Vacuum heat treatment furnace and titanium-zirconium-niobium-tin alloy heat treatment method

By employing a guiding mechanism and clamping components in a vacuum heat treatment furnace, the automatic entry and exit of quartz tubes is achieved, solving the problem of non-target phase precipitation caused by long quartz tube transfer time, and improving cooling efficiency and alloy heat treatment quality.

CN121109718BActive Publication Date: 2026-02-10HUAQIAO UNIVERSITY
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Patent Information

Application Number
CN202511635813.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-11-10
Publication Date
2026-02-10
Estimated Expiration
2045-11-10

AI Technical Summary

Technical Problem

During the heat treatment of titanium-zirconium-niobium-tin alloys, the time required for the quartz tube to be transferred from the vacuum heat treatment furnace to the ice-water bath is relatively long, which may cause the alloy to cool slowly in the air, resulting in the precipitation of non-target phases and affecting the mechanical properties of the alloy.

Method used

A vacuum heat treatment furnace was designed, employing a guiding mechanism and clamping components to achieve automatic loading and unloading of quartz tubes. Combined with the design of the partition plate and extension section, it ensures that the quartz tubes are quickly transferred to the ice water insulation tank during cooling, shortening the transfer time and improving the cooling efficiency.

Benefits of technology

While ensuring safety, the transfer time of the quartz tube was shortened, the cooling efficiency was improved, the precipitation of non-target phases was avoided, and the heat treatment quality and safety of the alloy were ensured.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to the technical field of vacuum heat treatment furnaces, and discloses a vacuum heat treatment furnace and a titanium-zirconium-niobium-tin alloy heat treatment method. The vacuum heat treatment furnace comprises a base, a furnace body, a furnace door, a guide mechanism, two guide rails symmetrically arranged in the furnace body, a material rack comprising a supporting rod and a rotating plate rotatably arranged on the supporting rod, the supporting rod being fixedly connected with the furnace door, the supporting rod being slidably arranged on one guide rail when the material rack is located in the furnace body, one end of the rotating plate being slidably connected with the other guide rail, the rotating plate being rotated away from the furnace body when the material rack is separated from the furnace body, the rotating center line of the rotating plate being parallel to the central axis of the furnace body, a clamping assembly comprising a sliding frame and two clamping blocks, the sliding frame being provided with a control element for controlling the movement of the clamping blocks, the sliding frame being slidably arranged on the rotating plate, the sliding frame being slid downward along the rotating plate and separated from the furnace body after the sliding frame is rotated under the action of gravity, and the sliding frame falling into a heat preservation barrel. The application can shorten the cooling waiting time of a test piece.
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Description

Technical Field

[0001] This application relates to the technical field of vacuum heat treatment furnaces, and in particular to a vacuum heat treatment furnace and a heat treatment method for titanium-zirconium-niobium-tin alloys. Background Technology

[0002] Titanium-zirconium-niobium-tin (Ti–Zr–Nb–Sn) shape memory alloys can achieve approximately 7.5% superelastic recoverable strain at room temperature, comparable to the performance of commercial titanium-nickel-based alloys. They show excellent biomedical application prospects in medical devices such as vascular stents, orthodontic archwires, spinal fixation devices, and bone implants.

[0003] Titanium-zirconium-niobium-tin alloys, by introducing a high tin content into their composition, combined with high-temperature solution treatment and large-deformation cold rolling, and finally annealing at an appropriate temperature, achieve a β-phase alloy microstructure with excellent superelasticity. High-temperature solution treatment is a type of heat treatment and one of the core heat treatment processes commonly used to optimize the performance of metallic materials such as titanium-zirconium-niobium-tin alloys. It requires heating the material to a high temperature (usually above the phase transformation point, such as the β-phase region of titanium-zirconium-niobium-tin alloys, about 800-1000℃), holding it at that temperature for a period of time (to allow the solute elements to fully dissolve), and finally rapidly cooling it (such as water cooling or ice-water bath quenching).

[0004] After the titanium-zirconium-niobium-tin alloy is melted and formed into button-shaped ingots weighing 25-30 grams, the ingots are ultrasonically cleaned with anhydrous ethanol for 10-15 minutes and dried. They are then vacuum-sealed in quartz tubes and placed in a vacuum heat treatment furnace (vacuum degree (1.0-1.5) × 10⁻³ Pa) and held at 1000°C for 2 hours. After heat treatment, the quartz tubes are removed from the furnace and immediately placed in an ice-water bath for quenching and rapid cooling. The key to successfully connecting the vacuum heat treatment furnace and the ice-water bath is to complete the process of removing the quartz tube from the furnace and immersing it in ice water in the shortest possible time, while ensuring personnel safety.

[0005] Specific procedures: Place the ice-water bath device (containing crushed ice and purified water in an insulated container) next to the vacuum heat treatment furnace (≤1 meter away), ensuring an unobstructed transfer path to minimize handling time. After the heat treatment is complete, workers wearing high-temperature resistant gloves (to prevent burns) use a quartz tube clamping tool to remove the quartz tube from the vacuum heat treatment furnace. Slowly immerse the quartz tube vertically or at an angle into the ice-water mixture, ensuring the workpiece inside is completely encased in the ice-water. The same procedure applies after the annealing heating step of the heat treatment; quickly immerse the quartz tube in the ice-water bath for quenching and cooling.

[0006] In actual operation, if the titanium-zirconium-niobium-tin alloy is transferred slowly after homogenization or annealing (residing in air for more than 1-2 minutes), the workpiece will cool slowly in the air, and the β phase that should have been retained may precipitate prematurely into the α phase or other brittle second phases. The appearance of these non-target phases will lead to easy cracking of the sheet during subsequent cold rolling, or a significant decrease in the strength, toughness, and other mechanical properties of the final product. Summary of the Invention

[0007] To shorten the time required to transfer the insulated quartz tube to an ice-water bath, this application provides a vacuum heat treatment furnace and a heat treatment method for titanium-zirconium-niobium-tin alloy.

[0008] In a first aspect, this application provides a vacuum heat treatment furnace, which adopts the following technical solution:

[0009] A vacuum heat treatment furnace, comprising:

[0010] Base;

[0011] The furnace body is fixedly installed on the base;

[0012] The furnace door is detachably and sealingly installed on the furnace body;

[0013] A guide mechanism, mounted on the base, is used to control the furnace door to open or close the furnace body in the horizontal direction;

[0014] Two guide rails are symmetrically installed inside the furnace body;

[0015] The material rack includes a support rod and a rotating plate rotatably mounted on the support rod. One end of the support rod along its length is fixedly connected to the furnace door. When the material rack is located inside the furnace, the support rod is slidably mounted on one of the guide rails. One end of the rotating plate is slidably connected to another of the guide rails. When the material rack leaves the furnace, the rotating plate rotates away from the furnace. The rotation center line of the rotating plate is parallel to the central axis of the furnace.

[0016] The clamping assembly includes a slide and two clamping blocks. The slide is equipped with a control element that controls the movement of the clamping blocks, causing the clamping blocks to clamp the quartz tube. The slide is slidably mounted on the rotating plate. After the slide rotates with the rotating plate under the action of gravity, the quartz tube is in a vertical state and slides down the rotating plate with the slide as it moves away.

[0017] When the furnace door leaves the furnace body, a heat preservation bucket filled with ice water is placed on the base between the furnace door and the furnace body, and the slide falls into the heat preservation bucket along the rotating plate.

[0018] By adopting the above technical solution, during loading, the operator drives the clamping block to fix the vacuum quartz tube through the control component of the clamping assembly, slides the carriage onto the rotating plate of the material rack, and then the guide mechanism controls the horizontal movement of the furnace door, causing the support rod of the material rack and the rotating plate to slide along the corresponding guide rails, sending the quartz tube into the furnace body. Finally, the furnace door is closed for vacuum heat treatment. During cooling, the guide mechanism opens the furnace door, the material rack moves out with the furnace door, and the rotating plate rotates due to gravity after being separated from the guide rail support. After the rotating plate rotates, the carriage slides along the rotating plate and finally falls into the pre-placed ice water insulation tank with the quartz tube, realizing automatic entry and exit of the quartz tube. There is no need for manual handling of the high-temperature quartz tube, avoiding the risk of burns and improving operational safety. The cooperation between the rotating plate and the carriage allows the quartz tube to be quickly transferred from the furnace body to the ice water insulation tank, shortening the cooling waiting time and ensuring cooling efficiency and heat treatment quality.

[0019] Optionally, the carriage includes two main rods and a connecting seat. The two main rods are arranged in parallel. The rotating plate has a first sliding groove, and two second sliding grooves are symmetrically arranged with the first sliding groove as a reference. The connecting seat is slidably installed in the first sliding groove by a slider. One end of each of the two main rods along its length is slidably installed on the second sliding groove, and the control component is installed on the main rod.

[0020] By adopting the above technical solution, during cooling, the rotating plate rotates, the slider slides synchronously along the first slide groove and the main rod slides synchronously along the second slide groove, causing the carriage to smoothly detach from the rotating plate.

[0021] Optionally, the control component is a telescopic rod, which includes an outer rod and an inner rod. The outer rod is fixedly connected to the clamping block, and the inner rod is fixedly connected to the main rod. The inner rod is threaded with a nut. When the clamping block clamps the quartz tube wall, the nut abuts against the outer rod.

[0022] By adopting the above technical solution, the outer rod is pushed to make the clamping block clamp the quartz tube, and then the nut is tightened so that the nut abuts against the outer rod, fixing the length of the telescopic rod and thus locking the position of the clamping block. The telescopic rod has a simple structure, and the clamping force can be adjusted by turning the nut.

[0023] Optionally, the carriage further includes:

[0024] Two rods, one end of each rod is slidably installed in the first groove, the rotating plate is connected to a limiting rod, the limiting rod has a third groove, and the other end of each rod is slidably installed in the third groove;

[0025] An additional rod is located between the main rod and the support rod;

[0026] A rotating rod, with collars fixedly connected to both ends of the rotating rod, and the rotating rod connecting the main rod and the auxiliary rod, the support rod and the auxiliary rod through the collars;

[0027] When the quartz tube is mounted on the carriage and the carriage is mounted on the rotating plate, the ends of the support rod and the quartz tube are in contact, and an angle is formed between two adjacent rotating rods.

[0028] By adopting the above technical solution, the rotating plate and the limiting rod cooperate to ensure that the carriage can only slide into the rotating plate along the slide groove. The main rod and the support rod are connected by an additional rod. The main rod is always located in the second slide groove, and the support rod is always located in the first slide groove. Therefore, moving the support rod can change the position of the additional rod, thereby causing the angle between the two rotating rods on the same additional rod to change, so that the support rod can adapt to quartz tubes of different lengths.

[0029] Optionally, one of the support rods has a larger outer diameter, and two auxiliary rods corresponding to the support rod with the larger outer diameter are fixedly installed with abutment rods. The first slide groove includes a first section and a second section. The width of the first section is smaller than the width of the second section. The support rod with the smaller outer diameter and the slider pass through the first section and the second section in sequence. The support rod with the larger outer diameter is located on the second section. When the rotating plate rotates, the support rod with the larger outer diameter slides along the second section in a direction away from the quartz tube, driving the corresponding auxiliary rod to move. When the abutment rod abuts against the quartz tube, the support rod stops sliding.

[0030] By adopting the above technical solution, when the carriage is mounted on the rotating plate, the thin support rod and the slider are in the first section of the first slide groove, and the thick support rod is in the second section. At this time, the abutment rod is not in contact with the quartz tube. When the rotating plate rotates, the thick support rod slides away from the quartz tube along the second section due to gravity, which drives the corresponding additional rod to move, so that the angle of the two adjacent rotating rods is gradually adjusted. When the rotating rods are coaxial, the thick support rod stops sliding, and the additional rod drives the abutment rod to move to abut the outer wall of the quartz tube, further fixing the quartz tube from the side. This realizes the automatic triggering of the abutment rod when the rotating plate rotates. The abutment rod and the clamping block cooperate to form a double fixation, further preventing the quartz tube from shaking during the transfer process and ensuring the stability of the cooling process.

[0031] Optionally, the rotating plate has an installation groove in the first section of the first slide groove. A stop block and a spring are installed in the installation groove. The spring drives the stop block to extend out of the installation groove. The stop block has a guide slope at the beginning of its symmetrical shape. The support rod and the slider with the smaller outer diameter push the slider back into the installation groove through the guide slope in sequence. When the rotating plate rotates under the action of gravity, the slide slides vertically downward. The support rod and the slider squeeze the slider away from the first slide groove in sequence.

[0032] By adopting the above technical solution, during the installation of the carriage, the thin support rod and the slider press against the stop block along the guide slope, the spring is compressed, and the stop block retracts into the mounting groove, allowing the carriage to slide smoothly into the first slide groove. After the carriage is in place, the spring resets and pushes the stop block out of the mounting groove to prevent the carriage from sliding accidentally during the heat treatment process. During the rotation of the rotating plate, the carriage is restricted by the stop block and basically does not slide. Only the thick support rod slides. Only after the rotating plate naturally droops under gravity does the carriage slide vertically under gravity. The support rod and the slider press against the stop block together, the spring is compressed again, the stop block returns to the groove, and the carriage smoothly leaves the first slide groove.

[0033] Optionally, the material rack further includes partition plates mounted on the support rod. The partition plates are spaced apart, and a rotating plate and a clamping assembly are accommodated between two adjacent partition plates. The furnace opening of the furnace body extends into an extension section, and the guide rail extends into the extension section. When the partition plate passes through the extension section, the outer periphery of the partition plate is in contact with the inner wall of the extension section. The guiding mechanism drives the furnace door to move intermittently. When the furnace door stops moving, one of the partition plates is located in the extension section.

[0034] By adopting the above technical solution, during loading, the rotating plate and clamping assembly between each partition plate fix a set of quartz tubes respectively. The guide mechanism drives the furnace door to move intermittently, driving the material rack into the furnace body. The guide rail extends to the extension section to ensure the smooth sliding of the material rack. At the same time, when heating multiple sets of quartz tubes, during the cooling stage, the partition plate and the extension section adhere to and block the passage, so that the quartz tubes that have not left the furnace body still have a certain heat preservation effect, realizing the heat treatment of multiple sets of quartz tubes and improving the heat treatment efficiency.

[0035] Optionally, the support rods on both sides of the partition plate are respectively connected to the two guide rails, and the two adjacent rotating plates are also slidably connected to the guide rails. One insulated bucket receives one slide, and the insulated bucket is placed in a different position when the insulated bucket is replaced.

[0036] By adopting the above technical solution, the falling position of the slide varies depending on the rotation position of the rotating plate. The position of the barrel can be adjusted accordingly to achieve continuous replacement of the insulation barrel. The support rod is connected to different guide rails to make the material rack slide more smoothly. At the same time, it provides different falling paths for the slide, which facilitates the alternating reception of the insulation barrel and improves the continuity of the cooling process.

[0037] Optionally, the support rod with a larger outer diameter is connected to a counterweight, which is inserted into the second section of the first groove.

[0038] By adopting the above technical solution, when the rotating plate rotates, the counterweight block drives the thick support rod to slide quickly along the second section of the first slide groove due to gravity, which accelerates the process of the abutment rod abutting the quartz tube and shortens the fixing time. When the slide slides down, the gravity of the counterweight block assists the thick support rod in squeezing the blocking block, ensuring that the slide smoothly leaves the slide groove.

[0039] Secondly, this application provides a heat treatment method for titanium-zirconium-niobium-tin alloys, employing the following technical solution:

[0040] A heat treatment method for titanium-zirconium-niobium-tin alloy, using the aforementioned vacuum heat treatment furnace, includes the following steps:

[0041] S1. Preparation before homogenization: washing and drying;

[0042] S2. Homogenization packaging: Vacuum-packing titanium-zirconium-niobium-tin alloy ingots into quartz tubes;

[0043] S3. Homogenization heating: First, place the quartz tube into the slide. After the two clamping blocks clamp and fix the quartz tube, slide the slide with the quartz tube in it horizontally into the rotating plate and the limiting rod. The guide mechanism pushes the furnace door, so that the support rod and the counterweight slide in along the guide rail. Close the furnace door to keep the quartz tube in the furnace at 1000℃ for 2 hours.

[0044] S4. Homogenization cooling: The furnace door is driven to move intermittently by a guide mechanism. When the furnace door stops moving for the first time, the partition plate closest to the furnace door is located in the extension section. The insulation bucket is placed on the base of the furnace door and the furnace body. When the furnace door moves again, the rotating plate gradually moves away from the furnace body. The furnace door stops moving, the rotating plate moves away from the furnace body and rotates downward. During the rotation, the counterweight drives the large-diameter support rod to move downward and drives the abutment rod to abut the quartz tube. The rotating plate stops rotating, and the slide moves vertically downward along the rotating plate. The quartz tube enters the insulation bucket while maintaining a vertical state.

[0045] S5, cold rolling deformation;

[0046] S6. Annealing heat treatment: Samples are cut from cold-rolled sheet along the rolling direction, mechanically polished and ultrasonically cleaned with anhydrous ethanol, and then vacuum-sealed in a quartz tube. The quartz tube is first placed in the slide, and after the two clamping blocks clamp and fix the quartz tube, the slide with the quartz tube is slid horizontally into the rotating plate and the limiting rod. The guide mechanism pushes the furnace door, so that the support rod and the counterweight slide in along the guide rail. The furnace door is closed, and the sample is annealed at different temperatures for 30 minutes.

[0047] S7. Annealing and cooling: The furnace door is driven to move intermittently by the guide mechanism. When the furnace door stops moving for the first time, the partition plate closest to the furnace door is located in the extension section. The insulation bucket is placed on the base of the furnace door and the furnace body. When the furnace door moves again, the rotating plate gradually moves away from the furnace body. The furnace door stops moving, the rotating plate moves away from the furnace body and rotates downward. During the rotation, the counterweight drives the large-diameter support rod to move downward, driving the abutment rod to abut the quartz tube. The rotating plate stops rotating, and the slide moves vertically downward along the rotating plate. The quartz tube enters the insulation bucket while remaining vertical.

[0048] By adopting the above technical solution, the homogenization stage involves cleaning and drying the titanium-zirconium-niobium-tin alloy ingot, encapsulating it in a quartz tube, fixing it with a clamping assembly, and then sending it into the furnace. It is held at 1000℃ for 2 hours, followed by rapid cooling. The cold rolling deformation stage involves cold rolling the homogenized alloy to change its morphology. The annealing stage involves cutting cold-rolled sheet samples, cleaning and encapsulating them, and then sending them into the furnace. They are held at different temperatures for 30 minutes, followed by cooling to complete the heat treatment. The combination of homogenization heating (holding at 1000℃ for 2 hours) and rapid cooling ensures safety while shortening the quartz tube transfer time. Furthermore, the quartz tube is vertically inserted into the heat-insulating barrel during cooling, further improving the stability of the alloy quality after heat treatment.

[0049] In summary, this application includes at least one of the following beneficial effects:

[0050] 1. While ensuring safety, shorten the quartz tube transfer time;

[0051] 2. During the cooling stage, the partition plate and the extension section are fitted together to block the passage, so that the quartz tube that has not left the furnace body still has a certain heat preservation effect, enabling multiple groups of quartz tubes to undergo heat treatment and improving heat treatment efficiency. Attached Figure Description

[0052] Figure 1 This is a schematic diagram of the overall structure of an embodiment of this application;

[0053] Figure 2 This is a schematic diagram illustrating the structure of the material rack and guide rail in an embodiment of this application;

[0054] Figure 3 This is a cross-sectional view of the material rack portion located inside the furnace body in an embodiment of this application;

[0055] Figure 4 This is a schematic diagram illustrating the state of the rotating plate after it has rotated downwards, according to an embodiment of this application.

[0056] Figure 5 This is an overall schematic diagram illustrating the clamping assembly and rotating plate in an embodiment of this application;

[0057] Figure 6 This is a schematic diagram illustrating the overall structure of the clamping component in an embodiment of this application;

[0058] Figure 7 This is a schematic diagram illustrating the overall structure of the clamping assembly and the rotating plate in an embodiment of this application;

[0059] Figure 8 This is a schematic diagram illustrating the cooperation between the abutment rod and the quartz tube in an embodiment of this application;

[0060] Figure 9 This is a schematic diagram illustrating the structure of the rotating plate in an embodiment of this application;

[0061] Figure 10 This is a cross-sectional view of the interior of the rotating plate as shown in the embodiment of this application;

[0062] Figure 11 This is a schematic diagram illustrating the installation of counterweights on the support rod in an embodiment of this application;

[0063] Figure 12 This is a flowchart of the heat treatment process for titanium-zirconium-niobium-tin alloy according to an embodiment of this application.

[0064] Explanation of reference numerals in the attached drawings: 100, base; 110, groove; 200, furnace body; 210, furnace door; 211, protrusion; 220, guide rail; 230, extension section; 300, guiding mechanism; 310, guide rod; 320, screw; 330, servo motor; 400, material rack; 410, support rod; 420, rotating plate; 421, first slide rail; 4211, first section; 4212, second section; 422, second slide rail; 423, extension rod; 430, partition plate; 431, rotating shaft; 440, limit switch. 441. Rod; 450. Third slide groove; 460. Mounting groove; 461. Stop block; 470. Guide slope; 500. Spring; 510. Clamping assembly; 511. Slide carriage; 512. Main rod; 512. Connecting seat; 5121. Slider; 513. Support rod; 514. Additional rod; 515. Rotating rod; 516. Collar; 517. Abutment rod; 520. Clamping block; 530. Control component; 531. Outer rod; 532. Inner rod; 533. Nut; 600. Insulation tank; 700. Counterweight; 800. Quartz tube. Detailed Implementation

[0065] The following is in conjunction with the appendix Figure 1 -Appendix Figure 12 This application will be described in further detail.

[0066] Example 1 of this application: Refer to Figure 1 A vacuum heat treatment furnace is disclosed, comprising a base 100, a furnace body 200, a furnace door 210, and a guide mechanism 300. The entire furnace is mounted on the base 100, which is placed horizontally. The furnace body 200 is horizontally fixed on the base 100, with the furnace opening facing one side. The interior of the furnace body 200 is a sealed heat treatment chamber. The heating and vacuum treatment within the furnace body 200 are existing technologies and have not been improved.

[0067] Reference Figure 1The furnace door 210 is detachably and sealingly installed at the furnace opening of the furnace body 200. The central axis of the furnace door 210 coincides with the central axis of the furnace body 200, ensuring that the furnace opening is completely sealed when the furnace door 210 is closed, maintaining a vacuum environment inside the furnace. The guide mechanism 300 includes two guide rods 310 and one screw 320. The base 100 has three grooves 110, and the two guide rods 310 and the screw 320 are rotatably installed in the grooves 110 of the base 100, with the screw 320 located between the two guide rods 310. The bottom of the furnace door 210 is fixedly connected to three protrusions 211, through which a guide tube passes. The screw 320 is threadedly connected to the protrusions 211. The guide mechanism 300 also includes a servo motor 330, the output shaft of which is fixedly connected to the screw 320, driving the screw 320 to rotate, thereby closing or opening the furnace door 210. The servo motor 330 is controlled by a program to drive the furnace door 210 to move intermittently.

[0068] Reference Figure 1 Two guide rails 220 are symmetrically installed inside the furnace body 200, and the extension direction of the guide rails 220 is consistent with the axial direction of the furnace body 200. A material rack 400 is installed on the furnace door 210, so that the material rack 400 moves in and out of the furnace body 200 along with the furnace door 210. The material rack 400 includes a support rod 410, a rotating plate 420, and a partition plate 430. The partition plate 430 is circular and is fixedly installed on the support rod 410. The support rod 410 extends along the axial direction of the furnace body 200, and one end in the length direction is fixedly connected to the inner side wall of the furnace door 210.

[0069] Reference Figure 2 The rotating plate 420 is rotatably mounted on the partition plate 430 via a rotating shaft 431, which is fixedly mounted on the partition plate 430. A rotating sleeve is fixedly connected to the rotating plate 420, and the rotating sleeve rotates around the rotating shaft 431. The rotation center line of the rotating plate 420 is parallel to the central axis of the furnace body 200, and an extension rod 423 is connected to the end of the rotating plate 420 away from the support rod 410. The extension rod 423 is slidably connected to one of the guide rails 220, and the support rod 410 is slidably connected to the other guide rail 220. This allows the support rod 410 and the extension rod 423 to slide along their respective guide rails 220 when the furnace door 210 is opened or closed, allowing the material rack 400 to enter and exit the furnace body 200 as a whole. When the material rack 400 leaves the furnace body 200, the rotating plate 420 loses the support of the guide rails 220 and rotates downward around the rotating shaft 431.

[0070] Reference Figure 3 and Figure 4A clamping assembly 500 is slidably mounted on the rotating plate 420 to clamp the quartz tube 800, keeping the quartz tube 800 horizontal as it enters the furnace body 200 for heat preservation. When the rotating plate 420 leaves the furnace body 200, the clamping assembly 500 rotates with it. When the rotating plate 420 stops rotating, the quartz tube 800, in a vertical position, leaves the rotating plate 420 along with the clamping assembly 500. A heat preservation tank 600 filled with ice water is placed between the furnace door 210 and the base 100 of the furnace body 200. The vacuum quartz tube 800, along with the clamping assembly 500, falls into the heat preservation tank 600, achieving rapid transfer of the quartz tube 800.

[0071] Reference Figure 2 and Figure 3 The partition plates 430 are spaced apart along the length of the support rod 410, forming a receiving space between two adjacent partition plates 430. Each receiving space is equipped with a rotating plate 420 and a clamping assembly 500, enabling simultaneous heat treatment of multiple sets of quartz tubes 800. An extension section 230 extends from the furnace opening of the furnace body 200, with a guide rail 220 extending from inside the furnace body 200 into the extension section 230. When the partition plates 430 move with the material rack 400 through the extension section 230, the outer periphery of the partition plates 430 fits tightly against the inner wall of the extension section 230. Simultaneously, the guide mechanism 300 drives the furnace door 210 in an intermittent manner, ensuring that after each movement, a partition plate 430 is positioned within the extension section 230, sealing the furnace opening and reducing heat loss from the furnace.

[0072] Reference Figure 2 and Figure 4 The two support rods 410 connected to the same partition plate 430 are respectively connected to the two guide rails 220, and the extension rods 423 of the two adjacent rotating plates 420 are also slidably connected to the guide rails 220. Therefore, the sliding position of the carriage 510 varies depending on the rotation position of the rotating plate 420. One insulated bucket 600 receives one clamping assembly 500, and two insulated buckets 600 can be placed on the base 100 at the same time to receive the clamping assembly 500 that slides down for the first and second time. After the clamping assembly 500 that slides down for the first time has completely entered the insulated bucket 600, the insulated bucket 600 can be transferred and replaced with a new insulated bucket 600 to prepare for receiving the clamping assembly 500 for the third time, so that people can change buckets easily and improve the continuity of bucket changing.

[0073] Reference Figure 5 and Figure 6The clamping assembly 500 includes a slide 510, two clamping blocks 520, and a control component 530. The slide 510 includes two main rods 511 and a connecting seat 512. The main rods 511 and the connecting seat 512 are fixedly connected, and the two main rods 511 are parallel to each other. The slide 510 also includes two parallel support rods 513, which form a four-point distribution with the two support rods 511, and the lines connecting the four points form a rectangular structure. An auxiliary rod 514 is installed between the main rods 511 and the support rods 513. Rotating rods 515 are connected between the main rods 511 and the auxiliary rod 514, and between the support rods 513 and the auxiliary rod 514. Both ends of the rotating rods 515 are fixedly connected to collars 516, and the two collars 516 are rotatably mounted on the main rods 511 and the auxiliary rods 514, and the support rods 513 and the auxiliary rods 514, respectively. When the carriage 510 is not yet installed on the rotating plate 420, the main rod 511, the support rod 513 and the auxiliary rod 514 can rotate relative to each other.

[0074] Reference Figure 5 and Figure 6 The control component 530 includes an outer rod 531 and an inner rod 532. One end of the outer rod 531 is fixedly connected to the clamping block 520, and one end of the inner rod 532 is fixedly connected to the main rod 511. The outer periphery of the inner rod 532 is threaded and threadedly connected to a nut 533. When it is necessary to clamp the vacuum quartz tube 800, the outer rod 531 is pushed to drive the clamping block 520 closer to the quartz tube 800. After the clamping block 520 is in contact with the wall of the quartz tube 800, the nut 533 is tightened so that the nut 533 abuts against the end of the outer rod 531, locking the length of the telescopic rod, thereby stably clamping the quartz tube 800.

[0075] Reference Figure 5 and Figure 6 The rotating plate 420 is provided with a first sliding groove 421 and two second sliding grooves 422. The two second sliding grooves 422 are symmetrically distributed on both sides of the first sliding groove 421 with the first sliding groove 421 as the reference. The bottom of the connecting seat 512 is fixed with a slider 5121. One end of the support rod 513 and the slider 5121 are slidably installed in the first sliding groove 421. One end of the two main rods 511 in the length direction is slidably installed in the corresponding second sliding grooves 422, so that the slide 510 can slide along the sliding groove as a whole.

[0076] Reference Figure 6 When the quartz tube 800 is mounted on the carriage 510 and the carriage 510 is located on the rotating plate 420, the main rod 511 slides in the second groove 422, and the support rod 513 slides in the first groove 421. The positional changes of the main rod 511 and the support rod 513 are restricted. When the support rod 513 changes position along the first groove 421, an angle of less than or equal to 180° is formed between two adjacent rotating rods 515. The end of the support rod 513 contacts the end of the quartz tube 800, and an angle of less than 180° is formed between two adjacent rotating rods 515, providing end support for the quartz tube 800.

[0077] Reference Figure 5 and Figure 7 An L-shaped limiting rod 440 is connected to the rotating plate 420. A third sliding groove 441 is provided on the limiting rod 440. The other end of the support rod 513 slides in the third sliding groove 441, so that the slide 510 slides stably on the rotating plate 420. When the rotating plate 420 is located inside the furnace body 200, one end of the limiting rod 440 is also inserted into the guide rail 220. The limiting rod 440 and the rotating plate 420 together provide support for the clamping assembly 500.

[0078] Reference Figure 8 Furthermore, the two support rods 513 have different outer diameters. The support rod 513 with a larger outer diameter is farther away from the rotating shaft 431, and the two corresponding auxiliary rods 514 are also fixedly equipped with abutment rods 517. The end of the abutment rod 517 has an arc groove. When the support rod 513 with a larger outer diameter moves away from the quartz tube 800, it drives the auxiliary rods 514 to move. When the arc groove of the abutment rod 517 abuts against the outer circumference of the quartz tube 800, the support rod 513 stops sliding and cooperates with the clamping block 520 to achieve double fixation of the quartz tube 800. Inside the furnace body 200, the two support rods 513 abut against the ends of the quartz tube 800 respectively. Only when the rotating plate 420 rotates, the support rod 513 with a larger outer diameter automatically moves away from the quartz tube 800 under the action of gravity, driving the abutment rod 517 to abut against the quartz tube 800, thereby enhancing the stability of the quartz tube 800 during rotation.

[0079] Reference Figure 9 The first slide groove 421 is divided into a first section 4211 and a second section 4212. The width of the first section 4211 is smaller than the width of the second section 4212. The smaller outer diameter support rod 513 and the slider 5121 of the connecting seat 512 can pass through the first section 4211 and the second section 4212 in sequence, while the larger outer diameter support rod 513 can only be located within the second section 4212. The positions of the two support rods 513 can be quickly determined through the first section 4211 and the second section 4212.

[0080] Reference Figure 10The rotating plate 420 has an installation groove 450 in the first section 4211 of the first slide groove 421. A stop block 460 and a spring 470 are installed in the installation groove 450. One end of the spring 470 is fixedly connected to the bottom of the installation groove 450, and the other end is fixedly connected to the stop block 460. In the natural state of the spring 470, a part of the stop block 460 extends out of the installation groove 450. Guide slopes 461 are symmetrically provided on both sides of the stop block 460. When the slide 510 is installed, the smaller outer diameter support rod 513 and slider 5121 press against the stop block 460 along the guide slope 461, compressing the spring 470. The stop block 460 retracts into the mounting groove 450, allowing the slide 510 to slide in. When the rotating plate 420 rotates under gravity, the slide 510 slides vertically downwards along the rotating plate 420 under gravity. The support rod 513 and slider 5121 press against the stop block 460 in sequence, causing the stop block 460 to retract into the mounting groove 450 again, allowing the slide 510 to smoothly leave the first slide groove 421. This ensures that the slide 510 remains stable as the rotating plate 420 rotates.

[0081] Furthermore, refer to Figure 11 A counterweight 700 is fixedly connected to a large-diameter support rod 513. The counterweight 700 is inserted into the first sliding groove 421 and partially extends out of the first sliding groove 421. When the material rack 400 is located inside the furnace body 200, the counterweight 700 is also inserted into the guide rail 220, forming a sliding connection with the guide rail 220. The counterweight 700, located outside the furnace body 200, causes the abutment rod 517 to press against the quartz tube 800, improving the stability of the quartz tube 800's transfer.

[0082] Additionally, the extension rod 423 can also be fixedly connected to the counterweight 700. The length of the extension rod 423 is matched with the sliding stroke of the counterweight 700. When the extension rod 423 abuts against the rotating plate 420, the counterweight 700 stops sliding in, thus avoiding excessive sliding that could affect the sliding of the support rod 513.

[0083] The implementation principle of a vacuum heat treatment furnace according to an embodiment of this application is as follows:

[0084] The support rod 410 of the material rack 400 is fixed to the furnace door 210. The rotating plate 420 and the support rod 410 are slidably engaged with different guide rails 220. When the furnace door 210 moves, it drives the material rack 400 in and out of the furnace body 200. After the material rack 400 leaves the furnace body 200, the rotating plate 420 loses its support and rotates downwards due to gravity. The slide 510 of the clamping assembly 500 is slidably connected to the rotating plate 420. When the rotating plate 420 rotates, it uses the gravity of the counterweight 700 to make the thick support rod 410 rotate downwards. 13 First, slide, driving the abutment rod 517 to automatically press against the quartz tube 800 to form a double fixation; the partition plates 430 are distributed at intervals on the material rack 400 and cooperate with the furnace mouth extension section 230. When the guide mechanism 300 drives the furnace door 210 to move intermittently, a partition plate 430 will block the furnace mouth after each movement. The cooperation between the partition plate 430 and the extension section 230 can play a role in moving and heat preservation for the quartz tube 800 that has not been transferred, and at the same time realize the batch processing of multiple sets of quartz tubes 800.

[0085] Example 2: Refer to Figure 12 This paper discloses a heat treatment method for titanium-zirconium-niobium-tin alloy, which is carried out in the vacuum heat treatment furnace described in Example 1. The method includes three stages: homogenization treatment, cold rolling deformation, and annealing heat treatment. The specific steps are as follows:

[0086] S1. Preparation before homogenization: Clean the ingot with anhydrous ethanol for 10–15 min by ultrasonic cleaning and then dry it.

[0087] S2. Homogenization and Packaging: The dried titanium-zirconium-niobium-tin alloy ingots are placed into multiple vacuum quartz tubes 800. Vacuum packaging equipment is used to evacuate and seal each quartz tube 800 to ensure that the vacuum degree inside the quartz tube 800 is not less than 1×10⁻³Pa, so as to prevent the ingots from oxidizing during the heat treatment process.

[0088] S3. Homogenization Heating: First, place the vacuum quartz tube 800 with the ingot encapsulated between the two clamping blocks 520 of the slide 510. Push the outer rod 531 of the telescopic rod to make the two clamping blocks 520 fit against the outer periphery of the quartz tube 800. Then tighten the nut 533 on the inner rod 532 to lock the position of the clamping blocks 520, completing the clamping of the quartz tube 800. Next, slide the slide 510 with the quartz tube 800 installed horizontally into the rotating plate 420 along the first slide groove 421 and the second slide groove 422. In the matching structure of the limiting rod 440, the wall of the support rod 513 contacts the end of the quartz tube 800, at which time the adjacent rotating rods 515 form an angle; the guide mechanism 300 is activated, driving the furnace door 210 to move horizontally into the furnace body 200. The furnace door 210 drives the support rod 410, the extension rod 423 on the rotating plate 420 and the counterweight 700 to slide along the corresponding guide rails 220 respectively, sending the quartz tube 800 into the furnace body 200; after all the quartz tubes 800 have completely entered the furnace body 200, the furnace door 210 is just sealed and fitted with the furnace body 200, completing the closure of the furnace door 210, keeping the inside of the furnace body 200 in a vacuum state, and then the heating device of the furnace body 200 is activated to raise the furnace temperature to 1000℃, and hold it at this temperature for 2 hours to complete the homogenization heating of the alloy ingot.

[0089] S4. Homogenization Cooling: After the heat preservation is completed, the guide mechanism 300 is activated, driving the furnace door 210 to move intermittently in a direction away from the furnace body 200. When the furnace door 210 stops moving for the first time, the partition plate 430 closest to the furnace door 210 just enters the extension section 230 of the furnace body 200, and its outer periphery fits against the inner wall of the extension section 230, sealing the furnace opening; at this time, a heat preservation tank 600 filled with ice water is quickly placed between the furnace door 210 and the base 100, and the position of the heat preservation tank 600 corresponds to the subsequent descent path of the slide 510. Subsequently, the furnace door 210 starts moving again, causing the rotating plate 420 closest to the furnace door 210 to gradually move away from the furnace body 200. After leaving the furnace body 200, the rotating plate 420 loses its support and rotates downward around the rotating shaft 431. During the rotation of the rotating plate 420, the furnace door 210 is in a stopped state. Under the action of gravity, the counterweight 700 drives the large-diameter support rod 513 to slide away from the quartz tube 800, which in turn drives the auxiliary rod 514 to move until the abutment rod 517 abuts against the quartz tube 800. When the rotating plate 420 stops rotating, the slide 510 slides vertically downward along the rotating plate 420 under the force of gravity. The support rod 513 and the slider 5121 press against the stop block 460 in sequence, causing the stop block 460 to retract into the mounting groove 450. The slide 510 smoothly leaves the rotating plate 420, causing the quartz tube 800 to slowly fall into the ice water of the insulation tank 600 while maintaining a vertical position, thus achieving rapid cooling. After changing the position of the insulation tank 600, the furnace door 210 continues to move intermittently to cool the subsequent quartz tubes 800.

[0090] S5. Cold rolling deformation: The homogenized and cooled titanium-zirconium-niobium-tin alloy ingot is taken out from the quartz tube 800 and cold rolled using a cold rolling machine. A sample with a size of 20 (length) × 10 (width) × 10 (height) mm³ is cut from the ingot and cold rolled along the length direction at room temperature with a total reduction of 95–98% to obtain a plate with a thickness of 0.15–0.2 mm.

[0091] S6. Annealing heat treatment: Cut samples of uniform specifications from the cold-rolled sheet along the rolling direction. After mechanical polishing and ultrasonic cleaning with anhydrous ethanol, place the samples into new vacuum quartz tubes 800 and seal them in vacuum again. Then, in the same manner as in S3, install the quartz tubes 800 containing the samples on the rotating plate 420 of the material rack 400 via the slide 510. Start the guide mechanism 300 to close the furnace door 210 and maintain a vacuum state inside the furnace. According to the heat treatment requirements, set the furnace body 200 temperature to different annealing temperatures (such as 850°C, 900°C, 950°C, 1000°C, 1050°C, and 1100°C). Hold the samples at each temperature for 30 minutes to complete the annealing heat treatment.

[0092] S7. Annealing and Cooling: After the annealing and heat preservation are completed, the furnace door 210 is driven in the same intermittent movement manner as in S4. When the furnace door 210 stops for the first time, the furnace opening is sealed with the partition plate 430 and the heat preservation barrel 600 is placed. The furnace door 210 moves again, causing the rotating plate 420 to leave the furnace body 200 and rotate downward. The counterweight 700 drives the support rod 513 to slide, causing the abutment rod 517 to abut against the quartz tube 800. The slide 510 drives the quartz tube 800 to fall vertically into the heat preservation barrel 600 for cooling. After all the samples have been cooled in sequence, the samples are taken out, and the entire heat treatment process is completed.

[0093] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A vacuum heat treatment furnace, characterized in that, include: Base (100); The furnace body (200) is fixedly installed on the base (100); The furnace door (210) is detachably and sealingly installed on the furnace body (200); A guide mechanism (300) is installed on the base (100) and is used to control the furnace door (210) to open or close the furnace body (200) in the horizontal direction. Two guide rails (220) are symmetrically installed inside the furnace body (200); The material rack (400) includes a support rod (410) and a rotating plate (420) rotatably mounted on the support rod (410). One end of the support rod (410) along its length is fixedly connected to the furnace door (210). When the material rack (400) is located inside the furnace body (200), the support rod (410) is slidably mounted on one of the guide rails (220). One end of the rotating plate (420) is slidably connected to the other guide rail (220). When the material rack (400) leaves the furnace body (200), the rotating plate (420) rotates away from the furnace body (200). The rotation center line of the rotating plate (420) is parallel to the central axis of the furnace body (200). The clamping assembly (500) includes a slide (510) and two clamping blocks (520). The slide (510) is equipped with a control element (530) that controls the movement of the clamping blocks (520) to drive the clamping blocks (520) to clamp the quartz tube (800). The slide (510) is slidably mounted on the rotating plate (420). After the slide (510) rotates with the rotating plate (420) under the action of gravity, the quartz tube (800) is in a vertical state and slides downward away from the rotating plate (420) along with the slide (510). When the furnace door (210) leaves the furnace body (200), a heat preservation bucket (600) filled with ice water is placed on the base (100) between the furnace door (210) and the furnace body (200), and the slide (510) falls into the heat preservation bucket (600) along the rotating plate (420); The carriage (510) includes two main rods (511) and a connecting seat (512). The two main rods (511) are arranged in parallel. The rotating plate (420) has a first sliding groove (421). Two second sliding grooves (422) are symmetrically arranged with the first sliding groove (421) as a reference. The connecting seat (512) is slidably installed in the first sliding groove (421) through a slider (5121). One end of each of the two main rods (511) is slidably installed on the second sliding groove (422) in the length direction. The control component (530) is installed on the main rod (511). The carriage (510) also includes: Two support rods (513), one end of the two support rods (513) is slidably installed in the first slide groove (421), the rotating plate (420) is connected to a limit rod (440), the limit rod (440) is provided with a third slide groove (441), and the other end of the two support rods (513) is slidably installed in the third slide groove (441); An additional rod (514) is located between the main rod (511) and the support rod (513); A rotating rod (515) has a collar (516) fixedly connected to both ends of the rotating rod (515). The rotating rod (515) is connected to the main rod (511) and the auxiliary rod (514), the support rod (513) and the auxiliary rod (514) through the collar (516). When the quartz tube (800) is mounted on the carriage (510) and the carriage (510) is mounted on the rotating plate (420), the end of the support rod (513) and the quartz tube (800) are in contact, and an angle is formed between two adjacent rotating rods (515); One of the support rods (513) has a larger outer diameter. The two auxiliary rods (514) corresponding to the support rod (513) with the larger outer diameter are fixedly installed with abutment rods (517). The first slide groove (421) includes a first section (4211) and a second section (4212). The width of the first section (4211) is smaller than the width of the second section (4212). The support rod (513) with the smaller outer diameter and the slider (5121) pass through the first section (4211) and the second section (4212) in sequence. The support rod (513) with the larger outer diameter is located on the second section (4212). When the rotating plate (420) rotates, the support rod (513) with the larger outer diameter slides along the second section (4212) away from the quartz tube (800), driving the corresponding auxiliary rod (514) to move. When the abutment rod (517) abuts against the quartz tube (800), the support rod (513) stops sliding.

2. The vacuum heat treatment furnace according to claim 1, characterized in that, The control component includes an outer rod (531) and an inner rod (532). The outer rod (531) is fixedly connected to the clamping block (520), and the inner rod (532) is fixedly connected to the main rod (511). The inner rod (532) is threaded with a nut (533). When the clamping block (520) clamps the wall of the quartz tube (800), the nut (533) abuts against the outer rod (531).

3. A vacuum heat treatment furnace according to claim 1, characterized in that, The rotating plate (420) has an installation groove (450) in the first section (4211) of the first slide groove (421). A stop block (460) and a spring (470) are installed in the installation groove (450). The spring (470) drives the stop block (460) to extend out of the installation groove (450). The stop block (460) has a guide slope (461) symmetrically. The support rod (513) and the slider (5121) with smaller outer diameter push the slider (5121) back into the installation groove (450) through the guide slope (461). When the rotating plate (420) rotates under the action of gravity, the slide (510) slides vertically downward. The support rod (513) and the slider (5121) squeeze the slider (5121) away from the first slide groove (421) in turn.

4. A vacuum heat treatment furnace according to claim 1, characterized in that, The material rack (400) also includes a partition plate (430) installed on the support rod (410). The partition plates (430) are spaced apart. A rotating plate (420) and a clamping assembly (500) are accommodated between two adjacent partition plates (430). The furnace opening of the furnace body (200) extends into an extension section (230). The guide rail (220) extends into the extension section (230). When the partition plate (430) passes through the extension section (230), the outer periphery of the partition plate (430) is in contact with the inner wall of the extension section (230). The guide mechanism (300) drives the furnace door (210) to move intermittently. When the furnace door (210) stops moving, one of the partition plates (430) is located in the extension section (230).

5. A vacuum heat treatment furnace according to claim 4, characterized in that, The support rods (410) on both sides of the partition plate (430) are respectively connected to the two guide rails (220), and the two adjacent rotating plates (420) are also slidably connected to the guide rails (220). One heat preservation bucket (600) receives one slide (510). When the heat preservation bucket (600) is replaced alternately, the placement position of the heat preservation bucket (600) is different.

6. A vacuum heat treatment furnace according to claim 5, characterized in that, The support rod (513) with a large outer diameter is connected to a counterweight (700), which is inserted into the second section (4212) of the first groove (421).

7. A heat treatment method for titanium-zirconium-niobium-tin alloy, comprising heat treatment using a vacuum heat treatment furnace as described in claim 6, characterized in that... Includes the following steps: S1. Preparation before homogenization: washing and drying; S2. Homogenization packaging: Vacuum packing of titanium-zirconium-niobium-tin alloy ingots into quartz tubes (800); S3. Homogenization heating: First, place the quartz tube (800) into the slide (510). After the two clamping blocks (520) clamp and fix the quartz tube (800), slide the slide (510) with the quartz tube (800) installed horizontally into the rotating plate (420) and the limiting rod (440). The guide mechanism (300) pushes the furnace door (210) so that the support rod (410) and the counterweight (700) slide in along the guide rail (220). Close the furnace door (210) so that the quartz tube (800) is kept warm in the furnace body (200) at 1000℃ for 2 hours. S4. Homogenization cooling: The furnace door (210) is intermittently moved by the guide mechanism (300). When the furnace door (210) stops moving for the first time, the partition plate (430) closest to the furnace door (210) is located inside the extension section (230). The heat preservation barrel (600) is placed on the base (100) of the furnace door (210) and the furnace body (200). When the furnace door (210) moves again, the rotating plate (420) gradually moves away from the furnace body (200). When the furnace door (210) stops moving, the rotating plate (420) leaves the furnace body (200) and rotates downward. During the rotation, the counterweight (700) drives the large-diameter support rod (513) to move downward, and drives the abutment rod (517) to abut the quartz tube (800). The rotating plate (420) stops rotating, and the slide (510) moves vertically downward along the rotating plate (420). The quartz tube (800) enters the heat preservation barrel (600) while maintaining a vertical state. S5, cold rolling deformation; S6. Annealing heat treatment: Samples are cut from cold-rolled sheet along the rolling direction, mechanically polished and ultrasonically cleaned with anhydrous ethanol, and then vacuum-sealed in a quartz tube (800). The quartz tube (800) is first placed in the slide (510). After the two clamping blocks (520) clamp and fix the quartz tube (800), the slide (510) with the quartz tube (800) is horizontally slid into the rotating plate (420) and the limiting rod (440). The guide mechanism (300) pushes the furnace door (210) so that the support rod (410) and the counterweight (700) slide in along the guide rail (220). The furnace door (210) is closed. The sample is annealed for 30 minutes at different temperatures. S7. Annealing and cooling: The furnace door (210) is intermittently moved by the guide mechanism (300). When the furnace door (210) stops moving for the first time, the partition plate (430) closest to the furnace door (210) is located inside the extension section (230). The heat preservation barrel (600) is placed on the base (100) of the furnace door (210) and the furnace body (200). When the furnace door (210) moves again, the rotating plate (420) gradually moves away from the furnace body (200). When the furnace door (210) stops moving, the rotating plate (420) leaves the furnace body (200) and rotates downward. During the rotation, the counterweight (700) drives the large-diameter support rod (513) to move downward, and drives the abutment rod (517) to abut the quartz tube (800). The rotating plate (420) stops rotating, and the slide (510) moves vertically downward along the rotating plate (420). The quartz tube (800) enters the insulation barrel (600) while maintaining a vertical position.

Citation Information

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