, the upper cavity and the lower cavity in the pipe assembly are baked at 180-200°C and kept warm for 24 hours; the pipe assembly, the upper cavity and the lower cavity are baked by wrapping a heating tape around the corresponding components and wrapping them with aluminum foil, and heating and baking them by connecting the heating tape to a power supply; the first sputtering ion pump and the second sputtering ion pump are baked by wrapping aluminum foil around the corresponding components, and baking them by directly plugging the first sputtering ion pump and the second sputtering ion pump into a 220V power supply; temperature sensors are placed on the pipe assembly, the upper cavity and the lower cavity for temperature measurement feedback.
[0016] In the above-mentioned S8, after the coating device reaches the ultimate vacuum, the first sputtering ion pump and the second sputtering ion pump are turned off, and the second all-metal angle valve is opened to allow the molecular pump unit to evacuate the vacuum, and the first thin film vacuum gauge and the second thin film vacuum gauge are started at the same time; then the all-metal micro-leak valve is opened to allow the sputtering gas to pass through, and current is applied to the solenoid to generate a magnetic field; then the electrode is connected to the RF power supply, and the high-voltage alternating electric field generated by the RF power supply and the magnetic field generated by the solenoid jointly generate plasma, and the plasma reacts or collides with the residual micro-particle pollutants or metal oxide layer in the pipe to be coated to form volatile substances, and finally these volatile substances are extracted by the molecular pump unit to achieve the cleaning of the pipe to be coated and the titanium-zirconium-vanadium alloy target material; in the above-mentioned S9, the RF power supply is first disconnected, and the electrode is connected to the DC power supply to ionize the gas to carry out the coating process.
[0017] The beneficial technical effects of the present invention are: 1. The present invention makes the thin film deposition process more efficient and stable by optimizing the process flow of cleaning, installation, leak detection and exhaust, baking, radio frequency cleaning and DC magnetron sputtering, and adjusting the coating parameters (magnetic field strength, gas pressure, sputtering current, etc.).
[0018] 2. This invention has designed a dedicated batch coating apparatus that fully considers ease of operation, economical maintenance, and the required film performance. The rational layout and precise coordination of the various components within the apparatus enable simultaneous coating of multiple pipes, effectively improving production efficiency. Furthermore, the apparatus's high vacuum environment and stable sputtering conditions help ensure consistent film thickness and uniformity, thereby guaranteeing film quality and performance. Through the aforementioned process optimization, coating parameter adjustment, and apparatus construction, the goal of stably coating non-evaporable getter films on the inner walls of high aspect ratio, small aperture (L / D ≥ 20) vacuum chambers has been achieved.
[0019] 3. This invention is not only applicable to particle accelerators but also has broad application in other high-vacuum environments, such as vacuum technology. In particle accelerators, non-evaporable getter films can effectively reduce the dynamic air load within the vacuum chamber, improve vacuum distribution, and thus enhance the accelerator's operational stability and beam quality.
[0020] 4. This invention introduces an RF pre-sputtering stage prior to the actual magnetron sputtering coating process, leveraging the self-bias effect created by the RF electric field to achieve dual cleaning functions. Firstly, the RF electric field creates a self-bias (negative potential) on the target surface, accelerating ions to bombard the target, effectively removing oxides and impurities from the target surface and reducing sparking during magnetron sputtering. Secondly, the sputtered atoms possess higher energy, enabling initial in-situ cleaning of the inner wall of the pipe, removing residual surface gas molecules and other substances, thus providing excellent preconditions for actual thin film deposition.
[0021] 5. Based on a precise analysis of the magnetic field distribution within a large-diameter solenoid, this invention optimizes the spatial arrangement of multiple working chambers and matches the magnetic field intensity distribution, thereby addressing the existing problem of poor coating quality stability and consistency caused by uneven magnetic fields during multi-cavity simultaneous coating. By designing and constructing a "multi-cavity parallel" batch coating system, perfectly compatible with the coating method proposed in this invention, it solves the problems of difficult target centering, poor background vacuum, and low efficiency associated with batch coating of non-evaporable getter films within a high-aspect-ratio, small-aperture vacuum chamber.
[0022] 6. The present invention improves the quality and performance of non-evaporable getter films while increasing the efficiency of batch preparation, and provides a stable and efficient batch coating device, which is of great significance for large-scale batch coating on the inner wall of slender pipes.
[0023] 7. This invention fundamentally solves the problem of uneven film composition by employing a titanium-zirconium-vanadium alloy target. Simultaneously, through process improvements and coating device design, a background vacuum better than 5E-8 Pa is achieved, an improvement of 1 to 2 orders of magnitude compared to conventional devices, significantly reducing the risk of residual gas contamination of the film. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 This is a schematic diagram of the structure of the present invention Figure 1 .
[0025] Figure 2 This is a schematic diagram of the structure of the present invention Figure 2 .
[0026] Figure 3 It is a schematic structural diagram of the present invention after the solenoid is removed.
[0027] Figure 4 This is a schematic diagram of the structure of the upper cavity of the present invention Figure 1 .
[0028] Figure 5 This is a schematic diagram of the structure of the upper cavity of the present invention Figure 2 .
[0029] Figure 6 This is a schematic diagram of the structure of the lower cavity of the present invention Figure 1 .
[0030] Figure 7 This is a schematic diagram of the structure of the lower cavity of the present invention Figure 2 .
[0031] Figure 8 It is a structural schematic diagram of the support frame of the present invention.
[0032] Figure 9 It is a structural schematic diagram of the support assembly of the present invention.
[0033] Figure 10 It is a schematic diagram of the connection structure of the electrode and the target material of the present invention.
[0034] Figure 11 It is a cross-sectional view of the connection between the electrode and the target material of the present invention.
[0035] Figure 12 It is a schematic diagram of the exploded structure of the electrode and target material of the present invention.
[0036] Figure 13 Schematic diagram of the structure of the pipe assembly of the present invention.
[0037] Figure 14 It is a schematic diagram of the connection between the pipe assembly and the fixed column of the present invention.
[0038] Figure 15 This is the test result of the getter performance of the non-evaporable getter film of Example 1 of the present invention.
[0039] Figure 16 Surface image a and cross-sectional microstructure feature image b of the non-evaporable getter film of Example 1 of the present invention.
[0040] The symbols in the above drawings are: upper chamber 1, first sputtering ion pump 11, first thin film vacuum gauge 12, first cold cathode ionization vacuum gauge 13, observation window 14, support base 15, arc plate 151, arc baffle 152, two columns 16, lower chamber 2, second sputtering ion pump 21, second thin film vacuum gauge 22, second cold cathode ionization vacuum gauge 23, second all-metal angle valve 24, support foot 25, upper transition bellows 3A, lower transition bellows 3B, electrode 4, vacuum chamber 41, vertical chamber 411, horizontal chamber 412, electrode threaded rod 42, nut 421, Gasket 422, electrode conductor 43, columnar body 431, circular chassis 432, conductive welding part 44, rod section 441, cylindrical section 442, high-voltage electrode head 45, electrode rod 451, connecting head 46, first ceramic tube 47, upper ceramic tube 481, middle ceramic tube 482, lower ceramic tube 483, upper transition tube 5A, lower transition tube 5B, flange welding block 51, pipe to be coated 6, titanium-zirconium-vanadium alloy target 7, solenoid 8, frame body 81, top plate 82, support plate 83, threaded rod 84, fixed column 9, fixed base 91, positioning plate 92, right-angle connector 93. DETAILED DESCRIPTION
[0041] The present invention will be further described below with reference to the accompanying drawings: like Figure 1 、 Figure 2 、 Figure 3The device shown is for batch coating non-evaporable getter films in small-diameter pipes with a high aspect ratio. It includes an upper cavity 1 and a lower cavity 2, which are concentrically arranged and both have a sealed structure. A tube assembly is provided between the upper cavity 1 and the lower cavity 2 to connect the two. The device also includes a solenoid 8 located between the upper cavity 1 and the lower cavity 2 and sleeved on the tube assembly. A gap is left between the inner wall of the solenoid 8 and the tube assembly. The solenoid 8 is concentric with the upper cavity 1 and is fixed to the ground by a support frame.
[0042] Further, such as Figure 4 、 Figure 5 As shown, the upper chamber 1 is connected to a first sputtering ion pump 11, a first thin film vacuum gauge 12, a first cold cathode ionization vacuum gauge 13, a first all-metal angle valve and an observation window 14, wherein: the first sputtering ion pump 11 is sealed with the CF100 vacuum flange on the top surface of the upper chamber 1, and four groups of observation windows 14 are provided. The four groups of observation windows 14 are respectively sealed with the CF35 vacuum flange on the top surface of the upper chamber 1, the first thin film vacuum gauge 12, the first cold cathode ionization vacuum gauge 13 and the first all-metal angle valve are respectively sealed with the three groups of CF35 vacuum flanges on the side wall of the upper chamber 1, and the bottom surface of the upper chamber 1 is further provided with four groups of CF35 vacuum flanges for sealing with the upper transition bellows 3A in the pipe assembly.
[0043] like Figure 6 、 Figure 7 As shown, the lower chamber 2 is connected to a second sputtering ion pump 21, a second thin-film vacuum gauge 22, a second cold cathode ionization vacuum gauge 23, a second all-metal angle valve 24, and an all-metal micro-leakage valve. Four sets of CF35 vacuum flanges are provided on the top surface of the lower chamber 2 for sealing connection with the lower transition bellows 3B in the tube assembly. The second sputtering ion pump 21 is sealed to a CF150 vacuum flange on the side wall of the lower chamber 2. The second thin-film vacuum gauge 22, the second cold cathode ionization vacuum gauge 23, the second all-metal angle valve 24, and the all-metal micro-leakage valve are each sealed to the four sets of CF35 vacuum flanges on the side wall of the lower chamber 2. The lower chamber 2 is placed on the ground via support legs 25.
[0044] In this embodiment, the first all-metal angle valve and the second all-metal angle valve 24 are connected to the molecular pump unit via an upper bellows and a lower bellows, respectively. The all-metal micro-leakage valve is connected to the gas source via a stainless steel air pipe, where the gas source is krypton or argon. The nominal pumping speed of the first sputtering ion pump 11 is 100 L / s, and the nominal pumping speed of the second sputtering ion pump 21 is 200 L / s. It should be noted that the first all-metal angle valve, the all-metal micro-leakage valve, the upper bellows, the lower bellows, the molecular pump, and the stainless steel air pipe are not shown in the drawings of this application.
[0045] Further, such as Figure 13As shown, at least four groups of tube assemblies are evenly arranged along the circumference, and each group of tube assemblies includes an upper transition bellows 3A, an electrode 4, an upper transition tube 5A, a pipe to be coated 6, a lower transition tube 5B, and a lower transition bellows 3B, which are connected in sequence from top to bottom. The electrode threaded rod 42 inside the electrode 4 is connected to the upper end of the titanium-zirconium-vanadium alloy target 7 via a connector 46. The lower end of the titanium-zirconium-vanadium alloy target 7 is an overhanging end, and the titanium-zirconium-vanadium alloy target 7 passes through the upper transition tube 5A, the pipe to be coated 6, the lower transition tube 5B, and the lower transition bellows 3B in sequence. In this embodiment, the connection ends of the upper transition bellows 3A, the electrode 4, the upper transition tube 5A, the pipe to be coated 6, the lower transition tube 5B, and the lower transition bellows 3B are all flange structures. The upper transition bellows 3A is connected to the CF35 vacuum flange at the bottom of the upper chamber 1, and the lower transition bellows 3B is connected to the CF35 vacuum flange at the top of the lower chamber 2. In this embodiment, the L / D of the pipe to be coated 6 is ≥20.
[0046] The four sets of pipe assemblies are connected by fixing devices, specifically, Figure 14 As shown, the fixing device includes a fixing column 9 arranged in a vertical direction, and the two ends of the fixing column 9 are respectively connected to the bottom surface of the upper cavity 1 and the fixing base 91. The fixing base 91 is disc-shaped and is located at the center of the inner circle of the support plate 83. The fixing base 91 is provided with a U-shaped hole for the pipe assembly to pass through, and the fixing base 91 is fixed to the flange welding block 51 on the lower transition pipe 5B; the fixing device also includes a positioning plate 92 mounted on the fixing column 9, and the positioning plate 92 is a cross-shaped structure. The center of the positioning plate 92 is provided with a central positioning hole that matches the fixing column 9, and the four ends thereof are respectively provided with pipe positioning holes for four groups of pipe assemblies to pass through. Two groups of positioning plates 92 are arranged in the up and down directions, and the two groups of positioning plates 92 are respectively connected to the upper transition pipe 5A and the lower transition pipe 5B of the pipe assembly through right-angle connectors 93.
[0047] Further, such as Figure 8 As shown, the support frame includes a frame body 81 with an overall trapezoidal structure, a top plate 82 fixed to the top of the frame body 81, and a support plate 83 located inside the frame body 81, wherein: a through hole for the solenoid 8 to pass through is opened at the center of the top plate 82, the support plate 83 is an annular structure, and the support plate 83 and the top of the frame body 81 are connected by a threaded rod 84, the bottom of the solenoid 8 is placed on the support plate 83, and the bottom of the upper cavity 1 is against the top of the solenoid 8 through the support assembly.
[0048] like Figure 9As shown, there are four groups of support components evenly distributed along the circumference of the solenoid 8, and each group of support components includes a support base 15 and two columns 16. The support base 15 is an overall arc-shaped bent structure, including a horizontally arranged arc plate 151 and an arc-shaped baffle 152 folded downward along the inner arc surface of the arc plate 151. The arc plate 151 is mounted on the upper surface of the solenoid 8, and the arc-shaped baffle 152 is attached to the inner wall of the solenoid 8; the upper and lower ends of the two columns 16 are respectively fixed to the bottom of the upper cavity 1 and the upper plate surface of the arc plate 151.
[0049] Further, such as Figure 10 、 Figure 11 、 Figure 12 As shown, the electrode 4 includes a vacuum chamber 41, an electrode threaded rod 42, an electrode conductive member 43, a conductive welding member 44, and a high-voltage electrode head 45. The vacuum chamber 41 is generally tee-shaped, consisting of a vertical cavity 411 and a horizontal cavity 412. The two ends of the vertical cavity 411 are respectively connected to the upper transition bellows 3A and the upper transition tube 5A, and the horizontal cavity 412 is connected to the high-voltage electrode head 45.
[0050] The electrode threaded tube 42 is located in the vertical cavity 411 and is concentrically arranged with the vertical cavity 411. The upper end of the electrode threaded rod 42 is connected to the flange structure at the upper end of the vertical cavity 411 through a nut 421 and a gasket 422. The lower end of the electrode threaded tube 42 is threadedly connected to the connector 46.
[0051] The electrode conductive member 43 is sleeved on the electrode threaded tube 42 and is threadedly connected to the electrode threaded tube 42 . The electrode conductive member 43 is an inverted T-shaped structure as a whole, and consists of a columnar body 431 and a circular base 432 .
[0052] The conductive welding part 44 includes a rod body segment 441, which is located in the horizontal cavity 412 and is concentrically arranged with the horizontal cavity 412. One end of the rod body segment 441 is provided with a cylindrical segment 442 perpendicular to it, and the cylindrical segment 442 is sleeved on the columnar body 431 of the electrode conductive part 43. The other end of the rod body segment 441 is threadedly engaged with the electrode rod 451 in the high-voltage electrode head 45.
[0053] Ceramic tubes are sheathed around the rod section 441 of the conductive welding member 44 and the electrode threaded tube 42. Specifically, the rod section 441 is sheathed with a first ceramic tube 47, while the ceramic tube sheathed around the threaded tube 42 is a split structure consisting of an upper ceramic tube 481, a middle ceramic tube 482, and a lower ceramic tube 483. These three tubes are fastened together by a nut 421 and the electrode conductive rod 43.
[0054] The present invention also provides a method for batch coating a non-evaporable getter film in a small-aperture pipe with a high aspect ratio, comprising the following steps: S1: Cleaning the pipe to be coated; S2: connecting the upper transition bellows, the electrode, the upper transition pipe, the cleaned pipe to be coated, the lower transition pipe and the lower transition bellows in sequence to form a pipe assembly; S3: Install the tube assembly between the upper cavity and the lower cavity to complete the assembly of the coating device; S4: Connect the helium mass spectrometer leak detector to the lower bellows to perform a leak test on the coating device. When the leak rate is less than the set value, remove the helium mass spectrometer leak detector. S5: Connect the upper bellows and the lower bellows to the molecular pump unit at the same time to perform vacuuming until the vacuum degree at the pump port of the molecular pump unit reaches the set value; S6: baking and keeping the tube assembly, the upper cavity, the lower cavity, the first sputtering ion pump, and the second sputtering ion pump warm; S7: While S6 is baking and keeping warm, the first sputtering ion pump and the second sputtering ion pump are bombarded by a high-voltage power supply to perform a degassing treatment. The bombardment mode is "flash". When the upper cavity, the lower cavity and the tube assembly begin to cool down, the baking of the first sputtering ion pump and the second sputtering ion pump is stopped, the first all-metal angle valve and the second all-metal angle valve are closed to isolate the molecular pump unit, and the first sputtering ion pump and the second sputtering ion pump are started to evacuate the film coating device to a limit vacuum of ≤5E-8 Pa. S8: Radio frequency magnetron cleaning of the coating pipe and titanium zirconium vanadium alloy target; S9: Use DC magnetron sputtering to coat the pipe to be coated.
[0055] Furthermore, in S1, cleaning includes the following steps: S1.1: First, place the pipe to be coated in the cleaning solution and clean its inner and outer surfaces with a dust-free cloth to remove surface impurities and oxide layers. Then, rinse the remaining cleaning solution on the pipe to be coated with running deionized water. S1.2: Transfer the pipe to be coated into the passivation solution for passivation, and then rinse the residual passivation solution on the pipe with running deionized water; S1.3: Use flowing compressed nitrogen to dry the inner and outer surfaces of the pipe to be coated; S1.4: Perform a visual inspection to ensure that there are no obvious stains, water spots, or scratches on the inner surface of the pipe to be coated.
[0056] Furthermore, in S1.1, the cleaning solution is a 10-15% concentration of copper acid cleaning solution and deionized water, and the cleaning time is 15-20 minutes; in S1.2, the passivation solution is a 5% concentration of ammonium citrate and deionized water, and the passivation time is 15 minutes; in S1.3, the pressure of the flowing compressed nitrogen is 0.5 MPa.
[0057] Furthermore, in S6, the pipe to be coated in the pipe assembly is baked at 180°C and kept warm for 24 hours; the remaining components, the upper cavity and the lower cavity in the pipe assembly are baked at 180-200°C and kept warm for 24 hours; the baking method for the pipe assembly, the upper cavity and the lower cavity is to wrap a heating tape around the corresponding components and wrap aluminum foil, and heat and bake the heating tape through a power supply; the baking method for the first sputtering ion pump and the second sputtering ion pump is to wrap aluminum foil around the corresponding components, and bake them by directly plugging the first sputtering ion pump and the second sputtering ion pump into a 220V power supply; temperature sensors are placed on the pipe assembly, the upper cavity and the lower cavity for temperature measurement feedback.
[0058] Furthermore, in S8, after the coating device reaches the ultimate vacuum, the first sputtering ion pump and the second sputtering ion pump are turned off, the second all-metal angle valve is opened to allow the molecular pump unit to evacuate, and the first thin film vacuum gauge and the second thin film vacuum gauge are opened at the same time; then the all-metal micro-leak valve is opened to allow the sputtering gas to pass through, and current is applied to the solenoid to generate a magnetic field; then the electrode is connected to the RF power supply, and the high-voltage alternating electric field generated by the RF power supply and the magnetic field generated by the solenoid jointly generate plasma, and the plasma reacts or collides with the residual micro-particle pollutants or metal oxide layer in the pipe to be coated to form volatile substances, and finally these volatile substances are extracted by the molecular pump unit to achieve the cleaning of the pipe to be coated and the titanium-zirconium-vanadium alloy target material; in the above-mentioned S9, the RF power supply is first disconnected, the electrode is connected to the DC power supply, and the gas is ionized to carry out the coating process.
[0059] A more specific description is as follows: First, the pipes to be coated are pre-cleaned. Four groups of pipes to be coated are placed in a 10-15% concentration of a cleaning solution composed of copper acid cleaning solution and deionized water. The inner and outer surfaces of the pipes to be coated are cleaned with a dust-free cloth to remove surface impurities and oxide layers. After 15-20 minutes of cleaning, the remaining cleaning solution on the pipes to be coated is rinsed off with running deionized water. The pipes to be coated are then transferred to a 5% passivation solution composed of ammonium citrate and deionized water for passivation for 15 minutes. The remaining passivation solution is rinsed off again with running deionized water. The inner and outer surfaces of the pipes to be coated are then blown dry with flowing compressed nitrogen (at a pressure of approximately 0.5 MPa). After cleaning, a visual inspection is performed to ensure that the inner surfaces of the pipes to be coated are free of obvious stains, water marks, and scratches.
[0060] Next, the upper transition bellows, electrodes, upper transition tube, cleaned pipe to be coated, lower transition tube, and lower transition bellows are sequentially connected to form a tube assembly. The upper and lower transition bellows are then connected to the upper and lower chambers, respectively, completing the assembly of the entire device. Each component is connected via CF vacuum flanges.
[0061] Next, connect the lower bellows to the helium mass spectrometer leak detector and perform a leak test on the flange connection and weld of the coating device. When the leak rate is less than the set value, remove the helium mass spectrometer leak detector and connect the upper and lower bellows to the molecular pump unit at the same time for vacuum treatment until the vacuum degree of the pump port of the molecular pump unit reaches the set value.
[0062] Next, the pipe to be coated is baked at 180°C and held at this temperature for 24 hours. Simultaneously, the remaining components of the pipe assembly, the upper chamber, and the lower chamber are baked at 180-200°C and held at this temperature for 24 hours. The first and second sputtering ion pumps are also baked. The pipe assembly, upper chamber, and lower chamber are baked by wrapping the corresponding components with heating tape and aluminum foil, then heating and baking the heating tape via a power supply. The first and second sputtering ion pumps are baked by wrapping the corresponding components with aluminum foil and then directly plugging the first and second sputtering ion pumps into a 220V power supply. During this baking and holding period, the first and second sputtering ion pumps are degassed by flashing them with a high-voltage power supply. This flashing process involves turning on the high voltage for a few seconds, then turning it off for about 10-20 seconds, and then flashing again. This process is repeated several times to degas the ion pumps. When the upper cavity, the lower cavity and the tube assembly begin to cool down, the baking of the first sputtering ion pump and the second sputtering ion pump is stopped, the first all-metal angle valve and the second all-metal angle valve are closed to isolate the molecular pump unit, and the first sputtering ion pump and the second sputtering ion pump are started to evacuate the film coating device so that the coating device finally reaches a limit vacuum better than ≤5E-8 Pa.
[0063] Then, the coating pipe and titanium-zirconium-vanadium alloy target are cleaned with radio frequency magnetron technology. Specifically, when the coating device reaches ultimate vacuum, the first and second sputtering ion pumps are shut down, the second all-metal angle valve is opened to allow the molecular pump unit to evacuate the vacuum, and the first and second thin-film vacuum gauges are simultaneously opened. The all-metal micro-leak valve is then opened to allow sputtering gas to flow in, and current is applied to the solenoid to generate a magnetic field. The electrode is then connected to an RF power supply. The high-voltage alternating electric field generated by the RF power supply and the magnetic field generated by the solenoid together generate plasma. This plasma reacts or collides with residual microparticle contaminants or metal oxide layers in the coating pipe to form volatile substances. Finally, these volatile substances are extracted by the molecular pump unit, completing the cleaning of the coating pipe and titanium-zirconium-vanadium alloy target.
[0064] Finally, DC magnetron sputtering is used to coat the pipe to be coated. That is, after the RF magnetron cleaning is completed, the RF power supply is disconnected first, and the electrode is connected to the DC power supply to ionize the gas and then the coating process can be carried out. The coating parameters can be set by yourself, for example: a constant current mode can be used (the current can be gradually increased from 0.1A to 0.3A). The free electrons in the space are accelerated by the electric field to fly towards the pipe to be coated. During the flight, they collide with the working gas, causing it to dissociate into positively charged ions (Kr + ) and an electron. Under the influence of the electric field, the positively charged ions bombard the surface of the cathode target, sputtering neutral molecules from the target and depositing them on the substrate. Dissociated secondary electrons, similarly influenced by the electric and magnetic fields, fly toward the target in a combined cycloidal and helical motion. This significantly lengthens the electron's trajectory, increases the probability of collisions with gas molecules, and continuously replenishes the electron supply. This process repeats, depositing a thin film on the surface of the pipe to be coated. Using four or more DC magnetron sputtering power supplies during the coating process enables batch thin-film deposition. Example 1
[0065] The pipe to be coated is a copper alloy pipe in the shape of a straight pipe with a circular cross-section, an inner diameter of 26 mm, a wall thickness of 1 mm, and a length of 1000 mm.
[0066] The copper alloy pipe was pickled in a 10% cleaning solution for 15 minutes, then passivated in a 5% passivation solution for 10 minutes, dried with 0.5 MPa nitrogen, and installed on the device for inspection, evacuation, and baking to achieve ultimate vacuum. The ultimate vacuums of the upper and lower chambers were 3.9E-8 Pa and 2.5E-8 Pa, respectively. The first and second sputtering ion pumps were turned off, the molecular pump was turned on, krypton gas was introduced, and the pressure in the upper and lower chambers was adjusted to 9 Pa. The difference between the first and second thin film vacuum gauges was controlled to within 0.1 Pa. RF cleaning was performed for 20 minutes at a power of 100 W. After cleaning, the device was switched to a pulsed DC magnetron sputtering power supply in constant current mode. The current was gradually increased from 0.1 A to 0.25 A, with a pulse period of T = 1.1 μs and a frequency of F = 40 kHz. The deposition time was 8 hours, and the magnetic field current intensity was 110 A.
[0067] like Figure 15 、 Figure 16 As shown, after the non-evaporable getter film of Example 1 was deposited, microscopic testing, pumping speed and capacity testing were performed to test the parameters. The pumping speed per unit area of the film was 5.94 L / (s·cm 2 ), with an adsorption capacity of 4.77E-5 mbar·L / cm 2 , the quality of the getter film meets the requirements for use.
[0068] The same specification of the coating pipe was coated using a traditional single-station coating system. The measured pumping speed per unit area of the film was 0.824 L / (s·cm 2 ), with an adsorption capacity of 4.01E-5 mbar·L / cm 2 It can be seen from this that the getter film produced by the device and method of the present invention can effectively improve the air extraction performance of the film, and can be plated in batches to improve efficiency.
[0069] The embodiments described above are merely descriptions of preferred implementations of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should fall within the scope of protection determined by the claims of the present invention.
Claims
1. An apparatus for batch coating non-evaporable getter films in small-diameter pipes with high aspect ratios, characterized by: The invention comprises an upper cavity (1) and a lower cavity (2) which are concentrically arranged and both have a sealed structure. A pipe assembly is provided between the upper cavity (1) and the lower cavity (2) to connect the two. The upper cavity (1) is connected to a first sputtering ion pump (11), a first thin film vacuum gauge (12), a first cold cathode ionization vacuum gauge (13), a first all-metal angle valve and an observation window (14); the lower cavity (2) is connected to a second sputtering ion pump (21), a second thin film vacuum gauge (22), a second cold cathode ionization vacuum gauge (23), a second all-metal angle valve (24) and an all-metal micro-leakage valve. The first all-metal angle valve and the second all-metal angle valve (24) are connected to the molecular pump unit through an upper bellows and a lower bellows respectively. The all-metal micro-leakage valve The lower cavity (2) is connected to the gas source via a stainless steel gas pipe, and is placed on the ground via a supporting foot (25); the tube assembly is evenly arranged in at least four groups along the circumference, and each group of the tube assembly comprises an upper transition bellows (3A), an electrode (4), an upper transition pipe (5A), a pipe to be coated (6), a lower transition pipe (5B), and a lower transition bellows (3B) that are sequentially connected from top to bottom; the electrode threaded rod (42) inside the electrode (4) is connected to the upper end of the titanium-zirconium-vanadium alloy target (7) via a connector (46), the lower end of the titanium-zirconium-vanadium alloy target (7) is an overhanging end, and the titanium-zirconium-vanadium alloy target (7) passes through the upper transition pipe (5A), the pipe to be coated (6), the lower transition pipe (5B), and the lower transition bellows (3B) in sequence; It also includes a solenoid (8) located between the upper cavity (1) and the lower cavity (2) and sleeved on the tube assembly, a gap is left between the inner wall of the solenoid (8) and the tube assembly, and the solenoid (8) is concentric with the upper cavity (1), and the solenoid (8) is fixed to the ground through a support frame.
2. The device for batch coating non-evaporable getter films in high aspect ratio small-aperture pipes according to claim 1, characterized in that: The support frame comprises a frame body (81) of overall trapezoidal structure, a top plate (82) fixed on the top of the frame body (81), and a support plate (83) located inside the frame body (81), wherein: a through hole for the solenoid (8) to pass through is opened at the center of the top plate (82), the support plate (83) is an annular structure, and the support plate (83) and the top of the frame body (81) are connected by a threaded rod (84), the bottom of the solenoid (8) is placed on the support plate (83), and the bottom of the upper cavity (1) is against the top of the solenoid (8) through the support assembly; the support assembly is arranged along There are four groups of support components evenly distributed around the solenoid (8), and each group of support components includes a support base (15) and two columns (16). The support base (15) is an overall arc-shaped bent structure, including a horizontally arranged arc plate (151) and an arc baffle (152) folded downward along the inner arc surface of the arc plate (151). The arc plate (151) is mounted on the upper surface of the solenoid (8), and the arc baffle (152) is attached to the inner wall of the solenoid (8); the upper and lower ends of the two columns (16) are fixed to the bottom of the upper cavity (1) and the upper plate surface of the arc plate (151), respectively.
3. The device for batch coating non-evaporable getter films in high aspect ratio small-aperture pipes according to claim 1, characterized in that: The four groups of pipe assemblies are connected by a fixing device, which includes a fixing column (9) arranged in a vertical direction, and the two ends of the fixing column (9) are respectively connected to the bottom surface of the upper cavity (1) and the fixing base (91), the fixing base (91) is disc-shaped and located at the center of the inner circle of the support plate (83), the fixing base (91) is provided with a U-shaped hole for the pipe assembly to pass through, and the fixing base (91) is fixed to the flange welding block (51) on the lower transition pipe (5B); the fixing device also includes a positioning plate (92) sleeved on the fixing column (9), the positioning plate (92) is a cross-shaped structure, the center of which is provided with a central positioning hole that matches the fixing column (9), and the four ends of the positioning plate are respectively provided with pipe positioning holes for the four groups of pipe assemblies to pass through, and the positioning plates (92) are arranged in two groups along the upper and lower directions, and the two groups of positioning plates (92) are respectively connected to the upper transition pipe (5A) and the lower transition pipe (5B) of the pipe assembly through right-angle connectors (93).
4. The device for batch coating non-evaporable getter films in high aspect ratio small-aperture pipes according to claim 1, characterized in that: The electrode (4) comprises a vacuum chamber (41), an electrode threaded rod (42), an electrode conductive member (43), a conductive welding member (44) and a high-voltage electrode head (45); the vacuum chamber (41) is in a three-way shape as a whole, and is formed by a vertical cavity (411) and a horizontal cavity (412) connected to each other, wherein: the two ends of the vertical cavity (411) are respectively connected to the upper transition bellows (3A) and the upper transition tube (5A), and the horizontal cavity (412) is connected to the high-voltage electrode head (45); the electrode threaded tube (42) is located in the vertical cavity (411) and is concentrically arranged with the vertical cavity (411), the upper end of the electrode threaded rod (42) is connected to the flange structure at the upper end of the vertical cavity (411) through a nut (421) and a gasket (422), and the lower end of the electrode threaded tube (42) is threadedly connected to the connector (46); The electrode conductive member (43) is sleeved on the electrode threaded tube (42) and is threadedly connected to the electrode threaded tube (42). The electrode conductive member (43) is an inverted T-shaped structure as a whole, consisting of a columnar body (431) and a circular base (432). The conductive welding member (44) includes a rod section (441). The rod section (441) is located in the horizontal cavity (412) and is concentrically arranged with the horizontal cavity (412). One end of the rod section (441) is provided with a cylindrical section (442) perpendicular to the rod section, and the cylindrical section (442) is sleeved on the columnar body (431) of the electrode conductive member (43). The other end of the rod section (441) is threadedly matched with the electrode rod (451) in the high-voltage electrode head (45). The rod section (441) and the electrode threaded tube (42) of the conductive welding member (44) are both sleeved with a ceramic tube.
5. The device for batch coating non-evaporable getter films in high aspect ratio small-aperture pipes according to claim 1, characterized in that: The connection ends of the upper transition bellows (3A), the electrode (4), the upper transition tube (5A), the pipe to be coated (6), the lower transition tube (5B), and the lower transition bellows (3B) are all flange structures. The upper transition bellows (3A) is connected to the CF vacuum flange at the bottom of the upper cavity (1), and the lower transition bellows (3B) is connected to the CF vacuum flange at the top of the lower cavity (2); The L / D ratio of the pipe to be coated (6) is ≥20; the nominal pumping speed of the first sputtering ion pump (11) is 100 L / s, and the nominal pumping speed of the second sputtering ion pump (21) is 200 L / s.
6. A method for batch coating non-evaporable getter film devices in small-diameter pipes with high aspect ratios according to any one of claims 1 to 5, characterized in that The steps include: S1: Cleaning the pipe to be coated; S2: connecting the upper transition bellows, the electrode, the upper transition pipe, the cleaned pipe to be coated, the lower transition pipe and the lower transition bellows in sequence to form a pipe assembly; S3: Install the tube assembly between the upper cavity and the lower cavity to complete the assembly of the coating device; S4: Connect the helium mass spectrometer leak detector to the lower bellows to perform a leak test on the coating device. When the leak rate is less than the set value, remove the helium mass spectrometer leak detector. S5: Connect the upper bellows and the lower bellows to the molecular pump unit at the same time to perform vacuuming until the vacuum degree at the pump port of the molecular pump unit reaches the set value; S6: baking and keeping the tube assembly, the upper cavity, the lower cavity, the first sputtering ion pump, and the second sputtering ion pump warm; S7: While S6 is baking and keeping warm, the first sputtering ion pump and the second sputtering ion pump are bombarded by a high-voltage power supply to perform a degassing treatment. The bombardment mode is "flash". When the upper cavity, the lower cavity and the tube assembly begin to cool down, the baking of the first sputtering ion pump and the second sputtering ion pump is stopped, the first all-metal angle valve and the second all-metal angle valve are closed to isolate the molecular pump unit, and the first sputtering ion pump and the second sputtering ion pump are started to evacuate the coating device to a limit vacuum of ≤5E-8Pa; S8: Radio frequency magnetron cleaning of the coating pipe and titanium zirconium vanadium alloy target; S9: Use DC magnetron sputtering to coat the pipe to be coated.
7. The method for batch coating non-evaporable getter films in high aspect ratio small-aperture pipes according to claim 6, characterized in that: In the above-mentioned S1, the cleaning comprises the following steps: S1.1: First, place the pipe to be coated in the cleaning solution and clean its inner and outer surfaces with a dust-free cloth to remove surface impurities and oxide layers. Then, rinse the remaining cleaning solution on the pipe to be coated with running deionized water. S1.2: Transfer the pipe to be coated into the passivation solution for passivation, and then rinse the residual passivation solution on the pipe with running deionized water; S1.3: Use flowing compressed nitrogen to dry the inner and outer surfaces of the pipe to be coated; S1.4: Perform a visual inspection to ensure that there are no obvious stains, water spots, or scratches on the inner surface of the pipe to be coated.
8. The method for batch coating non-evaporable getter films in high aspect ratio small-aperture pipes according to claim 7, characterized in that: In S1.1, the cleaning solution is a 10-15% concentration of copper acid cleaning solution and deionized water, and the cleaning time is 15-20 minutes; in S1.2, the passivation solution is a 5% concentration of ammonium citrate and deionized water, and the passivation time is 15 minutes; in S1.3, the pressure of the flowing compressed nitrogen is 0.5 MPa.
9. The method for batch coating non-evaporable getter films in high aspect ratio small-bore pipes according to claim 6, characterized in that: In S6, the pipe to be coated in the pipe assembly is baked at 180°C and kept warm for 24 hours; the remaining components, the upper cavity and the lower cavity in the pipe assembly are baked at 180-200°C and kept warm for 24 hours; the pipe assembly, the upper cavity and the lower cavity are baked by wrapping a heating tape around the corresponding components and wrapping them with aluminum foil, and heating and baking them by connecting the heating tape to a power supply; the first sputtering ion pump and the second sputtering ion pump are baked by wrapping aluminum foil around the corresponding components, and baking them by directly plugging the first sputtering ion pump and the second sputtering ion pump into a 220V power supply; temperature sensors are placed on the pipe assembly, the upper cavity and the lower cavity for temperature measurement feedback.
10. The method for batch coating non-evaporable getter films in small-diameter pipes with high aspect ratios according to claim 6, wherein: In the above-mentioned S8, after the coating device reaches the ultimate vacuum, the first sputtering ion pump and the second sputtering ion pump are turned off, and the second all-metal angle valve is opened to allow the molecular pump unit to evacuate the vacuum, and the first thin film vacuum gauge and the second thin film vacuum gauge are started at the same time; then the all-metal micro-leak valve is opened to allow the sputtering gas to pass through, and current is applied to the solenoid to generate a magnetic field; then the electrode is connected to the RF power supply, and the high-voltage alternating electric field generated by the RF power supply and the magnetic field generated by the solenoid jointly generate plasma, and the plasma reacts or collides with the residual micro-particle pollutants or metal oxide layer in the pipe to be coated to form volatile substances, and finally these volatile substances are extracted by the molecular pump unit to achieve the cleaning of the pipe to be coated and the titanium-zirconium-vanadium alloy target material; in the above-mentioned S9, the RF power supply is first disconnected, and the electrode is connected to the DC power supply to ionize the gas to carry out the coating process.
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